OCTOBER 2015 # 33 the Analytical Scientist

Upfront In My View Solution Sitting Down With Can a hydrogel sensor track The comparative bullet lead The innovative RISE of Bioanalytical trendsetter down microbial culprits? analysis (CBLA) showdown correlative microscopy Bob Kennedy

12 18 – 20 52 – 54 58 – 59

THE POWER LIST 2015

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The Power List 2015 –Online

You can find The Power List 2015 on page 31; however, space limitations have prevented us from sharing Chromatoraphy is everything our Power Listers had to say. what we do and who we are. Online, you can find The Power List in all its full glory, with responses We are an independent, international, and diverse team of employee-owners that range from most important life not shackled to a speci c brand of instrument or geographic region. We live lessons to encounters with serendipity and views on the future of groups, and breathe phase chemistry, peak separations, resolution, and inertness because niche areas or even analytical science while chromatography may be a necessary tool in your business, it is our business. as a whole. Tea With Rich conference. Gérard then discusses his And it is a business that we directly serve across 100+ countries and six continents Is one of your analytical heroes current research: multidimensional on The Power List – check online What’s better than a nice cup of tea and chromatography and its utility in finding with unrivaled Plus 1 service, applications, and expertise. to read more. a chat? “Tea With Rich” – an ongoing answers to global and complex problems, series of informal interviews with key before considering HPLC 2025... www.theanalyticalscientist.com/ analytical scientists in glorious settings We’re also treated to more “drone” From LC and GC columns to sample prep, reference standards to accessories, powerlist around the globe – makes a comeback footage and left wondering what Rich Restek is your rst and best choice for chromatography. from HPLC 2015 in Geneva with six Whitworth has been doing, as the final scientists that feature on The Power List. shot captures his departure... First up is Gérard Hopfgartner, who reflects on the responsibilities of Watch the video now: chairing the ever-successful HPLC tas.txp.to/1015/teawithgerard

It’s time for the TASIAs! i. Name of innovation ii. Brief description Do you have a piece of transformative (~10 words) technology or a brand new instrument iii. Detailed description that significantly raises the bar? Our (50-150 words) December issue will showcase the iv. The potential impact of the greatest analytical innovations of 2015. innovation (50-100 words) v. One image (if applicable) To nominate, email www.restek.com [email protected] with: Nominations close November 10

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 Contents ISSUE 33 - OCTOBER 2015 Editor - Rich Whitworth [email protected] Commissioning Editor - Iestyn Armstrong-Smith [email protected] Deputy Editor - Stephanie Sutton [email protected] Associate Editor - Roisin McGuigan [email protected] Associate Editor - Michael Schubert [email protected] Associate Editor - Victoria Barton [email protected] Scientific Director - Frank van Geel [email protected] Senior Designer - Marc Bird [email protected] Junior Designer - Emily Strefford-Johnson [email protected] Chief Executive Officer - Andy Davies [email protected] Chief Operating Officer - Tracey Peers [email protected] Publishing Director - Lee Noyes [email protected] Sales Manager - Chris Joinson [email protected] 10 Audience Insight Manager - Tracey Nicholls [email protected] Traffic and Audience Associate - Lindsey Vickers [email protected] Digital Content Manager - David Roberts [email protected] Traffic and Audience Associate - Jody Fryett [email protected] Mac Operator Web/Print - Peter Bartley [email protected] Tablet Producer - Abygail Bradley [email protected] Apprentice, Social Media / Analytics - Ben Holah [email protected] Editorial Advisory Board Monika Dittmann, Agilent Technologies, Germany Norman Dovichi, University of Notre Dame, USA Gary Hieftje, Indiana University, USA Emily Hilder, University of Tasmania, Australia Ron Heeren, FOM-AMOLF, The Netherlands Tuulia Hyötyläinen, VTT Technical Research Centre of Finland Hans-Gerd Janssen, Unilever Research and Development, The Netherlands Robert Kennedy, University of Michigan, USA Samuel Kounaves, Tufts University, USA Marcus Macht, SCIEX, Germany 12 58 Luigi Mondello, University of Messina, Italy Peter Schoenmakers, University of Amsterdam, The Netherlands Robert Shellie, University of Tasmania, Australia Ben Smith, University of Florida, USA Frantisec Svec, University of California at Berkeley, USA Ian Wilson, Imperial College London, UK 03 Online This Month Upfront Change of address: [email protected] 10 Fast Cell Sorting – on a Chip Tracey Nicholls, The Analytical Scientist, Texere Publishing Limited, Booths Hall, Booths Park, 07 Editorial Chelford Road, Knutsford, Cheshire, Tomorrow Never Knows, 12 Pathogen Identity Parade WA16 8GS, UK by Rich Whitworth General enquiries: www.texerepublishing.com 13 A Nose for Quality [email protected] +44 (0) 1565 752883 [email protected] 14 The Emotive List Distribution: On The Cover The Analytical Scientist (ISSN 2051-4077 ), is published monthly, by Texere Publishing Ltd

OCTOBER 2015 # 33 the Analytical Scientist 16 A Light Boost for Water and is distributed in the USA by UKP Worldwide,

Upfront In My View Solution Sitting Down With Can a hydrogel sensor track The comparative bullet lead The innovative RISE of Bioanalytical trendsetter 1637 Stelton Road B2, Piscataway, NJ 08854. down microbial culprits? analysis (CBLA) showdown correlative microscopy Bob Kennedy 12 18 – 20 52 – 54 58 – 59 The 2015 Power List goes Treatment Periodicals Postage Paid at Piscataway, NJ and “Revolver” – a pastiche of additional mailing offices POSTMASTER: Send US address changes to Klaus Voormann’s artwork THE POWER LIST 2015 The Analytical Scientist, Texere Publishing Ltd, 31 – 47 www.theanalyticalscientist.com for the 1966 Beatles album. C/o 1637 Stelton Road B2, Piscataway NJ 08854 Single copy sales £15 (plus postage, cost available on request [email protected]) Shimadzu_AnalyticalScientist_1014:Layout 1 19.09.14 15:18 Seite 1

Contents

In My View Features

18 Clifford Spiegelman and 31 The Power List 2015 William Tobin analyze the fall After a break in 2014 for of forensic comparative bullet the Top 40 Under 40, we lead analysis return with the Top 100 most influential people in the world 20 What is the role of high- of analytical science. precision istopic analysis Departments in medicine? asks Frank Vanhaecke Reports 52 Solutions: Supercharging Correlative Microscopy, 22 David Kofi Essumang thanks 28 The Analytical Scientist × by Olaf Hollricher you for your generosity, but Thermo Fisher Scientific needs more basic support Living in a Material World, by John Gilbert 24 The journal review process 56 Application Notes needs shaking up, says 48 The Analytical Scientist × Victoria Samanidou Thermo Fisher Scientific Orbitrap: Ten Years Young, 26 Lothar Brecker extols the by Alexander Makarov Sitting Down With virtues of NMR for greener chemistry 50 The Analytical Scientist × 58 Bob Kennedy, Distinguished Thermo Fisher Scientific Professor and Chair of A Taste of the Other Side, an Chemistry at the University of interview with Richard Fussell Michigan, Ann Arbor, USA.

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Ins_Mira_210x266_EN.indd 1 07.10.15 15:00 Tomorrow Never Knows Editorial “Turn off your mind, relax and float downstream...” The Power List is shining, it is shining.

elcome to what is perhaps the most anticipated issue of the year – if not for The Power List itself, then to find out how we could possibly Wlive up to our 2013 Sgt. Pepper’s Lonely Hearts Club Band cover... We hope you will agree that our pastiche of Klaus Voormann’s artwork for The Beatle’s 1966 album “Revolver” hits the right note – and emphasizes that The Power List should be about having fun first and foremost. As I indicate with the opening lyrics of Revolver’s final track – Tomorrow Never Knows – I hope that the majority of you are able to “turn off your (analytical) minds” and view The Power List as a source of entertainment (or inspiration) rather than a reason to become upset (or angry). As with our 2013 Power List, we do not pretend that our ranking is definitive or absolute. Rather, we want it to be a celebration of the analytical sciences, promoting the importance of the whole field to the wide world in a bid to raise the profile of the excellent and valuable work you do. Of course, many important and influential scientists are not present on the list. Why are they missing? Primarily, because you didn’t nominate them (or they didn’t nominate themselves). You see, The Power List represents more than just the influential people within. It stands as a testament to a wider You want to be sure community of analytical scientists that wants to get involved and join in with our cries for recognition. The Analytical Scientist itself is inclusive (not exclusive). And the reason we The new handheld Metrohm Instant have an open nomination process for The Power List is so that Raman Analyzer (Mira) for chemical and everyone and every niche area is given the opportunity. In pharmaceutical analysis. With 9000 spectra other words, we want it to be your list, not ours. in its library, Mira gives you unparalleled Once the nominations are in, our judges have the final power to identify what you are looking for daunting task of selecting their Top 100. Yes, this process is subjective – but the averaged views of five experts of the field – at the push of a button, anywhere! limits any unwitting (or otherwise) bias. The result? A list of 100 names that truly showcases the diversity metrohm-nirs.com – and this year, particularly – the personality of the people that make up the critical field of measurement science. Indeed, in 2015 our Power Listers explore topics such as serendipity and share To do list: some of their funniest or most unexpected moments (see page 31). 1. Enjoy The Power List while listening to Who will be on the 2016 or 2017 Power Lists? In the “Tomorrow Never Knows” by The Beatles immortal (and incomprehensible) words of Ringo Starr: (followed by the rest of Revolver). “Tomorrow Never Knows.”

Rich Whitworth Editor

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Upfront Reporting on research, personalities, policies and partnerships that are shaping analytical science.

We welcome information on interesting collaborations or research that has really caught your eye, in a good or bad way. Email: [email protected]

benchtop or floor-standing counterparts, Fast Cell Sorting one such device now rivals fluorescence cell sorters with its efficiency. The device, – on a Chip developed by a team of researchers led by Huang uses acoustic waves to rapidly sort A dime-sized microfluidic a continuous flow of cells on a dime-sized device harnesses acoustic chip (1). waves to efficiently sort cells “In recent years, microfluidics has emerged as a promising platform for Flow-cytometry based cell sorters aid in developing low cost, portable and disposal both medical diagnosis and biological equipment, says Huang. “Meanwhile, studies, but commercial systems tend the biosafety of acoustic waves has to be expensive (both to purchase and been proved in many applications maintain), large, and complex. Moreover, such as ultrasonic imaging. Thus, an according to Tony Jun Huang, associate acoustofluidic – the fusion of acoustics professor of engineering science and and microfluidics – cell sorter has great mechanics, Pennsylvania State University, potential to overcome the drawbacks of USA, they have been reported to fluorescence cell sorters.” significantly reduce cell viability, How does it work? According to Huang, especially when sorting fragile or sensitive the acoustic wave cell-sorting chip uses cells such as neurons, stem cells, and two focused interdigital transducers sperm cells. (FIDTs) to generate two surface acoustic And although lab-on-a-chip devices waves (SAWs) propagating in opposite typically struggle to keep up with their directions. The two SAWs interfere Shimadzu_AnalyticalScientist_1015:Layout 1 13.07.15 13:05 Seit

In-depth insights with each other, forming a standing a theoretical maximum throughput of with just a click SAW (SSAW) as well as pressure nodes 13,800 sorting events/s, comparable to Shimadzu‘s software solution and antinodes. “The cells/particles in commercial cell sorters”. ChromSquare V2 provides easy- the SSAW area experience an acoustic One limitation of the prototype is that to-use GCxGCMS data handling radiation force and are sorted to the it can only sort cells into two channels, nearest pressure node,” says Huang. Like compared with commercial cell sorters, for Comprehensive Chromato- a lens focuses light, the team used circular- which are capable of multi-channel graphy applications. shaped electrodes to focus the acoustic sorting. In previous work, Huang has waves. “We were so excited to figure demonstrated multi-channel sorting using • Most convenient features out that the performance of the FIDTs frequency-tunable IDTs and believes that benefit food, environmental, is highly dependent on the angle of the this could be applied in this case too: “We flavor & fragrance industries as circular-shaped electrodes. The 20° arc had plan to integrate the sorting unit with well as analytical chemistry the best focusing performance and could a laser-induced fluorescence detection achieve a focal beam with a similar size system to develop a high-performance • In-depth insights of the sample to that of the acoustic wavelength – this fully functional fluorescence-activated at any point in the process was the most critical step of the project,” acoustofluidic cell sorter. We will also adds Huang. apply this system in the sorting of fragile • All at a glance Many acoustic cell sorters have been cells, such as stem cells and sperm cells, via a user interface which shows developed in the past, but none have to prove the biosafety,” adds Huang. VB contour plot, chromatogram and rivaled the efficiency of commercial spectra in one window instrumentation (103-104 events per Reference second). Huang has already demonstrated 1. L Ren et al., “A high-throughput acoustic cell • Meets the needs error-free sorting at a throughput of sorter”, Lab Chip, 15, 3870-3879 (2015). for qualitative and quantitative 3300 events/s, but says, “Our device has DOI: 10.1039/C5LC00706B. comprehensive GCxGCMS

www.shimadzu.eu 12  Upfront

structures in a user-friendly manner, we visually monitored, measured with a Pathogen could have a broadly applicable sensor for spectrometer, or determined from the microbial pathogens,” says Liu. Debye diffraction ring diameter, and Identity Parade The sensor relies on a selective protein offer sensitivity of about 40 CFU/mL hydrogel coated with spatially-defined for C. albicans in aqueous solution. Two-dimensional photonic 2D photonic crystals (PC) – the latter Although the platform is sensitive, crystals combined with being an area in which the Asher group a key limitation is the lack of true spectroscopy shines a light on has significant expertise. In the proof- selectivity – the sensor detects any microbial culprits of-concept paper, the hydrogel was microbial organism with mannan on embedded with Concanavalin A (ConA), its cell surface. To that end, the team The best way to treat an antibacterial a lectin protein that multivalently is working towards achieving absolute infection is to target the root cause. So and selectively binds to poly-mannose selectivity – by integrating antibodies, why don’t we do it more often? “Detecting (mannan) – a carbohydrate structure that for example, with a focus on E. coli bacteria is a fairly lengthy process, so is found on the cell surface of Candida O157 for food poisoning, and MRSA – physicians tend to give patients a broad- albicans (the fungus responsible for a persistent scourge of hospitals. spectrum antibiotic that wipes out all the oral thrush). Liu says, “While there are Moreover, they are also working on bacteria as soon as possible instead of many ways to make a protein-engineered increased response time, portability and waiting to see which pathogen is actually hydrogel, we simply used the protein as reusability. Liu and Asher certainly have causing the problem,” explains Xinyu the polymeric backbone and cross-linked big plans for the future of their next- Liu, assistant professor at the University it to glutaldehyde. This worked out generation sensor: “If we can reduce of Pittsburgh, PA, USA. Liu, Sanford fantastically well (to my surprise at least)! the cost of its manufacture, it can be Asher, and their respective research The cross-linked Con A protein retains distributed to those in resource-poor groups, decided to develop a new method its secondary structure and was still able countries, where the sanitation of water to identify pathogens by combining 2D to recognize mannan efficiently.” and food is problematic,” adds Liu. VB photonic crystals with spectroscopy (1). When C. albicans is present, Con Liu decided to target carbohydrate A binds to mannan to form crosslinks Reference structures found on the cell surfaces of that shrink the protein hydrogel, 1. S A Asher et al., A photonic crystal protein microbial organisms: “We envisioned that which reduces 2D PC particle spacing, hydrogel sensor for Candida albicans, Angew. if we could come up with a way to rapidly causing a blue-shift in diffracted Chem. Int. Ed. (2015). DOI: 10.1002/ sense these microbial carbohydrate light. The diffraction shifts can be anie.201506205 Behind every great (U)HPLC A Nose for system… Quality

Sniffing out ‘off smells’ in drinking water with a is a great bioelectronic sensor column It’s clear that researchers Seunghun Hong, Hwi Jin Ko, and Tai Hyun Park, and the team at Seoul National University, South Korea, all have a nose We pride ourselves in: for sensing; they have already developed several human nose-like biosensors for different applications, such as disease diagnosis and food quality assessment. Selectivity Park explains why drinking water was • silica, polymer, hybrid, core shell technology next on the agenda: “Recently, a severe green algal bloom has wreaked havoc on the water supply in Korea. So we started to develop a bioelectronic nose for Scalability Robustness Reproducibility monitoring the quality of drinking water.” • UHPLC ↔ HPLC • pH • day to day Even the purest of water contains ↔ PREP • temperature • column to column compounds that contribute to its smell or • easy method transfer • 100% aqueous eluents • lab to lab flavor – and the human nose is extremely sensitive to two small, odorous molecules that often slip through the water treatment www.ymc.de | Phone: +49 2064 4270 | [email protected] process. “The bioelectronic sensor was able to selectively detect geosmin and 2-methylisoborneol in drinking water down to 10 ppt,” says Park. “Although YMC Island v4.indd 1 13/10/2014 13:27 these compounds are completely safe at this concentration, the result is an out which ones bind the odor-causing nanovesicles, such as olfactory receptor earthy, musty-smelling water, which is molecules. Once identified, a single-walled proteins, nanodiscs containing olfactory off-putting to drink – so the challenge carbon nanotube field-effect transistor was receptor proteins and peptides, and so on.” was to find the human olfactory receptors functionalized with olfactory nanovesicles. The researchers also have plans to take that bind specifically to geosmin and The human olfactory receptors afford their nose into the digital world: “Our next 2-methylisoborneol,” Park added. the bioelectronic nose higher selectivity step is to integrate the bioelectronic nose Current methods, such as GC-MS, are compared with any other sensing material, with a smartphone application by applying labor-intensive and time-consuming, but which allows it to detect odor molecules multi-channel sensing and wireless the bioelectronic nose can analyze water in various water samples without any pre- transport technologies,” adds Park. VB samples in real-time. “This makes the treatment process. sensor suitable to real applications through But the approach is not without Reference integration into a portable device that we its limitations, as Park explains: 1. M Son et al., “Real-time monitoring of geosmin are currently developing,” says Park. “Unfortunately, because nanovesicles and 2-methylisoborneol, representative odor Hong, Ko, Park and the team of are biological materials, they do have a compounds in water pollution using bioelectronic researchers first screened a number shelf-life – we are currently developing nose with human-like performance”, Biosensors of human olfactory receptors to find more stable and reusable alternatives to and Bioelectronics, 74, 199–206 (2015).

www.theanalyticalscientist.com 14  Upfront

The Emotive List?

The 2015 Power List will likely thrill, disappoint and annoy in (possibly) equal measures – but what does it mean to the people on it? In short: don’t take it too seriously...

“The Power List is great fun – and I like to think that it doesn’t really matter that much! But I also know that I will probably be mildly disappointed when I eventually – and inevitably – fall off it when I am displaced by much abler analytical scientists. With apologies to “I could paraphrase Groucho Marx – do I technology that underpins measurements Oscar Wilde: “There is only one thing want to trust a list that includes me among made in other more high profile fields.” worse than being on The Power List, and its members? It’s certainly a difficult job to – EH that is not being on it.” – IW come up with such a list and quantify the influences of analytical chemists, especially “Obviously I love it, if I keep moving “It is an interesting exercise, but I think with all the subfields around the world. up! Actually, I think it is a little for every person on this list who’s happy You have to include a balance between uncomfortable to be ranked in such a and appreciative, there’s an unhappy research topics, geography, gender and so dramatic fashion; however, my latest one who feels he or she ought to be on. Such lists always ignite controversy – thoughts are that it shouldn't be taken listed!” – HKL and when a group is under represented on too seriously and instead should be the list – it promotes conversation, which considered a bit of fun and a conversation “Anything that draws attention to the is a good thing. But – as with any list – it piece for those of us in the field.” – BK profound influence analytical science has will include some important individuals on our lives is a very good thing. By sheer while others are left out. It’s important to “It is always very nice to have a high Visually intuitive software designed for your separation accident, this corner of science, which make it clear that no one should take it ranking in The Power List and this frankly underpins most of modern life, too seriously!” – JS obviously caresses your ego. For those now with Robustness Testing has found itself in something of a corner, involved in drawing up the list, it must vital but somehow too reliable, essential “The Power List is fun and flattering be a big challenge to maintain credibility yet bizarrely undervalued. If The Power – but shouldn’t be taken too seriously.” and remain unbiased.” – PS List helps raise the profile of work in the – CF field, then its a good thing, whether that “It is an interesting exercise and a bit be with users, industry, agencies that “I think it is a great effort – and being of fun (and it’s nice to be included). fund research or early career researcher on it means huge peer recognition. However, the list is very subjective.” thinking of entering the field. If smart The fact that the ranking is based on – PH people don't enter the field then we are expert opinions lends credibility and DryLab® globally in big trouble.” – AL transparency.” – RA “The Power List is a measure of scientific 4 impact convoluted with personal “The thing I like most about The Power “I like that The Power List has got people popularity and visibility. That said, it for UHPLC Modeling List is that it raises awareness of not only talking about the analytical sciences might be important to recognize impact Visit www.molnar-institute.com to learn more analytical science but also some of the in general and that it highlights the on the scientific community other then tremendous science done in that field.” – JG importance the development of the strictly via ‘H-index’.” – JP Upfront 15

“It is a bold move to publish such a list, as needs – especially if it relates to such “To be honest, I personally do not there is any number of ways to find fault an ill-measurable quality as “power”. take lists very seriously. However, my in the method used to generate it. It is a Conclusion: great advertisement for colleagues actually recognized me on challenging – maybe impossible – task the field, but the individual ranking of The Power List 2013 and informed me, to accurately generate this list. It is easy somebody – or the mere fact that she so there are a lot of people who do take to think of people that you think are or he is in the list or not – should be lists very seriously! Since then, I feel very missing or should be in the Top 20 – but taken with the largest possible grain of honored of course to be on the list. I really at the end of the day, it’s just one list. salt.” – GD appreciate that this list is alternated with It generates discussion and it’s probably a young scientist list, such as the Top 40 good for people to think about who has “I’m honored to be included with such Under 40. After all, they are the boys and contributed to our field.” – MR a talented group of individuals, but girls who will take over and continue to emphasize that this has only happened boost analytical science and technology “No doubt The Power List helps because of the great team that I work in the future!” – MN promoting the analytical sciences and with.” - DS adds great prestige to the field. On “A good idea. It gets noticed by my the other hand, scientists are already “It is rather nice to be recognized by your colleagues, who have been known to part continuously compared and ranked by peers. Even if there might be some bias with money to buy me a beer...” – CP their citations, number of PhD students, in the list. It is quite an exclusive group h-index, and so on... Yet another type of scientists to belong to after all...” – AF Make up your own mind about the 2015 of ranking maybe not what this field Power List on page 31.

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Based Optimization Of Sewage on the composition and characteristics of A Light Boost Treatment) – a project that aims to a particular water sample.” “provide the water industry with a John Bridgeman, a professor of for Water robust yet straightforward technique, environmental engineering at Birmingham Treatment based on novel developments in the initially came up with the idea for the Advance your career in science field of fluorescence spectroscopy, project following positive preliminary with professional recognition that showcases your to optimize wastewater treatment studies (2). “The topic fitted my expertise Exploring fluorescence works performance, to reduce energy so we submitted a proposal under the experience, expertise and dedication spectroscopy’s ability to consumption and to monitor final Marie Curie Intra-European Fellowship monitor quality – and reduce effluent quality in real time”. Elfrida programme in 2012,” Carstea says, “Not Stand out from the crowd operating costs in wastewater Carstea, a researcher at the University only does the project bring research on Prove your commitment to attaining excellence in your field treatment works of Birmingham, UK, has been working wastewater monitoring a step forward, on the project, which comes to a close the prestigious fellowship also gives my Gain the recognition you deserve Thanks to substantial investment, the in October 2015 (1). career a boost!” Achieve a professional qualification that inspires confidence and trust EU has seen considerable improvements “From the beginning of my research One current method used for in the collection and treatment of career, I was interested in applying monitoring at wastewater treatment works Unlock your career potential wastewater. The downside? It has also fluorescence spectroscopy to water is the offline five-day biochemical oxygen Apply for our professional registers (RSci, RSciTech) increased pressure on current wastewater monitoring,” says Carstea. “The technique demand (BOD5) test, which measures or chartered status (CChem, CSci) treatment technologies. Enter is fascinating. Its beauty lies in its simplicity; the amount of oxygen consumed during FLUORO-BOOST (Fluorescence- it can provide a quick and effortless view the microbiological decomposition of Apply now

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organic material in water. Lower values BOD5 and fluorescence spectroscopy the fluorescence signal, but can be signal cleaner water; for example, pristine data, Carstea and the team collected significantly mitigated by regular cleaning rivers may give a reading of 1–2 mg/mL, both treated and untreated wastewater and anti-fouling copper tapes, according whereas untreated sewage could be several samples from five plants at different to Carstea. And temperature also has a hundred mg/mL. Although BOD5 is points along the process train. “We big impact on readings – Carstea applies very commonly used, it is labor intensive, measured BOD5 for all samples and a correction factor to the data. slow to yield data, and insensitive and recorded the fluorescence using different Despite the challenges, Carstea unreliable at low concentrations, all bench-top and portable instruments. The believes the project has been a success. of which make it unsuitable for online large dataset was essential in establishing The speed, sensitivity, accuracy and monitoring and process control. Indeed, a good correlation between fluorescence relatively inexpensive nature of the with an uncertainty in accuracy of 10– data and BOD5,” says Carstea. “The technique offers the potential for 15 percent, wastewater treatment works analysis of the data is in progress, but from a more modern approach to water tend to “over treat” water to ensure what we have seen so far, it challenges quality monitoring. VB compliance with regulations – and that’s our current knowledge about these two where potential savings can be made. parameters. We now know more about Reference Replacing the BOD5 method with the limitations of both techniques and 1. http://cordis.europa.eu/news/rcn/123830_en.html fluorescence spectroscopy could enable on how to improve fluorescence.” 2. J Bridgeman, et al., “Determination of changes in real-time control and adjustment of plant Carstea also discovered that the wastewater quality through a treatment works performance, which could in turn cut use of spectroscopy in this atypical using fluorescence spectroscopy”, Environ Technol, energy costs by up to 40 percent. application presents its own challenges. 34, 23, 3069-3077 (2013). DOI:10.1080/0959 To investigate the relationship between Biofilm formation on sensors can affect 3330.2013.803131.

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lead, and concluded – in a 1970 contract Quis Custodiet report to the AEC – that three analytes In My were insufficient to uniquely characterize Ipsos Custodes lead sources (known as “pots” in lead smelting parlance). View Conducting an autopsy of the It took almost two decades of forensic flaws of comparative bullet lead application using the three original analysis in forensic practice. In this opinion section, analytes before the FBI Laboratory added silver, bismuth, tin, and eventually experts from across the cadmium. The FBI Laboratory then world share a single confidently, but misguidedly, intuitively strongly-held view or concluded that six (and eventually seven) key idea. analytes, coupled with the precision of sophisticated instrumental analysis of neutron activation analysis (NAA) and/ Submissions are welcome. By Clifford Spiegelman, distinguished or optical emission spectroscopy (OES) Articles should be short, professor of statistics, Texas A&M University, to parts per million (ppm) levels, surely focused, personal and College Station, Texas, and William Tobin, must be sufficient to “fingerprint” a forensic metallurgist and failure analyst, molten source of lead. For nearly forty passionate, and may Forensic Engineering International LLC, years, FBI laboratory examiners testified deal with any aspect of Lake Anna, Virginia, USA. that crime scene bullets and defendant analytical science. (suspect) bullets “originated from the same They can be up to 600 Back in the 1960s, civilian research source of lead produced on the same day.” words in length and scientists at Gulf General Atomic Eventually examiners became emboldened (GGA) studied the feasibility of using to claim (and testify) source attribution as written in the first compositional comparisons of questioned the “same box of bullets.” person. (crime scene) and known (suspect) bullets The curiosity of forensic metallurgist and bullet fragments to determine putative William Tobin and his subsequent Contact the editors at source. The scientists were on contract research team was piqued in the late [email protected] from the US Atomic Energy Commission 1990s because the underlying premises (AEC, now the Department of Energy, required for efficacy of forensic CBLA DoE), which was seeking commercial practice contradicted well-established Find treasure in the most applications for its considerable capital metallurgical principles. Three underlying (nuclear reactors) and intellectual premises – or assumptions – are logically challenging of places resources. The research actually ascended required to validate opinions offered in to high profile forensic significance during criminal trials by CBLA examiners: i) 50- Biocompatible Solid Phase Microextraction the JFK assassination investigation after 60 mg samples used for forensic analyses one of the original researchers on the are representative of their sources, ii) the (SPME) probes and LC Tips GGA team testified before the US Senate “sources” were compositionally uniform Subcommittee on Assassinations to the (homogeneous), and iii) that each of the BioSPME devices enable direct sampling of biofluids, results of the JFK analyses. “sources” was unique. eliminating the need for time-consuming sample The US Federal Bureau of Investigation In 1998, out of scientific interest and preparation steps used in current bioanalytical methods. (FBI) Laboratory seized the opportunity an attempt to reconcile the apparent to expand its forensic services by adopting contradiction to long-established the methodology used by the GGA metallurgical principles and phenomena, To learn more, visit scientists for comparative bullet lead the forensic metallurgy team began sigma-aldrich.com/biospme analysis (CBLA). The original GGA team to research the scientific and legal used three analytes (antimony, copper and underpinnings of the practice, including arsenic) in efforts to characterize bullet secondary lead smelting and refining, the ©2015 Sigma-Aldrich Co. LLC. All rights reserved. SIGMA-ALDRICH and SUPELCO are trademarks of Sigma-Aldrich Co. 12382 LLC, registered in the US and other countries. Solutions within is a trademark of Sigma-Aldrich Co. LLC.

the Analytical Scientist In My View  19

complete domain literature, and transcripts If everyone owned bullets of the same publications, and court testimonies of of testimonies from judicial proceedings. composition in a geographical locale forensic metallurgical and statistical The team was shocked at what they found. of a shooting homicide, a finding of research team members, a consequent Although there was extensive peer- “analytically indistinguishable” bullets in study by the National Research Council reviewed literature on the analytical the possession of a suspect compared to (NRC) of the US National Academy of chemistry methodology of neutron those recovered from a victim should never Sciences (NAS), publications by the NRC activation analysis (NAA) and inductively be presented to courts as incriminating statisticians, and reporting by the media, coupled plasma atomic (and later optical) evidence. In such a hypothetical scenario, the following objectionable aspects of the emission spectroscopy (ICP/OES) for there is no probative value of a claimed forensic practice were exposed: generating precise compositional data “match” between bullets recovered from for bullet lead, there was not a single a crime scene and those recovered from a • The forensic practice was developed comprehensive or meaningful publication suspect. Therefore, unless comprehensive almost exclusively by forensic establishing or corroborating the validity of and meaningful studies have been examiners and analytical chemists. the three required underlying assumptions conducted and presented as to rarity or There was no evidence of vital cross- for the practice. Worse still, researchers prevalence of analytically indistinguishable discipline input from metallurgists or in a subsequent study of retail product bullets in a regional population of bullets statisticians; distribution in the USA found shocking at the time of a shooting crime, such • No comprehensive or meaningful geographic concentrations of same- evidence should not be used to determine study existed of the assumption that composition bullets in local and regional guilt or innocence in judicial proceedings. each pot (‘source’) of lead was unique areas, dealing a fatal blow to forensic and Based primarily on flaws demonstrated in composition; probative utility of the practice. by the metallurgical research, consequent • No comprehensive or meaningful

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study existed of the assumption • There had never been any true practice, that “same composition that each forensic sample was (mainstream) scientific oversight = same source” (the legal “task at representative of its original source; during development of the forensic hand”) was never tested. • No comprehensive or meaningful practice; study existed that each source was • Papers promoting the practice had As it turns out, the FBI practitioners had compositionally homogeneous; been “peer-reviewed” only by the established themselves as “the world’s • No study existed as to whether or very insular community of CBLA CBLA experts” based on nothing more not bullet composition “matches” practitioners themselves and/or only than speculative and intuited assumptions had any probative value for criminal by chemists relating to the analytical that were eventually shown to be trials, largely because there chemistry methodology, which was false, perpetuating probably the most existed no study of retail product never under challenge. The actual sophisticated “junk science” that ever distribution in the USA; underlying assumption for the deluded jurisprudence in North America.

while the heavier will prefer the strongest MS can analyze a broader range of The Isotopic bonding environment. target elements. Indeed, geochemists In ‘traditional’ isotope systems welcomed MC-ICP-MS with open arms Doctor (hydrogen, nitrogen, carbon, oxygen for studying non-traditional isotope and sulfur), variations can be studied systems in various application areas. High-precision isotopic using gas source isotope ratio mass Today, a few institutions around the analysis of essential metals spectrometry (IRMS). But for heavier world are using MC-ICP-MS for high- is beginning to show elements, the relative difference in precision isotopic analysis of metals in real promise for medical mass between the isotopes was initially body fluids as a potential new tool for diagnoses. Here, I share thought too to be small to result in a medical diagnosis. In a NASA-funded ENVIRONMENTAL TOTAL PETROLEUM some of the progress in this measurable variation in the isotopic study, a research group at Arizona State Tom Bontes, HYDROCARBON (TPH) ANALYSER® exciting application area. composition. However, with the advent University, USA, discovered that natural official competitor World Championships • Removes chemical splitting for ali/aro speciation of improved instrumentation – especially changes in the isotopic composition of Fencing 2015 • Ali/aro determination in one step/injection that of multi-collector inductively calcium in urine indicate bone loss in bed Empowered by JSB! coupled plasma-mass spectrometry rest patients. In follow-up work, they The five critical challenging areas were: (MC-ICP-MS) in the early 1990s – it is demonstrated that the approach could • Reduce sample preparation steps • Minimise the number of methods for TPH analysis now generally accepted that all elements also signal multiple myeloma disease • Visually display and report more accurate TPH data with two or more isotopes show natural activity. In a pilot study, researchers • Visually display and report of banding, fractions, classes variation in their isotopic composition at the École Normale Supérieure of compounds and individual compounds • UKAS & MCERTS accreditation By Frank Vanhaecke, professor, because of isotope fractionation effects. de Lyon, France, showed that the Department of Analytical Chemistry, Before the introduction of MC- isotopic composition of serum copper Results Summary Ghent University, Belgium. ICP-MS, only thermal ionization in breast and colorectal cancer patients • Clear separation of aliphatics from aromatics • Unambiguous banding mass spectrometry (TIMS) provided reflected response to chemotherapeutic • Quantitation 5-5000 ppm TPH linearity The lightest elements vary in their sufficient precision for studying natural treatment more quickly than traditional >0.995 - RT %RSD’s column 1 <0.01% isotopic composition due to isotope variation in the isotopic composition biomarkers. • Result repeatability <1% • Recovery 98 -101% fractionation; this is something we’ve of heavier elements. However, its Ghent University, Belgium, is among (500 – 2500ppm doped soil) known for quite a while. It occurs when widespread use was hampered because these pioneering institutions. In the SHARPER PEAKS, the isotopes of an element do not take of low sample throughput capability and work performed so far, we have shown Mineral Oil part with exactly the same efficiency in a the limited ionization power of its source that Wilson’s disease, a hereditary illness BETTER SEPARATIONS Aliphatics physical process or (bio)chemical reaction. (only elements with an ionization energy that interferes with the excretion of Aromatics

Differences in reaction rates (kinetics) up to 7 eV are efficiently converted into excess copper into the bile, leads to a GCxGC 3D Plot and in equilibrium (thermodynamics), M+ ions). With the ICP providing a significantly lighter isotopic composition Mineral Oil therefore, occur – for example, the lighter much more powerful ionization source of serum copper. In liver cirrhosis of two isotopes will react more quickly, at atmospheric pressure, MC-ICP- sufferers, we have revealed that the Local offices in: [email protected] • UK & Ireland • Belgium the Analytical Scientist www.go-jsb.com • Germany • Netherlands In My View  21

ETH-Zürich, Switzerland. The serum earlier and non-invasive diagnosis and “We have shown concentration of ferritin is the clinically prognosis of diseases. Are we there yet? most useful measure of iron storage. Not exactly. Several issues, such as the that Wilson’s disease Low serum ferritin levels indicate specificity and reproducibility of the depleted iron, whereas increased levels shift in the isotopic signature of the leads to a may indicate overload. Inflammatory target element(s), need assessing, and conditions (or infections, cancer and we need a more thorough understanding significantly lighter liver disorders) will also influence ferritin of the underlying causes of the changes concentration; as a result, a large number we observe in isotopic composition. isotopic composition of patients remain at risk from iron However, we are working on this, depletion or overload. We have seen a experimenting in vitro and in vivo to of serum copper.” link between iron status and the isotopic gain greater insights. composition of whole blood iron. This is In a biomedical context, the isotopic a potentially better marker for iron status analysis of non-traditional isotope isotopic composition of serum copper and it has the benefit of offering access systems is, therefore, intriguing, reflects the severity of the disease. This to both short term (via serum iron) and particularly as it shows real potential breakthrough is potentially useful for longer term (via red blood cells or whole for clinical practice. I am glad that prioritizing liver transplant patients. blood iron) information. my research group and I – and our Another promising application is Despite the relatively high cost of colleagues from the Ghent University isotopic analysis of whole blood/serum an MC-ICP-MS analysis, the medical Hospital – can contribute to progress in iron, as pioneered by researchers at world is interested in the approach for this exciting area.

ENVIRONMENTAL TOTAL PETROLEUM Tom Bontes, official competitor HYDROCARBON (TPH) ANALYSER® World Championships • Removes chemical splitting for ali/aro speciation Fencing 2015 Empowered by JSB! • Ali/aro determination in one step/injection The five critical challenging areas were: • Reduce sample preparation steps • Minimise the number of methods for TPH analysis • Visually display and report more accurate TPH data • Visually display and report of banding, fractions, classes of compounds and individual compounds • UKAS & MCERTS accreditation Results Summary • Clear separation of aliphatics from aromatics • Unambiguous banding • Quantitation 5-5000 ppm TPH linearity >0.995 - RT %RSD’s column 1 <0.01% • Result repeatability <1% • Recovery 98 -101% SHARPER PEAKS, (500 – 2500ppm doped soil)

Mineral Oil

BETTER SEPARATIONS Aliphatics

Aromatics

GCxGC 3D Plot Mineral Oil

Local offices in: [email protected] • UK & Ireland • Belgium www.go-jsb.com • Germany • Netherlands 22  In My View

chromatography (HPLC) and Fourier Letter to the transforms infrared spectroscopy (FTIR). Receiving help to buy such equipment “We’ve experienced YOU CONGRATS! DID THE IT TO BEST PERFORMANCE! Editor: Supplied is certainly a great start, but some of the suppliers who sell the equipment don’t always substantial periods but not Supported follow in the same charitable footsteps; for no reason Still use them? to example, by refusing to supply an accessory of instrument The gift of analytical that renders the equipment unusable capability is welcomed with through its absence. Indeed, there are downtime just open arms, but needs to go currently several types of instrumentation beyond core instrumentation. that have become ‘white elephants’ in several because a fuse laboratories in the developing world. In doing so, they are denying laboratories the needed changing.”

full benefit of the contribution of donor NO agencies and their efforts to support quality YES research and development in Africa – and just because a fuse needed changing. I also they are still failing to line their own pockets remember a time when we had some ion- in many cases. selective electrodes, but once the calibrating By David Essumang, Professor, Sadly, I have come to the conclusion that solutions ran dry, the set-up was not used Department of Chemistry, University of it is illogical to ask for new equipment from again. Why? Because there was no clear Are you already using them? already you Are Cape Coast,Cape Coast, Ghana. donors when the ones supplied earlier sit method that indicated how we could untouched, having never performed a single prepare more solution. Rich Whitworth’s editorial “How Do analysis. I remember in 2004, the chemistry Certainly, some of these difficulties may You Measure Success?” last month struck department at the University of Cape Coast seem trivial to someone in a well-stocked a chord with me. He posed a question: received some analytical equipment to boost laboratory with easy access to technical “Is your nation successful because it has research and development in the university. support and almost limitless resources. But assured the safety of its citizens with high- The equipment included GC-MS, FTIR their combined affect on the development quality food and drugs (or simply shelter) or and atomic absorption spectroscopy of analytical chemistry in the developing because it is rolling out more charitable and (AAS) detector and was supplied through world is very real. NO

advanced programs to help resource-poor the vendor’s African agent in Egypt. But To that end, I would like to make a YES nations do the same?” I believe Whitworth we never received the full complement of passionate appeal to the international +49 (0)89/ 93 99 62 37 [email protected] www.shodex.de Middle East, Europe, Russia Africa, was indicating that countries with advanced accessories and the instrumentation has community for continued help. Our doors analytical capability could do more to aid never been used. In fact, we do not even are wide open to any organization that is nations that are less fortunate in that regard. know what to do with it. In such cases, it is prepared to support the development of And he is half right. But in my country clear that we are not getting value for (our analytical chemistry in Ghana and other of Ghana, the difficulty for analytical charitable donor’s) money. And so here, I developing nations. It is my sincere hope chemists goes beyond the simple lack of would like to kindly ask both donors and that better analytical capability will help analytical equipment. suppliers to ensure that any equipment – us to identify most of the human health It is a known fact that science in most and all accessories – are supplied in full and risk factors that result from the presence developing countries is not so advanced supported with proper training; otherwise, of numerous emerging chemicals in our despite several efforts by governmental and all the effort – and financial support – is environment. It would also afford us the GmbH Denko Europe Showa Business Shodex Konrad-Zuse-Platz 4 81829 Munich, Germany non-governmental agencies to support it. for naught. opportunity to give proper training to In some cases, charitable organizations The lack of adequate maintenance our students and start a more positive support governments in their efforts to schemes for analytical equipment is another cycle. But there is a small caveat: simply develop science by financing the purchase serious challenge to raising our scientific throwing financial resources at a problem of analytical equipment. Equipment game. When equipment fails, the lack of does not always make it go away; we that is very much in demand includes technical know-how makes it very difficult also need support in terms of accessories, gas chromatography-mass spectrometry for us to attempt a repair. We’ve experienced consumables and training to ensure that the (GC-MS), high-performance liquid substantial periods of instrument downtime big investments do not go to waste. HPLC Polymeric Columns

the Do you know Do you the advantages HPLC of polymer-based columns? Analytical Scientist columns: of polymer-based the advantages are These 13). chemical stability (2 to an extended pH range leads to great The - detection. the use of sensitive bleeding allows low The - a higher resolution. variety properties- Large of material create techniques. almost all separation for available are They - per injection price due to The is cheaper than in silica-based columns - (2-3 times longer than silica-based). their extended lifetime You can test a Shodex column for for column a Shodex can test You us! just contact free, +49 (0)89/ 93 99 62 37 Showa Denko Europe GmbH [email protected] Shodex Business www.shodex.de YES Konrad-Zuse-Platz 4 Europe, Middle East, CONGRATS! YOU 81829 Munich, Germany Africa, Russia HPLC Polymeric Columns DID IT TO THE BEST You can test a Shodex column for PERFORMANCE! free, just contact us!

YES Are you already using them?

Do you know the advantages of polymer-based HPLC columns?

NO NO

These are the advantages of polymer-based columns:

- The great chemical stability leads to an extended pH range (2 to 13). - The low bleeding allows the use of sensitive detection. - Large variety of material properties create a higher resolution. Still no reason - They are available for almost all separation techniques. to use them? - The price per injection is cheaper than in silica-based columns due to their extended lifetime (2-3 times longer than silica-based). 24  In My View

Critical, manuscripts and provide a report that notes weak points or suggests improvements, “Unfortunately, the Constructive or generally maintaining standards of quality and reliability. The role is advisory and system is often Crass? the editor has no obligation to accept the opinion of the referee, though it is often biased, unjustified, used and adapted. Peer reviewers are The somewhat imperfect peer qualified experts of the same or relevant incomplete – and review process has a long scientific field – a valuable resource indeed. way to go before it could be But recruiting referees is a difficult sometimes plain considered ‘standardized’ task, as they offer their time and expertise – but at least we should be on a voluntary basis. Sometimes they insulting, unfair, heading in the same direction. are suggested by the authors, but with restrictions; they should typically not be ignorant, or from the same university, country, research team, and so on. In the case of any conflict incorrect.” of interest, editors are informed. The peer review process is usually anonymous (single-blind review), where For example, International Standards the names of the reviewers are hidden exist in the food industry that set out By Victoria Samanidou, professor of from the author. In some cases, both the requirements to harmonize existing analytical chemistry, Department of the reviewer and the author remain methods through an internationally Chemistry, Aristotle University of anonymous, which further ensures fair recognized system to ensure that food Thessaloniki, Greece. judgment (double-blind review). Open is safe for the consumer. International reviews are rare, but possible. Standards guarantee that products and Upon completion of research, scientists The peer review process should promote services are safe, reliable and of good typically want to communicate their integrity in research publications. quality. They are developed using a findings to the scientific community, with Unfortunately, the system is often biased, consensus-based approach and comments the greater goal of driving science forward. unjustified, incomplete – and sometimes from all experts are taken into account. There is no doubt that publication in peer- plain insulting, unfair, ignorant, or Could all publishers be in a consensus and reviewed journals is currently the most incorrect. I suspect that most scientists guarantee the same degree of integrity and acceptable way of sharing the outcome of have faced, at some time, a criticism that reliability for the authors? scientific investigation. No surprise then was not scientifically accurate. I recall one The Committee on Publication Ethics, that a great variety of journals, with high, reviewer who wondered if QuEChERS which is a forum for editors and publishers medium or low impact factor, have jumped was referring to a German car! Irony, of peer reviewed journals that provides to the demand, offering the opportunity ignorance, arrogance – or all of the above? advice on all aspects of publication ethics, to present their work to audiences in the And so here is my question: can peer helps steer us in the right direction, but still same niche or broad field. reviewing be harmonized or standardized is not enough. In my view, the reputation The journals’ editors, who essentially by standards organizations? Manuscript of a scientist alone is not sufficient to prove decide whether the work deserves reviewing is based on the volunteer work of integrity of judgment. publication or not, must handle all scientists who spend time and effort giving Perhaps there is long way to go before all manuscripts at some point. Initially, the editors advice and also helping authors to parties involved can agree upon standards task of accepting or rejecting was solely improve the presentation of their work – of expected ethical behavior in the world the role of the editors-in-chief or editorial and this is undoubtedly highly appreciated. of publishing. Clearly, we cannot apply committees. But the sheer volumes of But harmonized procedures are essential standards as strictly as other more rigorous POWERED BY 40 YEARS OF GFC EXPERIENCE: TSKgel UP-SW3000 manuscripts flying around our increasingly when it comes to offering unbiased ISO systems, but I do believe the principles electronic and interconnected world have judgment. Are all parties – journal editors, could and should be adapted and adjusted HIgHER RESOlUTION FOR mAb AggREgATE ANAlySIS COMPATIBlE WITH All UHPlC INSTRUMENTS demanded the need for hordes of so-called authors and referees – ready to work to fit the needs of a scientific community SHORT RUNTIMES IN QUAlITy AND PROCESS CONTROl SEAMlESS TRANSFER OF HPlC METHODS referees or reviewers. Reviewers evaluate together to aim for such standardization? that wants to share the fruits of its labor. FIND OUT MORE ABOUT OUR NEW gEl FIlTRATION COlUMNS FOR UHPlC ON HTTP://BIT.ly/1lOjS3N

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From Analysis civilization came to our planet, and so Goes to Play. enzymes are not at all optimized for “NMR spectroscopy to Synthesis biosynthetic applications in chemical synthesis of artificial products. The is an alternative development of usable biocatalyzed Using saturation-transfer synthetic processes demands the selection versatile analytical difference (STD) NMR and of a suitable enzyme as well as optimization in situ NMR spectroscopic of the molecular interaction between method that allows analyses of biocatalyzed enzymes, co-factors, substrates and the reactions to optimize desired product. Indeed, we must apply fast and accurate application of enzymes in a complex combination of wet chemical organic synthesis. synthesis and analysis in addition to in silico determination of simulation to guide such a process. During development, it is necessary to gain detailed reliable information analytical information about the catalytic process at a molecular level, including about catalysis at a kinetics of the biotransformation as well as concentrations and structural data of all molecular level.” molecules involved in the catalytic event. By Lothar Brecker, Department of Organic Furthermore, detailed knowledge of the Chemistry, University of Vienna, Austria. binding processes is indispensable. technique to determine complete mapping Such data can be recorded using several of ligand/enzyme binding in a global as Sustainability in chemistry and the concept labor-intensive and costly analyses. well as in-site specific way. The determined of green chemistry has become an important However, NMR spectroscopy is an binding patterns allow analysis of the topic in modern synthetic applications alternative versatile analytical method that specific substrate, intermediate and product over the last two decades. Nowadays, the allows fast and accurate determination of binding to enzymes on a molecular basis. chemical industry checks their production reliable information about catalysis at a And a concomitant specific co-substrate processes with respect to sustainability, and molecular level. In particular, 1H-NMR is and co-enzyme binding can be determined, several companies are seeking novel and good at monitoring biocatalyzed reactions, including detailed analysis of ternary sustainable solutions in synthesis. as the proton is ubiquitous in organic enzyme/co-enzyme/substrate complexes. One important and widely used approach molecules and has a high sensitivity of the All of the resulting binding patterns can in this development is the application of NMR active nuclei. To that end, on-line be studied during catalysis as well as under biocatalyzed reactions to synthesize monitoring can be performed to measure binding-only conditions, meaning that organic compounds. The biocatalysts are spectra in situ at any stage of enzyme this NMR-based analytical technique Pittcon is the leading conference and exposition for the latest easily available from microbial growth catalyzed reactions without sampling is particularly suited to performing a and combine a couple of properties that the reaction mixture, which makes comparison of wild type and corresponding advances in Laboratory Science. Attending Pittcon gives you are important for performing sustainable manipulating the biotransformation mutant enzyme binding. a unique opportunity to get a hands-on look at cutting-edge chemical synthesis. Notably, they distinctly much more accessible. All the data about In summary, the combination of reduce activation energy in the catalyzed molecular structures and compound both STD NMR and in situ 1H NMR product innovations from leading companies. 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Living in a Material World

Research into migration of packaging materials into food began decades ago. And despite the relatively inconspicuous nature of this niche area, it is characterized by some of the most significant modern-day conversion to the polymer, oligomers may substances of much higher molecular challenges in food analysis. remain. Moreover, as indicated above, weights like mineral oils. Migrants range plastics need numerous additives to make in polarity from highly polar to non-polar By John Gilbert, Director at FoodLife them suitable for packaging – antioxidants, organic molecules through to classical International, York, UK. heat stabilizers, UV absorbers, plasticizers metals, as well as metal nanoparticles. and colorants, and so on – there are literally Therefore, the full range of analytical tools I first got involved in analysis of food hundreds of potential substances, which must be employed in migration testing, contact materials back in the mid-1970s, represents a significant analytical challenge. including headspace GC-MS for volatiles, when it was recognized that vinyl chloride It’s fair to say that food-packaging LC-MS/MS, LC-high-resolution accurate monomers could migrate into foods. analysis is very niche compared with, for mass (HRAM) MS (Orbitrap) through to Needless to say, subsequent investigations example, pesticide residues, but there is AAS and ICP-MS. Even DART-Orbitrap led to regulations being introduced that a lot of awareness within the packaging MS has been investigated for direct analysis controlled monomer levels both in plastic industry – and the food industry certainly of both plastics materials as well as extracts and in food, and a new aspect of food realizes it must comply with regulations. from plastics without any clean up. analysis was born, expanding into other food contact materials. Analytical drivers NIAS work Today, a food contact material is, by Over the years, a great deal of food In 2011, Commission Regulation (EU) definition, one that is approved for food packaging regulation has actually been No. 10/2011 brought together numerous applications – the EU, for example, has driven by developments in analytical previous regulations, and introduced a positive list of starting materials and techniques. Going back to the 1970s, the concept of non-intentionally added plastics additives restricted to substances MS and GC-MS were around, but the substances (NIAS). The new regulations that are deemed safe for food packaging. techniques were relatively specialized. place responsibility on food producers Polyolefins (HDPE, LDPE and PP), People were using headspace GC with to demonstrate due diligence for PET and polystyrene are probably the FID, and LC-MS was yet to be developed. untargeted substances – a challenging most important plastics in common use in As instrumental techniques have become feat. With NIAS, the substance could be a bottle, sheet and film formats. Films can more sensitive – and as costs have come decomposition product from additives used be particularly complex in construction, down – methods have been developed in the plastic packaging or an adventitious involving multiple laminate layers to achieve and regulations established using the contaminant – there is a huge range of the desired properties, sometimes with techniques available. Indeed, today’s possibilities. And that has led to a real adhesive between layers, and printing on regulations were beyond the realms of interest in non-targeted analysis using the outer surface. Coated paperboard is also possibility back in the 1970s because the LC-HRAM (Orbitrap-based) systems, widely used; for example, in drinks cartons. technology simply wasn’t available. where the ability to gain full-scan data at Although polymers are generally inert, Substances of below 1000 daltons in accurate mass is extremely useful. high-molecular weight, cross-linked molecular weight are of particular interest, Right now, NIAS regulations are very substances that don’t migrate – the residual but can vary from simple volatile chemicals general; they simply state that not only are monomers used to prepare them can, and like vinyl chloride, acrylonitrile, vinylidene you responsible for showing compliance since it’s not possible to get a complete chloride through to complex mixtures of to the positive list of substances, you also

the Analytical Scientist The Analytical Scientist × Thermo Fisher Scientific  29

have to prove you have considered other cannot be contaminated in the process. potential contaminants, which by NIAS Indeed, all of these innovations represent definition are unknown. It’s very typical new analytical challenges. And with Webinar in the regulatory world to begin with an nanomaterials, unlike other contaminants, it indication of intention and then firm up on is not simply a case of measuring compound the detail of compliance later on. In time, concentrations – particle size and particle someone might suggest an approach for size distribution are also important. There’s providing assurance, and someone else will a good paper that uses Thermo Scientific Analytical suggest it is validated. If CEN adopts it, it ICP-MS to look at the migration of silver Challenges in will become a definitive CEN standard for nanoparticles incorporated into plastic NIAS measurement. But, of course, these chopping boards into chicken meat (1). Food Contact things take time... The regulators have to balance food Materials Right now, I would say that the industry safety (from a contaminant point of view) is largely self-policing – especially given on one hand, but on the other, limit that food control or public analysts have controls that get in the way of packaging John Gilbert worked at the Central limited resources. But that doesn’t mean innovations that are advantageous to the Science Laboratory (CSL) as research it isn’t being proactive. The big worry for producer, retailer and consumer. Indeed, director for 15 years until 2009, the food industry is a sudden scare and the it is all too easy to think negatively about when it was renamed Food and resultant damage in reputation – and there packaging when you consider substance Environment Research Agency (Fera; have been several related to packaging. migration and contaminants. But the now Fera Science Ltd). In 2009, John Photoinitiators represent a recent scare reality is that packaging has made a huge took up a teaching position at the – especially as they decompose into difference to the food chain in terms of University of Natural Resources free radicals when exposed to sunlight. extending shelf life and availability; we no (BOKU) in Vienna, Austria, and Bisphenol A is also on the list, as it can longer have to rely on locally available food at the same time, with a colleague, migrate into food from the epoxy resin products, and I would say the advantages set up a consultancy company – coating on the can or from polycarbonate far outweigh the disadvantages – it’s just FoodLife International Ltd (www. food containers in certain circumstances. a question of striking the right balance foodlife.com) –. John has also been I believe that in due course, contract labs and using the right analytical tools and editor-in-chief of Food Additives and will offer comprehensive analysis using techniques to ensure safety. Contaminants for the past 15 years. HRAM mass spectrometry for migrating In my opinion, the push for sensitivity John has always maintained an substances from food packaging, just as they has largely ended (which was getting a interest in food contact material do for other residues and contaminants. little ridiculous in terms of identifying analysis, and chaired the ILSI miniscule amounts of anything and Europe Packaging Task Force for The future of food contact materials everything). I believe specificity is also many years, and was also involved Packaging never stands still; innovation adequate – as long as the analysis is in one of the scientific panels is continual. Take nanotechnology – the performed properly. What the food and undertaking evaluations. John also industry is looking for ways to improve the packaging industries want is the ability helped to develop packaging recycling performance of packaging with nanoclays to cover more analytes, at lower cost – and guidelines for PET, and is currently and other materials, such as nano-silver. with greater speed. And as attention turns working on a new project called There’s also a great deal going on in increasingly to non-intentionally added “Better Training for Safer Food,” active packaging, where examples include substances, we’ll see a concomitant growth which is funded by the EU, and plans ‘moisture absorbers’ used in meat trays, in untargeted analyses. run courses for inspectors of plastic ‘scavengers’ found in small sachets used recycling plants from 2016. to absorb residual ethylene or oxygen, Reference or ‘releasing systems’ that slowly release 1. R J B Peters et al., “Development and validation To watch John Gilbert’s comprehensive antimicrobial agents to extend shelf-life. of single particle ICP-MS for sizing and webinar on: “Analytical challenges in There is also interest in whether it’s possible quantitative determination of nano-silver in measuring migration from food contact to incorporate antimicrobial substances chicken meat”, J Anal Bioanal Chem 406 (16), materials” – register here: into the packaging itself. Clearly, the food 3875–3885 (2014). tas.txp.to/1015/FCMwebinar

www.theanalyticalscientist.com Thinking Forward. GPC/SEC Theory or

PSS are world leaders in macromolecular characteri- practice? zation and have the expertise to help you with your analysis requirements. We offer a range of products and services from instruction courses and training thru contract analysis, consulting, method development If there is one and qualifi cation services all the way up to supplying turnkey GPC/SEC and LC/2D systems. thing we can All this comes with the personal and direct support of our dedicated team of innovative and pioneering do, it’s both. specialists. Is there any better way of achieving your analysis goals?

Driving GPC/SEC forward

Phone + 49 6131 962390 You‘ll fi nd the ideal GPC/SEC solution at PSS under: www.pss-polymer.com [email protected] Thinking Forward. GPC/SEC Theory or

PSS are world leaders in macromolecular characteri- practice? zation and have the expertise to help you with your analysis requirements. We offer a range of products and services from instruction courses and training thru contract analysis, consulting, method development If there is one and qualifi cation services all the way up to supplying turnkey GPC/SEC and LC/2D systems. thing we can All this comes with the personal and direct support of our dedicated team of innovative and pioneering do, it’s both. specialists. Is there any better way of achieving your analysis goals?

Driving GPC/SEC forward Welcome to The Power List 2015 – our second foray into the Top 100 most influential people in the world of analytical science. Though we realize our list can (and should) never be definitive, who can argue that the faces within – both familiar and new Phone + 49 6131 962390 – do not beautifully highlight the brilliance and diversity found within our sometimes You‘ll fi nd the ideal GPC/SEC solution at PSS under: www.pss-polymer.com undervalued field? Here, we celebrate 100 reasons to be proud of analytical science. [email protected] www.theanalyticalscientist.com 32  Feature

Yoshinobu Baba Allen Professor of Physical Chemistry, Bard Department of Medicinal Chemistry, Professor, Faculty Faculty of Pharmaceutical Sciences, Director, Center for University of Tokushima, Japan. Electrochemistry, Norman Hackerman-Welch Regents Perdita Barran Research Human genome analysis, Chair, The University Professor of Mass Spectrometry, Director of functional genomics, and proteome analysis. of Texas at Austin, USA. the Michael Barber Centre for Collaborative Mass Spectrometry, University of Research Electrochemical methods Manchester, UK. applied to chemical problems, conducting investigations in electro- Research Gas-phase ion chemistry and organic chemistry, photoelectrochemistry, the application and development of mass electrogenerated chemiluminescence, and spectrometry for complex chemical and electroanalytical chemistry. biological problems.

Lutgarde Marc Casper Buydens President and Chief Executive Paul Bohn Professor and Head, Analytical Officer Thermo Fisher Scientific, Arthur J. Schmitt Professor of Chemistry/Chemometrics, Radboud Massachusetts, USA. Chemical Biomolecular Engineering, University Nijmegen, The Netherlands. Professor of Chemistry and Biochemistry, Revenue: US$17 billion Director - Advanced Diagnostics & Research Chemometrical techniques for Employees: >50,000 Therapeutics Initiative, University of optimization of molecular structures with www.thermofisher.com Notre Dame, Indiana, USA. respect to (bio) chemical activity and for the processing/interpretation of (medical) Most important lesson It’s not about us – multivariate images. it’s about the students and young colleagues (courtesy of Peter Beak, UIUC). Encounters with serendipity Yes - in a Purnendu (Sandy) Dasgupta stunning pedagogical example from the Jenkins Garrett Professor of Chemistry and research lab, back in the late ‘90s. We Biochemistry, University of Texas at were injecting currents into chemically Arlington, USA. modified thin films and measuring molecular electrochemical effects on Most unexpected outcome Early in my important and what he did with the data! conduction. The whole experiment hinges career, a researcher from abroad visited Eye on the horizon Analytical science is on making µA current measurements in my lab. She had adopted a technique we simultaneously diverging in two directions: the presence of a mA (injected current) developed and, in fact, was already doing i) simpler, cheaper formats (for example, background. Fortuitously, even though far better than we had accomplished. paper-based assays) – my heart lies in this the background was 1000x larger than the Her boyfriend accompanied her and saw direction, and ii) increasingly sophisticated signal, the noise in the background was something unrelated that we were doing. instrumentation that provides heretofore 104 to 105 smaller than the background, so He said he was extremely interested in its unattained performance levels – my intellect the signal to noise ratio was respectable. implications (but delicately avoided telling admires this direction. Of course, the elusive It was the exceptional and wholly me what his program was about!) Later, I ideal is when you can combine the two, unanticipated character of the fluctuations received a fully-funded invite from him to perhaps with a completely new paradigm in the injected current (near the Johnson put up one of our trace gas measurement – in some parlance: disruptive technology. noise limit in most experiments) that instruments on a blimp for an extended Rarely is the latter merely a result of made this possible. period. Even now, I have no idea why it was systematic and methodical research.

the Analytical Scientist Andrew DeMello reaction dynamics area. At the time, he Professor of Biochemical Engineering, didn’t have funding but offered me the Institute for Chemical and chance to work with him on a new area: Monika Dittmann Bioengineering, Department of making chip-based devices to analyze Principal Scientist, R&D, Agilent Chemistry and Applied Biosciences ETH DNA. It was an incredibly fulfilling time Technologies, Germany. Zürich, Switzerland. and complete luck that I began working with microfluidic technology. Most important lesson The need for patience Most important lesson Trust the opinions Funniest moment The funniest is most and persistence. and instincts of young scientists and definitely not repeatable here! That said, Funniest moment During development an graduate students! turning round to see one of my colleagues instrument started a life of its own, throwing Encounters with serendipity I encounter (when I was student) covered from head microfluidic chips around the lab. We had to serendipity all the time. I remember to toe in two liters of rhodamine 6G in install webcams to find out what it was doing applying to Rich Mathies at Berkeley ethylene glycol (from a dye laser) did raise a at night and got some very funny videos to postdoc in the area of photochemical rather large smile. showing the robotics going crazy due to a firmware bug.

Norman Dovichi Paola Dugo Salvatore Fanali Grace-Rupley Professor of Professor of Food Head of the Capillary Chemistry and Biochemistry, Chemistry, University Electromigration and University of Notre Dame, of Messina, Italy. Chromatographic Methods Indiana, USA. Unit at the Institute of Chemical Most important lesson It is better to be Methodologies, National Research Research Developing tools to study the together than alone Council (CNR), Monterotondo, Italy. proteome with two-dimensional capillary Encounters with serendipity During my electrophoresis, coupled to either laser- masters degree, I was working on the Most important lesson Be honest in obtaining induced fluorescence or mass spectrometry synthesis of some 3-deoxyflavilium salts, results (useful in both science and one’s career). for detection. potentially useful as color additives. Only It is also very important to have great respect by serendipity, a 4-styrylflavilum cation for all. Funniest moment Back in 1991, I was with a remarkable hyperchromic effect delivering a lecture on CE and suddenly, with respect to the other 3-deoxyflavilium there was a power failure... I continued my salts was obtained. talk in the dark without any aids.

Catherine Justin Gooding Fenselau ACS Sensors Editor-in-Chief; Professor of Chemistry & Scientia Professor, ARC Australian Biochemistry, Department Laureate Fellow and founding Attila Felinger of Chemistry & Biochemistry, Co-Director of The Australian Professor, Department of Analytical and University of Maryland, USA. Centre for NanoMedicine, University Environmental Chemistry University of of New South Wales, Australia. Pécs, Hungary. Most important lesson Science progresses as a global team effort; rapid communication Most important lesson To be persistent. Most important lesson Never stop looking is critical. Eye on the horizon The sensing field is really beyond the frontiers of your specific area. Most unexpected outcome The most blossoming; there seems to be a move away Engineers, physicists, or biologists may have unexpected thing that happened to me in my from electrochemical to optical methods an answer to many fundamental problems scientific career was that I met a fellow with with nanoscale materials. For me, the really of analytical chemistry, but first you have to a big smile in the lab who eventually became exciting direction is towards digital assays understand their languages. my husband! that count single molecules.

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Christian Griesinger Davy Guillarme Director and Scientific Member, Senior lecturer, School of Max Planck Institute for Biophysical Pharmaceutical Sciences, Chemistry, Göttingen, Germany. University of Geneva, Switzerland. Detlef Günther Most important lesson Listen to your Most important lesson “We are stronger Professor, Department of Chemistry co‑workers. Don’t ignore mice since they together than we are alone”. This quote and Applied Biosciences; VP Research could become elephants. applies very well in analytical sciences, where and Corporate Relations, ETH Zurich, Encounters with serendipity When a people should work together as a team to Switzerland. co‑worker of mine – Jürgen Schleucher – attain a fixed objective. was experimenting with recently published Eye on the horizon I’m now strongly Research Trace element characterizations of pulse sequence and magnetic field gradients, involved in the analytical characterization different samples using inductively coupled he noticed that half of the scans were empty. of biopharmaceuticals, which is highly plasma-mass spectrometry (ICP-MS) and This lead to a general approach to coherence demanding for analysts and requires laser ablation-inductively coupled plasma- selection in NMR and later to theoretical a wide range of analytical techniques mass spectrometry (LA-ICP-MS). investigations that could be solved with the (electrophoresis, chromatography, mass help of the mathematician Sieveking. spectrometry, spectroscopy…). There are always new challenges to solve in this research area. Ron Heeren Co-director of the Maastricht MultiModal Molecular Imaging William Hancock Albert Heck (M4I) center, Maastricht Editor-in-Chief, Journal Chair, Biomolecular University, the Netherlands. of Proteome Research; Mass Spectrometry and Bradstreet Chair in Bioanalytical Proteomics Group, Most important lesson Have fun in Chemistry, Northeastern University, Utrecht University, the science we do. Enjoyment brings Massachusetts, USA. The Netherlands the creativity needed to solve complex problems and allows people to think Research Applying new analytical Research Technology development for without boundaries or restrictions. technology to current problems in the proteomics and structural biology. Funniest moment My daughter biotechnology industry as well as cancer unexpectedly asked me to help her on proteomics and the plasma proteome. a topic that we just proposed to the National Science Foundation (and got funded). She analyzed the hairs of her Amy Herr fellow high school students for drug Lester John & Lynne Dewar content with unexpected results on Lloyd Distinguished Professor numerous levels. Best of all, she won the of Bioengineering, University prize for best thesis of the year. of California, Berkeley, USA. Gary Hieftje Distinguished Professor; Robert and Most important lesson Thoughtful Marjorie Mann Chair in Chemistry; persistence pays off. Never give up, but and Group Leader, Laboratory for be adaptable in light of new learnings, Spectrochemistry, Indiana University, USA. approaches, and ideas. Eye on the horizon Biology and biomedicine Research Investigation of basic mechanisms are becoming more quantitative, so I see an in atomic emission, absorption, fluorescence exciting and perhaps even more central role and mass spectrometric analysis, and for the analytical sciences in tackling grand the development of instrumentation and challenges in the 21st century. techniques for atomic methods of analysis.

the Analytical Scientist Feature 35

Michal Emily Hilder Holcapek Director, ARC Training Centre Eye on the horizon I expect some Professor, Analytical Chemistry, Faculty for Portable Analytical Separation significant changes for my group in the of Chemical Technology, University of Technologies, University of Tasmania. future with my upcoming move to the Pardubice, Czech Republic. University of South Australia in Jan Most important lesson Never stop learning 2016 as the Director of the new Future Most important lesson The curiosity to new things, keep your interests as broad as Industries Institute. Separation Science understand the principles is a driving force possible and don’t be afraid to ask what you may appear to be a mature field, but there for scientists. This scientific enthusiasm is a think are stupid questions. I’ve seen many big is still plenty to be done. Developments natural attribute of any scientist. Talent must breakthroughs come from those who are able in detection technology, in particular be accompanied by hard work and patience to challenge the ‘right way’ of doing things, mass spectrometry, have already had a big to attain success. and often just because they approached the impact and will continue to demand new Funniest moment By far the most fun can problem from a totally new perspective. separation technologies. be encountered during the examination of students. The winning answer: the nucleus of a hydrogen atom contains half of proton and half of neutron, because the nucleon number is equal to one. Pavel Jandera Eye on the horizon The field of lipidomics is Gérard Professor, Department of growing and will continue to do so, because Hopfgartner Analytical Chemistry, Faculty lipids are connected to many biological Professor in Analytical Sciences and Mass of Chemical Technology, processes, including those associated Spectrometry and Head of the Mass University of Pardubice, with disease. Spectrometry Platform of the Sciences Faculty, University of Geneva, Switzerland. Most important lesson It is impossible to avoid mistakes when searching for new Elizabeth Holmes Research Bioanalysis, metabolism, solutions to problems; I cannot count mine. CEO and Founder, miniaturization of sample preparation, multi- However, the failures may be very useful and Theranos components analysis, ultra-high throughput and we often can turn them into an advantage. high sensitivity analysis, as well as studies on the Company valuation: US$ 10 billion rationalization of fragmentation mechanisms (tas.txp.to/1015/Theranos) for the identification of metabolites. www.theranos.com Sitting Down With interview: tas.txp.to/1015/Hopfgartner Klavs Jensen Michael Warren K. Lewis Professor Joseph (Jack) Laemmerhofer of Chemical Engineering, Kirkland Professor, Pharmaceutical and Professor of Materials Vice-President, Research and Analysis and Bioanalysis, Science and Engineering, Development, Advanced University of Tuebingen, Germany. Massachusetts Institute of Materials Technology (AMT), Technology, USA. Delaware, USA. Most important lesson Research demands hard work, persistence, and stern discipline Research Understanding and controlling Most important lesson During my R&D to pave the way for success. In this endeavor, the interaction of reaction and transport career, the most important lesson learned ambition to make small achievements processes in the realization and testing of is perseverance. This is a needed quality if represents a useful motor. functional micro- and nano-structured difficult problems are to be solved. Along Encounters with serendipity In biomarker materials and devices for chemical, with perseverance, patience is required, and analysis, serendipity happens all the time; biological, optical, electronic and that was difficult for me to accept molecules that you weren’t looking for often energy applications. and develop. pop up – the hope is that they are real...

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Frank Laukien Hian Kee Lee Chairman, President and Chief Executive Professor, Department of Chemistry, Officer, Bruker Corporation, Germany National University of Singapore.

Revenue: US $1.84 billion (2013) Most important lesson A few lessons, Employees: >6000 actually: Not to be deterred by setbacks, www.bruker.com have a sense of humour, cherish the support of the family and the friendship of about his family. Of his father, he wrote: colleagues, be grateful for the opportunity, “Daddy is a professor in the university, he’s Milton Lee and to students, and never stop learning learning to be a scientist.” Which basically H. Tracy Hall Professor of (see next item). sums it up. Chemistry, Department of Funniest moment When our son was in Eye on the horizon More focus on Chemistry and Biochemistry. his first year of primary school, he was automation and onsite applications: Brigham Young University, Utah, USA. asked by his teacher to write something “The environment is your lab”.

Research Development of new instrumentation and supporting technology in the fields of capillary and micro/nano Susan Lunte Mike MacCoss fluidic separations and mass spectrometry. Ralph N. Adams Distinguished Michael MacCoss, Professor Professor of Chemistry and of Genome Sciences, Pharmaceutical Chemistry; Department of Genome Director, Adams Institute for Sciences, University of Bioanalytical Chemistry, The Washington, USA. University of Kansas, USA. Most important lesson Be persistent Research Microanalytical methods for and consistent. Alastair (Ally) Lewis the investigation of the transport and Funniest moment Becoming a tenured Professor, National Centre for metabolism of peptides across the blood- professor from the same department that I Atmospheric Science, University of brain barrier; separation-based sensors was rejected admission for graduate school. York, UK. employing on-line microdialysis coupled to microchip electrophoresis; Cell-based assays Most important lesson Analytical science on chips; and microchip-based diagnostics is amazingly broad, innovative and for cardiovascular and metabolic diseases. flexible, so that someone, somewhere, has probably already solved your problem (even if they don’t yet know it). Encounters with serendipity In 1993, I had a chance encounter with John Phillips who described a new method called GC×GC. I subsequently managed to build the best part of a career out of his technique by applying it to atmospheric and pollution science. Fasha Mahjoor Funniest moment It’s strange that Founder, President, and Chief Executive different countries deliver gases in Officer, Phenomenex, California, USA different colored bottles. I once spent a week trying to light an FID in Portugal Revenue: unlisted Ron Majors that was fed with nitrogen rather than Employees: >700 Retired, former Senior Scientist Agilent air. I never even thought to ask. www.phenomenex.com Technologies, Delaware, USA.

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Andreas Manz Head of Research, Korea Institute of Science and Technology (KIST), Saarland University, Saarbrücken, Germany.

Research Lab on a chip, microfluidics, Matthias Mann miniaturized total analysis systems Director, Department of Proteomics and (microTAS), biomimetic microfabrication, Signal Transduction, Max Planck Institute clinical diagnostics and the Human of Biochemistry, Munich, Germany Document Project. Alan Marshall Professor of Chemistry and Director, Research Developing and applying methods National High Magnetic Field of mass spectrometry-based proteomics in a Laboratory ICR Program, Florida State variety of biological areas. David University, USA. McCalley Professor in Research Continuing development of new Hans Maurer Bioanalytical theory, techniques, and analytical/biological/ Full professor, Toxicology Science, University of environmental applications of Fourier and Pharmacology; Head, the West of England, UK. transform ion cyclotron resonance (FT-ICR) Department of Experimental & mass spectrometry. Clinical Toxicology, Saarland Most important lesson The communication University, Homburg/Saar, Germany. skills of scientific researchers are inversely proportion to their intelligence. Michael (Mike) Most important lesson If you have a new Funniest/most unexpected moment Being McMullen scientific idea, don’t wait for funding – start mistaken for “Mr. Bean” on my first visit to President and Chief directly with your available resources. Japan to attend a scientific conference. And Executive Officer, Most unexpected outcome I received a fax being amazed that 99 percent of the citizens Agilent Technologies the day before Christmas 2006, informing of Kyoto could actually understand the basic me that the Rector of the University of Japanese that I had learned but (perhaps Revenue: US$4 billion Ghent in Belgium would be presenting me unsurprisingly) disappointed that I could not Employees: ~12,000 with an Honorary Doctorate. understand 99 percent of their responses. www.agilent.com

Chad Mirkin Encounters with serendipity I was at the Director, International ISCC meeting in 2006, and together Institute for Nanotechnology; Luigi with my co-worker Peter Tranchida, we George B. Rathmann Professor, Mondello showed the benefits (in terms of resolution) Chemistry; Professor, Chemical Full professor of using a split-line in comprehensive and Biological Engineering, of Analytical GC experiments to Leonid Blomberg. Biomedical Engineering, Materials Chemistry Chemical, Leon took a look at the data (later Science & Engineering, and Medicine. Biological, Pharmaceutical, published in Anal. Chem. 2007, 79, Northwestern University, Environmental Sciences 2266-2275) and immediately made the Illinois, USA. Department, University of following observation “...apart from Messina, Italy. the split line, there must be some other Research Anisotropic nanostructures, factor contributing to such a great gain in on-wire lithography (OWL), dip-pen Most important lesson Always love what resolution”. He was right. But it took us nanolithography, organometallic chemistry, you are doing; only with enthusiasm and about six years to find the other factor (J. spherical nucleic acids. hard work can you reach recognition. Sep. Sci. 2013, 86, 212-218).

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Royce Murray Michel Milos Kenan Professor, Chemistry The Nielen Novotny University of North Carolina, USA Professor, Special Chair on Distinguished Professor Emeritus, Analytical Chemistry at Adjunct Professor of Medicine, Research Electrochemistry, molecular Wageningen University; Principal Director of the Institute for design, sensors. scientist, RIKILT Wageningen Pheromone Research, Director of the UR, Scientific director of COAST, Novotny Glycoscience Laboratory, Amsterdam, The Netherlands Indiana University Bloomington, USA. Christopher O’Connell Most important lesson Think outside of the Research Improving resolution of complex President and Chief Executive box (“what if?”), the impossible is possible! biological mixtures and identification of the Officer, Waters Corporation, Most unexpected outcome In the late eighties, separated compounds through techniques Massachusetts, USA. we tested professional kites for their ability to such as electrospray mass spectrometry carry air samplers in a weekend trial. All kites (MS) and matrix-assisted laser desorption/ Revenue: US$1.99 billion (2014) crashed – but how to tell the boss? ionization MS. Employees: ~6,000 www.waters.com

Most important lesson I have learned that it is always best to try to help other researchers when they need help to solve a problem – it always pays off with future opportunities and collaborations, as well as lifelong friendships. Most unexpected moment As a summer Colin Poole student in an analytical lab, I was asked to Professor, Department of help the police investigate a case. A man Chemistry Wayne State University, believed his wife was trying to kill him – Michigan, USA. and claimed his vermouth tasted “funny”. Michael Quilliam I discovered that the drink was adulterated Most important lesson Patience. Principal Research Officer, Biotoxin with N,N-diethyl-m-toluamide, more Laboratory work takes time and hustling Metrology, Measurement Science and commonly known as DEET – the insect does not get it done any faster. Standards, National Research Council, repellent. Apparently the wife thought her Encounters with serendipity While Nova Scotia, Canada. husband was a real pest! waiting to talk to the Dean I casually picked up a magazine that contained a short article suggesting that ethylammonium nitrate had Susan Olesik Jeanne physicochemical properties that Dow Professor and Chair, Pemberton resembled water. It proved to be far Department of Chemistry Professor, Chemistry, from the truth but commenced a 35- and Biochemistry, Ohio State University, USA. The University of year investigation into the synthesis and Arizona, USA. characterization of ionic liquids in my Most important lesson Hard work always research group. pays off. Research Chemistry at interfaces in Most unexpected outcome Presenting Eye on the horizon My group intends to electrochemistry and electrochemical a 45-minute lecture without visual aids contribute strongly in advancing the speed devices, chromatography, organized or access to a blackboard because of a of analysis using separation science and molecular assemblies, and projector failure. mass spectrometry. environmental systems.

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future for my research group because Pier Giorgio analytical atmospheric chemistry (with Righetti very good knowledge of separation science Full professor, Department .Marja-Liisa Riekkola and mass spectrometry) offers an excellent of Chemistry, Materials and Professor of Analytical Chemistry, Head basis for the development of new sampling Chemical Engineering, of the Laboratory of Analytical Chemistry, techniques, portable instruments and Politecnico di Milano, Italy. Department of Chemistry, University of other equipment to tackle fundamental Helsinki, Finland. climate change issues. In addition, Research Proteomics, combinatorial peptide the same expertise helps to develop ligand libraries, biomarker discovery, cancer Most important lesson Believe in your new miniaturized systems for human research, red blood cell pathologies, allergen scientific ideas and instincts, and take biomolecule studies. The topics mentioned discovery in food stuffs, cerebrospinal advantage of opportunities when offered. are so important and actual that I do not fluid analysis. Look rather into the future than into see any major problems in getting funding the past. although the economic situation is Eye on the horizon I see very positive getting worse. Gerard Rozing Technical Consultant, Rozing.com; Scientific Fred Regnier Advisory Board member, John H. Law Advanced Electrophoresis Distinguished Professor Solutions, Germany. of Chemistry, Purdue University, Indiana, USA Encounters with serendipity Serendipity occurs in our environment naturally and is part of it. Grabbing the unexpected potential to perform liquid chromatography in a CE capillary and instrument (capillary electochromatography) is an example from my Alison Rodger own career. Nevertheless, not all discoveries Professor, Head of make it – if asked for a “killer application”, Department of Chemistry, Peter Roepstorff an inventor or engineer will find it difficult to University of Warwick, UK. Professor, Department of Biochemistry and answer since the technology is new. Molecular Biology, University of Southern Research Biomacromolecule structure Denmark, Denmark. and function including DNA, membrane Frantisek (Frank) Svec proteins and fibrous proteins including Research Development of methodology for Lead Scientist; Facility director application to bacterial cell division. mass spectrometric protein analysis with at the Molecular Foundry, Intermolecular interactions. Developing focus on post-translational modifications Lawrence Berkeley National new polarized spectroscopy techniques for including protein oxidation as function of Laboratory, California, USA; Short-term biomacromolecules. Particular expertise in aging and also the use of mass spectrometric Principal Researcher, Beijing University circular and linear dichroism, fluorescence. protein analysis in the biotechnological and of Chemical Technology, International pharmaceutical industry. Research Center for Soft Matter, China.

Wilhelm Schaenzer Most important lesson Be patient. Good Head, Institute for Hamish results do not occur overnight. Also, wide Biochemistry, German Sport Small ranging teamwork is imperative. University Cologne, Germany. Retired Chemist/Research Encounters with serendipity Audaces fortuna Scientist, Dow Chemical, iuvat (fortune favors the bold); one must be www.dopinginfo.de Oregon, USA. prepared to discover something new.

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Koichi Tanaka Core Researcher/General Manager, Koichi Tanaka Laboratory of Advanced Science and Technology, Shimadzu Corporation, Japan.

Zoltan Takats Research Developing next-generation ultra- Professor of Analytical Chemistry, high-sensitivity mass spectrometry systems Department of Surgery & Cancer, to contribute to medical and pharmaceutical Faculty of Medicine, Imperial College fields, and a wide range of other sciences London, UK. and technologies. Nobuo Tanaka Research Ambient mass spectrometry. Professor Emeritus, Kyoto Institute of Technology, Japan.

Sarah Albert van Trimpin der Berg Associate Professor, Teruhisa Ueda Professor, MIRA and Department of Chemistry, President & CEO, MESA+ Institute, Wayne State University, Shimadzu Corporation, Japan University of Twente, Michigan, USA. The Netherlands. Revenue: ~US$2.63 billion (2014) Research Developing a fundamental Employees: ~10,800 (2015) Most important lesson That research is full understanding of a newly discovered process www.shimadzu.com of hurdles... but also unexpected bypasses! that brings into question what is currently Keep your eyes open for the unusual. taught relative to ionization methods in Encounters with serendipity The awarding mass spectrometry. of the Dutch Spinoza prize opened a new world of science for me – and also a totally unanticipated collaboration with a migraine expert and a mathematical expert on Jean-Luc Veuthey tipping points. Professor, School of pharmaceutical sciences, University of Geneva, Switzerland.

Most important lesson The importance of the scientific collaborations between colleagues from different domains to achieve relevant results. Most unexpected moment My nomination as techniques for these complex compounds. a full professor while I was a young scientist The size of the group will remain the same Joseph Wang working in a pharmaceutical company. but we must begin new partnerships with SAIC Endowed Chair, Distinguished Eye on the horizon We will not modify the industry, especially to face the analytical Professor, Chair of Nanoengineering, our main area of research (development challenge of biopharmaceuticals. University California San Diego, USA. of separation methods dedicated to I see the development of new stationary pharmaceutical compounds), but the phases in LC for increasing analytical Most important lesson Keep up the creativity importance of new biopharmaceuticals performance (for example, monolithic and passion! will certainly increase in the coming years, materials, pillar array) and the Eye on the horizon We will endeavor to be at inducing the implementation of new miniaturization of equipment. the cutting edge of analytical research.

the Analytical Scientist Nicholas Most important lesson Depressingly, I’ve Winograd found that persistence matters more than Evan Pugh Professor of Chemistry. inspiration (though inspiration helps!). Department of Chemistry. Most unexpected outcome That my career Penn State University, USA happened at all... Eye on the horizon Now is undeniably Most important lesson Perseverance. Don't the best time in all of human history to follow the crowd. be an analytical scientist given the speed Funniest/most unexpected moment Funny Ian Wilson and power of the technologies available events are usually provided by the students – Professor, Chair in Drug Metabolism and to us. The only problems are the expense like hooking up a vacuum pump backwards. Molecular Toxicology, Department of of modern equipment and the difficulty The most unexpected thing was winning the Surgery & Cancer, Faculty of Medicine, of thinking up good enough questions to Texas Instruments prize in 1984. Imperial College London, UK. answer with them. Eye on the horizon I have been at this for 45 years; it is time to let the younger researchers take over. Analytical sciences, since they depend heavily upon exponentially growing Kurt Wuthrich technology, has a terrific future... Professor of Biophysics, Institute of Molecular Biology and Biophysics, Zürich, Switzerland; Guowang Xu Cecil H. and Ida M. Green Professor Director for Metabonomics of Structural Biology, Scripps Research Research Center, Dalian Institute, California, USA. Institute of Chemical Physics, Mary Wirth Chinese Academy of W. Brooks Fortune Distinguished Professor, Nobel Prize in Chemistry: “for his Sciences, China. Department of Chemistry, Purdue development of nuclear magnetic resonance University, Indiana, USA. spectroscopy for determining the three- Most unexpected moment From 1995- dimensional structure of biological 1997, I worked in the University Hospital Pushing the limits of LC: tas.txp.to/1015/Wirth macromolecules in solution.” Tuebingen, Germany. When I returned Research Molecular structural biology, to China, I continued researching the protein science and structural genomics. relationship between urinary metabolic Ed Yeung products and health. I didn’t know this was Distinguished Professor metabonomics until 2001, when someone of Liberal Arts and Yukui Zhang told me. Later, I found that Professor Sciences, Iowa State Member of the Chinese Nicholson defined metabonomics in 1999; University, USA. Academy of Sciences (CAS), my group had been pioneers in a brand-new Research professor of Dalian field, but I didn’t even realize! Most important lesson To be observant Institute of Chemical Physics, – often scientific discoveries are in plain CAS, China. sight but only the few who take the time to Hanfa examine the data in detail are rewarded. Most important lesson If your research Zou Encounters with serendipity I was weighing cannot meet practical needs, you will be Professor, Vice Director of various options for a thesis topic when a kicked out of the game. Biotechnology Division, and second-year graduate student was suddenly M ost unexpected moment To obtain the Vice Director of Education Committee, drafted into the army. His research project life-time achievement award at HPLC 2015 Dalian Institute of Chemical Physics, became available and I stepped right in. If not in Beijing. To be honest, I think without Chinese Academy of Sciences, China. for this turn of events, I might not have taken the support of my friends, colleagues, and up an academic career in analytical chemistry. students, I could not win this award. Research Analytical biochemistry

www.theanalyticalscientist.com 42  Feature

19 Wolfgang Lindner Professor Emeritus, Analytical 18 Chemistry, University of Gert Desmet Vienna, Austria. Professorn and Faculty of Sciences Vice-dean, Vrije Most important lesson Stay curious Universiteit Brussel (VUB), Belgium. throughout your life and don’t be afraid to enter new fields and to learn the language of Most important lesson That the joy and fun 20 these fields. By doing so, one can gain new of being in science and research is the people Richard (Dick) Smith insights that otherwise one could only dream you can work and share with – be it on a Battelle Fellow and Chief Scientist, of. Never give up and “dig deep” in science in daily basis with students (who I prefer to call Biological Sciences Division, Pacific order to meet far-reaching goals. co-workers, by the way) or cooperating or Northwest National Laboratory Sitting Down With interview: discussing at conferences with colleagues. (PNNL), Washington, USA. tas.txp.to/1015/Lindner Feature article: tas.txp.to/1015/Desmet

Most important lesson Not to be constrained by conventional wisdom, 17 and to try to think beyond the next step J. Michael (Mike) – for example, if an experiment or study Ramsey works out as hoped or expected, Scientific founder, 908 Devices; then what? Goldby Distinguished Professor Encounters with serendipity Back in of Chemistry, University of North the early 1980s, I thought it would Carolina at Chapel Hill, USA. 15 be really fantastic to couple capillary Alexander Makarov zone electrophoresis (CZE) with Encounters with serendipity I always say it’s Director Global Research Life Science Mass mass spectrometry, but there was no better to be lucky than good. I am a great Spectrometry, Thermo Fisher Scientific, Germany. real option to do so. Later, in 1984, I believer in the adage: “The harder I work, happened to listen to a talk by future the luckier I get.” Most important lesson Play fair with people Nobel Laureate John Fenn, who was Eye on the horizon Smaller, faster, and nature; with people that simply means speaking on some of his early work better, cheaper! following normal moral maxima (like “treat with electrospray ionization-MS. I Feature article: tas.txp.to/1015/Ramsey others as you would like to be treated”), for immediately wondered how CZE might nature it means that you should not try to be used with it, and ultimately developed obtain anything from it using brute force (or an ESI-MS interface that allowed this – 16 “try and see what happens”) – instead we must and actually had broader utility. In 1988, Jeremy Nicholson gain deeper understanding and modeling Fenn reported how ESI enabled the Chair in Biological Chemistry, of the underlying principles, complications effective analysis of proteins by MS for Head of the Department of and pitholes, followed by a long-term and the first time, and while everyone in the Surgery & Cancer, Faculty systematic effort to reach our goals. MS community was suddenly interested of Medicine, Imperial College Funniest moments When I started working in the approach, instrumentation was London, UK. for HD Technologies in Manchester, there lacking. We’d already published our were only few of us but it was like being a initial explorations into CZE-MS, and Most important lesson To ignore the crew in a U-boat, working long hours in a our research was able to move forward opinions of so-called thought leaders and do close proximity. Learning the great British art much faster than others in a number my own thing. of understatement was very amusing during of important new directions. Certainly Encounters with serendipity Too many times those times. As was my colleague’s inability to some luck; perhaps even serendipity! to call – I find the whole of life a continuous remember I drank tea without milk. Sitting Down With interview: series of stochastic events. Feature article: tas.txp.to/1015/Makarov tas.txp.to/1015/Smith Feature article: tas.txp.to/1015/Nicholson See page 48 for more.

the Analytical Scientist 14 Janusz Pawliszyn Professor, Department of Chemistry, University of Waterloo, Ontario, Canada.

Most important lesson I learned that it is helpful when developing new science ideas to work with scientists who share the passion for the particular research direction. Encounters with serendipity Early in my carrier I discovered the significance of concentration gradient detection while investigating photothermal effects at the electrode interface. This work eventually have a dramatic impact on the practice of devices will result in devices facilitating led to development of microfluidics systems analytical chemistry. The number of new on-site multicomponent analysis, resulting for capillary electrophoresis based on single approaches based on rapid chromatography/ in rapid diagnostic tools in hospitals, point and whole column imaging detectors. MS, direct sample preparation/MS and rapid screening methods for food quality Eye on the horizon Further development direct sample introduction/MS will grow. determinations, and monitoring approaches of mass spectrometry instrumentation will Miniaturization of MS and front end for environment.

11 fact, that prevents us from getting bored. Barry Karger Most unexpected outcome In the Human Director, Barnett Institute; Genome Project, Molecular Dynamics used a Distinguished Professor and linear polyacrylamide polymer we developed James L. Waters Chair in Analytical for sequencing by CE. They designed 13 Chemistry, Northeastern University, the instrument with a maximum column Paul Haddad Massachusetts, USA. temperature of 43 °C, which was unfortunate; Emeritus Distinguished they could have sequenced 200-300 more Professor, Australian Centre Most important lesson There are many bases per run at 70 °C. It’s an example of for Research on Separation Science, lessons learned, but perhaps the most where (not) understanding the fundamentals University of Tasmania, Tasmania, Australia. important is that science continually of a process can have a major effect. changes, and we have to change with it. We Sitting Down With interview: Most important lesson To be persistent in can’t be afraid of going in new directions, in tas.txp.to/1015/Karger your endeavors and goals, even when things are not working out the way you had hoped. Encounters with serendipity Serendipity was a common occurrence when we regularly consulted paper copies of journals rather than electronic versions. With the paper copy you sometimes encountered an article that was on the adjacent page to the one you were reading and that article then turned out to 12 be pivotal in your future research directions. R. Graham Cooks Sadly, with electronic databases you find Henry B. Hass Distinguished Professor, only what the search engine provides and the Analytical Chemistry, Purdue University, magic of serendipity is lost. Indiana, USA. Feature article: tas.txp.to/1015/Haddad

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9 8 James (Jim) Jorgenson Daniel Armstrong W. R. Kenan, Jr. Professor of Robert A. Welch Distinguished Chemistry, University of North Professor, Department of Chemistry Carolina at Chapel Hill, USA. and Biochemistry, University of Texas at Arlington, USA. Most important lesson Relax, be patient, and enjoy the journey. Most important lesson If you have Encounters with serendipity I cannot think imagination and work harder (and more of a significant instance of serendipity, which effectively) than others, you are likely to be is surprising, as I certainly feel that I have successful. Create fads rather than been very fortunate in my work. following them. Eye on the horizon It’s time for a shocking, Most unexpected outcome Most unexpected blockbuster, paradigm-shifting development was the fact that our initial work in chiral in chemical separations. Such a development molecular recognition rapidly morphed is overdue. That’s no doubt wishful thinking into a practical commercial technique on my part, but I would love to see it happen. (enantiomeric separation) that changed the Right now, I am most impressed with trends pharmaceutical industry and regulatory 10 in miniaturization. The ability to easily focus. Even more surprising was that, over Richard Zare carry (not lug) truly sophisticated analytical a decade later, billions of dollars were being Marguerite Blake Wilbur Professor in instrumentation to just about any location spent in lawsuits between generic and more Natural Science, Stanford University, could have amazing consequences. "mainstream" drug companies. California, USA. Feature article: tas.txp.to/1015/Jorgenson Sitting Down With: tas.txp.to/1015/Armstrong

Most important lesson Expected results are Funniest moment The funniest thing I ever pleasing, but unexpected results are much came across was the most-sensitive LC more interesting. Of course, the correct detector ever - the Post-column Explosion application of analytical science requires that Detector (it was meant to be a post-column- most of our experiments are performed in reaction detector, but the reaction was a bit a repeatable manner. However, in scientific too fast.) It worked only for one peak (and research, unexpected results herald progress. after rebuilding, one more peak, so it proved Encounters with serendipity My best repeatable). The details of this highly exciting unplanned project came about on the way experiment in Barry Karger’s group were, back from Vienna from a conference. A unfortunately, never published. Philips plane was returning from Vienna Eye on the horizon My field, analytical half empty, and I got rescheduled from an separations, is far from mature. There is airline flight to the company plane. At the a great need for better separations of all time, I was interested in artificial intelligence kinds of complex mixtures – and we need – we were working on expert systems – and breakthroughs to fill these needs. My group I bumped into Frans Sijstermans (who was is in a good position because we have three 7 similarly rescheduled) and found out that he candidates for the next “Top 40 Under Peter Schoenmakers was into parallel computing. We got some 40” Power List; we need excellent young Education Director COAST; Editor, manpower from Lutgarde Buydens’ group in scientists to bring the field further. Indeed, Journal of Chromatography A; Professor, Nijmegen, used half of the nodes in a parallel the Top 40 under 40 is perhaps more Analytical Chemistry/Forensic Science, computer (without anyone noticing), important than The Power List... van't Hoff Institute for Molecular Sciences, and obtained really nice results on Sitting Down With interview: University of Amsterdam, The Netherlands. neural networks... tas.txp.to/1015/Schoenmakers

the Analytical Scientist 6 John Yates III Ernest W. Hahn Professor, Chemical Physiology and Molecular and Cellular Neurobiology, The Scripps Research Institute, California, USA.

Most important lesson Tenacity is most important. Encounters with serendipity Maybe, but there have been many more “aha” moments. One of the first was when I first tried to search tandem mass spectra through a set of sequences and it worked well. I expected it not to work. Most unexpected moments It’s always interesting to see famous people on airplanes. I was once flying to Germany on a business class ticket and, as I was alone, I was upgraded to first class and ended up sitting 4 that most of the PCBs were adsorbed on behind the actor Nick Nolte. I’ve sat next to Pat Sandra the Teflon stir bar used in the experiment. G. Gordon Liddy of Watergate fame and Emeritus Professor, Organic Chemistry, Within a minute, we came up with across the aisle from the US Supreme Court Ghent University; Founder and President, the idea to coat stir bars with PDMS, justice John Paul Stevens on flights. For the Research Institute for Chromatography, resulting in a very sensitive new sample Star Trek fans, I was once on a flight with Kortrijk, Belgium. preparation method. Thousands of stir Seven of Nine... bars, commercialized as Twister, have been Eye on the horizon I expect there to be a Most important lesson Never go in sold since that time. push to make proteomic technology better (scientific) competition with colleagues or Most unexpected moment By far the so that it can tackle increasingly complicated organizations that are stronger or have more most unexpected thing that happened problems – in particular, I think proteomics possibilities than yourself... try to collaborate. – and which was, in the end, of utmost needs to develop a capability for massively Encounters with serendipity Stir bar importance in my career development parallel analyses. sorptive extraction was invented (by – was the Belgian dioxin crisis in Feature article: tas.txp.to/1015/Yates accident) through a controversial 1999. I was able to prove the link discussion in the literature on the between dioxins present in our food absorption–adsorption properties and contamination with transformer of polydimethylsiloxane (PDMS). oil or polychlorobiphenyls (PCBs). The 5 Our observations on the partitioning result was that analysis of food could be George mechanism between water and PDMS restricted to PCB analysis rather than Whitesides were called into question. Solid phase the very expensive, time-consuming and Woodford L. and Ann microextraction with a PDMS fiber ultra-trace dioxin analysis via capillary A. Flowers University of polychlorobiphenyls spiked in water gas chromatography hyphenated to high- Professor, Department of indicated that adsorption was taking resolution mass spectrometry. Just imagine Chemistry and Chemical Biology, place because the log P value controlling more than 50,000 samples being analyzed Harvard University, Massachusetts, USA. the PDMS/water distribution was by the latter technique! not followed. However, repeating the Sitting Down With interview: Feature article: tas.txp.to/1015/Whitesides experiment, we came to the conclusion tas.txp.to/1015/Sandra

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Most important lesson I think one of the three consecutive summers. Had I not most important lessons I haven’t learnt gone there, I may have ended up doing is how to say “no” to the many requests I something completely different. Most receive. I do try, but it never seems to work people could say something similar, and for me. My colleagues and friends tell me I think that I got to where I am now I do too much – but I think it’s simply through random events and mentorship that I have too many things on my plate. by great people like Richard Zare and However, one of the important things I Richard Scheller at Stanford University. have learnt is that I will pick important but I see people like them as the hallmark for difficult research goals and I keep moving the rest of my career. Research is different towards them no matter the intervening though and I don’t think serendipity has challenges or obstacles, which clearly much of place; I consider research to be a keeps me on target. continuous effort to solve problems. Encounters with serendipity I didn’t Eye on the horizon There are a number expect to become editor of Analytical of areas that are getting a lot of press Chemistry. The job fell into my lap without attention and are obviously important; 3 any advanced thought or preparation – it for example, the integration of various Jonathan Sweedler just happened! I’m really enjoying the job, techniques with nanoscience, portable Editor-in-Chief, Analytical Chemistry; although it takes up a lot of my time. analysis through microfabrication, James R. Eiszner Family Endowed Chair My whole career is really just a collection the advances in mass spectrometry in Chemistry and Director of the School of of what seem to be fairly random events. instrumentation, and informatics driving Chemical Sciences, University of Illinois at My passion for analytical chemistry was new types of analysis. And then there’s the Urbana-Champaign, USA. ignited by working at the LBNL for big data problem...

2 pushed out of the lab by the quality of Robert (Bob) Kennedy my own student’s work. I specifically Hobart H. Willard Distinguished remember showing Lan Huang, one of University Professor of Chemistry, Chair of my first students, how to use an electrode Chemistry, College of LS&A; Professor of we had developed to measure insulin Pharmacology, Medical School, University secretion from single cells. I managed of Michigan, USA. to get a few puny signals from the cells. Lan worked on it over the weekend and Most important lesson The most on Monday morning she said something important product of my research is not like, “I don't think I'm doing this right. my papers or patents but trained people Here is what I got.” And of course she who can go off and achieve what they had beautiful signals. They were so much want to achieve. better than mine that she thought she was Another practical lesson is that there is doing something wrong. That was it for no such thing as an “easy” starter project. me in the lab. I used to think that it was good to have Of course, we’ve had many funny things people start on projects that eased them happen in the lab and at conferences over that it was drawn 1:10 scale. We received a into doing research, but actually those the years. One amusing “Spinal Tap” perfect miniature box, complete with little took just as long as the more ambitious moment happened when my student hinges and latches. The craftsmanship was sounding projects. So now we just start on Zech designed a light-tight box to cover excellent – if only it had been the right what we really want to do. a laser induced fluorescence detector he size. I'm not sure how they thought this Funniest moment I'm not sure it is funny, built. He sent the order to our shop but would hold a complete LIF detector... but I was stunned at how quickly I got apparently they didn’t get the message We Sit Down With Bob Kennedy on page 50.

the Analytical Scientist Feature 47

1 the opportunity to recruit the first group then the labor law in Switzerland demands Rudolf (Ruedi) Aebersold members with a computational background that I retire. Deputy Head, Department of Biology, from the Institute for Systems Biology in I think that my field will continue to rapidly Institute of Molecular Systems Biology, Seattle. They have transformed our work, the grow in size and significance because ETH Zurich, Switzerland. group structure, and our research approach. we finally have very robust proteomic Most unexpected outcome I was trained as technologies to learn new biology and make Most important lesson Understanding the a cell biologist at a time when computers headway in the translational arena. I see importance of the research environment, did not really matter in biology. So perhaps a broader dissemination of proteomics, specifically the colleagues around you, which the most unexpected outcome is that outside the traditional proteomics groups includes your immediate lab group, but also some of the significant achievements of and I see a significant development of the scientists in the broader environment. our group are algorithmic/computational. computational and data management Great colleagues are an inspiration, judges The early computational work was based systems in the cloud, further democratizing of ideas, a resource for innovation – and they on urgent needs and serendipity. We large-scale proteomics. make work pleasant and fun. recognized the demand for new algorithms In general, I think that the current tough Encounters with serendipity I never really for data analysis and we were able to funding climate will favor advances in had a master plan for my career. Great job recruit, largely through the philosophy analytical sciences that can demonstrate opportunities came about from unexpected at the ISB, a terrific initial cadre of a relatively timely impact via their angles and new lab members brought computational scientists into our group. application to urgent problems. ideas or skills that greatly enriched our Eye on the horizon I will continue to work research portfolio or drove our research in with my relatively large group of around Sitting Down With interview: new directions. Such an occurrence was 30 members for another four years, but tas.txp.to/1015/Aebersold

www.theanalyticalscientist.com 48  The Analytical Scientist × Thermo Fisher Scientific

™ Amelia Peterson (from the Coon Orbitrap : Ten Research Group) came to the Thermo Scientific research lab in Bremen, Germany Years Young to continue work on the GC-MS-LTQ Orbitrap instrument and, on her return Coupling gas chromatography to UW-Madison, presented several with Orbitrap™ technology applications in high-impact journals. wasn’t easy, but the outcome Although the projects were only exploratory – the introduction of the in nature, they proved invaluable in allowing Thermo Scientific Q Exactive™ us to gauge interest in GC-Orbitrap GC – represents a big step technology – and a number of customers towards bringing full-scan, began asking for more information. high-resolution, and accurate mass data into routine labs An essential confluence around the world. And my In reality, we were not able to dream of an “Orbitrap in every communicate any fixed date about GC lab” inches ever closer. Orbitrap technology to our customers. begin in earnest. At which point, the ball We needed to fully assess what was started rolling very quickly. By Alexander Makarov, Director, Global needed in the market and put together an Research Life Science Mass Spectrometry, entire development team – and Orbitrap What Orbitrap technology means for Thermo Fisher Scientific, Germany. technology was still not ready for GC. GC – and vice versa Over the next few years, information At ASMS 2015, exactly 10 years after We started thinking about GC Orbitrap was gathered and the potential became the introduction of the LTQ Orbitrap technology a long time ago – very soon clearer – but, more importantly, Orbitrap system, we launched the Q Exactive GC after the dust had settled following the technology development continued. – an excellent way to celebrate Orbitrap’s launch of the first commercial instrument By 2011, we had increased the speed anniversary. What does Q Exactive at the June 2005 ASMS Conference of the Orbitrap by a factor of four, by GC offer the world of GC-MS? The in San Antonio, Texas – the LTQ combining two innovations: i) enhanced real breakthrough is the combination of Orbitrap tandem mass spectrometer. Fourier transform algorithms, which accurate mass with high sensitivity. Imagine But back then it was clear that one or doubled resolving power, and ii) the a triangle of mass accuracy, sensitivity two second peaks were too narrow for the high-field “compact Orbitrap” (where an and speed – traditionally, optimization of wide application of Orbitrap technology increase from 3.5 kV to 5 kV boosted mass accuracy comes at the sacrifice of the in GC. Nevertheless, Joshua Coon (a frequency by 20 percent and the smaller other two factors. Instruments that were professor at the University of Wisconsin- trap provided a factor of 1.8 increase in not constrained by mass accuracy – triple Madison) expressed an interest and we speed.) Finally, we had an Orbitrap quadrupoles, for example – were far ahead initiated a research project to look at the analyzer that was completely compatible of the game in terms of sensitivity and potential. Originally, the project was with GC separations. At the same time, speed. On the other hand, the only accurate simply a continuation of the mainstream a talented development team became mass instruments – time-of-flight systems work in his lab, which focused on electron available in Austin, Texas, which could – suffered from a severe compromise in transfer dissociation (ETD) for the LTQ take on the not insignificant challenge other features. In other words, the size of Orbitrap instrument. At that time, ETD of giving GC its first new mass analyzer the triangle is limiting. Orbitrap technology utilized anions that essentially came in half a century. expands the triangle so drastically that we from the ion source of a GC quadrupole Without these streams coming can now match the speed and sensitivity system, and so the connection was together, we could not have moved of triple quadrupoles, but at the same time relatively straightforward. Indeed, the forward; the confluence of user demand, provides high mass accuracy and resolution. work resulted in the first rudimentary increased Orbitrap capability (in terms Since its launch, I’ve been pleased to GC Orbitrap system. The initial data of speed, sensitivity, mass accuracy and see an extremely enthusiastic reception to proved that there was high potential, but selectivity), and the necessary resources the Q Exactive GC from the community. also indicated some challenges. gave us the critical mass we needed to People are excited to learn how their

the Analytical Scientist Next Generation GC-MS  49

samples behave; we’ve already shared science applications. For me personally sector instruments, are still leading in stories from Hans Mol in pesticide that means a lot, because I believe that those areas where they confer a distinct analysis, Karl Burgess in metabolomics, the combination of easy mass accuracy advantage – and there are probably more and Jana Hajšlová in food authentication and sensitivity could benefit many other magnetic sector instruments produced in this article series – and I think there types of analysis – we just need to look today than 30 years ago. Yes, we will see will be many more interesting stories to further into where unique advantages can expansion and contraction of market share, be told as the technology is adopted in be gained. but each will retain its own niche – and it labs around the world. We also learned a lot in the really depends how attractive those niches GC is an interesting addition to development process, for example, how are. Certainly, LC and GC applications Orbitrap technology as it combines high to reduce or completely eliminate ion are growing rapidly, with thousands of resolution GC separation (with its large molecule reactions, which were not instruments worldwide, so this area often peak capacity) with the high resolving present in electrospray produced ions, gets all the limelight – and here I expect power (and mass accuracy) of the but were visible for ions produced by Orbitrap technology to continue expanding Orbitrap mass analyzer. The combination electron impact ionization. And we at a higher rate than other analyzers. allows us to look deeper into the volatile have now adopted a modular approach Why? Because it is fundamentally simple and semi-volatile end of the analytical – the Orbitrap is one module that can technology; it uses three electrodes with one spectrum than we have done before – be combined with a number of different voltage and its data system is a conventional and with high clarity. Moreover, classical front-end modules (ion sources). And PC. As a result, it has the potential to be GC-MS with electron ionization reduces excitingly, we now have two product competitive to quadrupole instruments in the need for MS/MS analyses, making development lines – one for LC and one terms of investment. straightforward full scan a routine for GC. Though the Q Exactive GC is an We’re not quite there yet – after all, we mode of operation, without losing vital important milestone in Orbitrap history, are working at the edge of what humanity fragment information. rather than considering that it completes can provide in terms of electrode Indeed, we were surprised how far the story, I like to believe that it is the accuracy and electronics stability – but simple full-scan MS analysis could beginning, with more expansion ahead. the simplification trend has already take us, using a combination of spectral begun; for example, if you consider the library matching (with the vast, Orbitrap trajectory evolution from LTQ Orbitrap with five commercially available nominal mass I can foresee several different trajectories turbomolecular pumps to Q Exactive libraries) and high resolution-accurate for Orbitrap technology; for example, with two, you can see the tendency to mass filtering. Acquisition using MS/ analysis of aerosols and other ion sources. use acquired knowledge and advances MS is still important, but is typically And we have even discussed the potential to decrease complexity and increase used with chemical ionization mode of sending Orbitrap technology into space accessibility. Another example is the in the search for further structural with various agencies – Orbitrap in orbit! introduction of the Q Exactive Focus information about a compound for Certainly, we are keen to investigate – specifically for heavy workloads in higher level confirmation – or, of course, any area where the combination of environmental and food safety – at a price to help us build an understanding of a analytical qualities that Orbitrap that is comparable with high-end triple compound that is not known and does technology provides can add real value quadrupoles. In other words, Orbitrap is not appear in libraries. The point is that, – and that takes time. But where serious on a continually shifting pathway – and I even though the technology appears to opportunities exist, we will be pushing hope that will continue for years to come. be more complex, the high resolution the boundaries of what is possible. In the end, the simplicity of the Orbitrap and accurate mass gained actually I would consider Orbitrap game- analyzer’s design will be key to the future make analyses simpler, reducing the changing or even disruptive technology – simplification of the technology – at that need for tedious method development. especially now that we’ve entered into the point, my dream of an “Orbitrap in every I think that has surprised a number of world of GC with the Q Exactive GC – lab” starts to sound realistic. experienced analysts. but I don’t think all other MS technology Clearly, Orbitrap brings something will (or should) retire just yet. If we look Video interview with Alexander very new to GC – but the innovation also back at the history of mass spectrometry, Makarov: tas.txp.to/1015/MakarovGC means that our technology is stepping even some of the earliest examples of To find out more: thermoscientific.com/ outside its more traditional setting in life hyphenated analyzers, such as magnetic QExactiveGC

www.theanalyticalscientist.com 50  The Analytical Scientist × Thermo Fisher Scientific

From there, I moved into a government A Taste of the laboratory – who paid for my education up to MSc level, and the rest is history. Other Side So much has changed since those early days. I remember when I first started doing When Richard Fussell still chromatography, we used a hacksaw and a worked at the UK’s Food file to cut and polish stainless steel tubing and Environment Research when building our own LC systems... Agency, he was the first customer to see the Thermo Why jump the fence? Scientific Q Exactive™ GC Over the years, I received quite a in action – well ahead of few tempting offers from instrument its official launch at ASMS companies – even as far back as the 2015. The latest Orbitrap™ 1980s. I was always intrigued by the innovation made him wonder prospect, but never quite attracted enough – not for the first time – if to make such a leap of faith. But when the grass was greener on the the recent opportunity to join the team other side. at Thermo Fisher Scientific ahead of the was the best we had at the time. And in launch of an exciting new addition to the the early 2000s, GC triple quadrupole Take us back to your pre-Thermo portfolio came along, the timing seemed MS systems came along, which added Fisher Scientific days... right. Why Thermo Fisher Scientific, a lot of advantages, both in terms of the I worked in government laboratories for a specifically? I honestly believed that selectivity and the signal to noise we could very long time before moving to Thermo Orbitrap technology was the best in the obtain for pesticides residue analysis. We Fisher Scientific – latterly at the Food field, so it seemed like the winning team. could suddenly analyze more pesticides in and Environment Research Agency in And that was confirmed when I visited even more difficult matrices, just because York, UK, working on a diverse range of Austin, Texas, to see the pre-launched of the extra selectivity. projects, spanning many research areas, Q Exactive GC. I was amazed; the But despite the advantages, I guess techniques and applications. Throughout performance of the instrument was almost I wasn’t alone in hoping for a full-scan those years, I very often found myself unbelievable. Aside from the technology, acquisition technique that would allow us working in close collaboration with one of the things that really impressed to capture as much information as possible. different manufacturers, helping to guide me was how open they were. We had That is possible with single quadrupole new and emerging technologies. As such great discussions – and it really felt instruments, but the problem is sensitivity an analytical scientist, I always found invigorating to be involved. Furthermore, – and the selectivity isn’t great either. it very exciting to be involved in such it was a really nice atmosphere, and it developments, contributing to advances seemed to me that I could learn a lot – not It seems the Q Exactive GC was and progress in the instrumentation we just in terms of the technology, but other highly anticipated in your field? used on a daily basis. skills as well. When you’ve worked in a Absolutely. GC Orbitrap technology My entry into the world of analytical particular environment for a long time, takes us a big step forward by essentially chemistry, which actually began in the you have to be careful that you don’t get combining the advantages of all techniques 1970s, was a little unconventional. I stale. Looking back, maybe I should have in one platform: much better sensitivity come from a working-class family of challenged myself at an even earlier stage, in full-scan acquisition mode, and electricians, carpenters, plumbers, and so but that’s just the way it worked out... better selectivity because we’ve got high on. I was never great (or perhaps interested resolution combined with high mass enough) at school and when I left, I went How has GC-MS changed? accuracy. Back in the days when we were into the building trade. I remember one I remember when GC-MS was first using single quadrupole systems, I don’t particularly nasty day in winter when my introduced into our laboratory (when it think anybody could have predicted we van broke down and I was late for my had finally become affordable enough). would get this far – that we would develop own birthday party. The very next day, I We started with GC-single-quadrupole cutting-edge instrumentation to the point applied for – and got – a job in a laboratory. MS, which had certain limitations but where it could become a routine technique.

the Analytical Scientist Next Generation GC-MS  51

Certainly, concurrent developments in constantly evolving, which increases the manufacturers will increasingly want computer science and electronics have knowledge base and reduces cost. For to screen their raw ingredients to been crucial... The first computer I used example, on the LC side we now have ensure that the whole finished product in a laboratory was a ZX Spectrum, so to the Thermo Scientific Q Exactive Focus, is consistent over time. They certainly get to where we are now, there really have which is an Orbitrap-based instrument don’t want any surprises that would been quantum leaps on many levels. intended for routine implementation at a undermine consumer confidence. more competitive price. What makes Q Exactive GC so Do you feel like instrument attractive for food analysis? What about the future of food analysis? manufactures are leading the charge? You have to remember that the whole New instrumentation empowers people Many of the potential trends I’ve indicated area of residues, contaminants, and food to do and look at things differently. It’s above would really not be possible safety has changed dramatically over already the case that labs are trying without HRAM technology – so it does the years – and there are a lot of other to combine different analyte classes in appear that in some aspects, analytical changes going on at the moment. For analytical methods; for example, looking laboratories are very much dependent on example, interest in authenticity and food at pesticide residues and mycotoxins in the development of new instruments to be integrity is burgeoning – looking at the the same analysis. Traditionally, these able to move forward in new directions. bigger picture is becoming increasingly areas have been separated; I suppose the Certainly, not everybody recognizes that important. Orbitrap technology not only laboratories become compartmentalized fact, but even if you consider something gives us the capability to look at residues – constrained by the instrumentation and as simple as the QuEChERS method, and contaminants, but allows us to tap methods available. would it really have become so successful into other aspects. A good example is the I see a future trend where, for certain without the introduction of LC-MS/MS? whisky profiling and characterization work samples, you’ll be able to look for multiple described by Jana Hajšlová last month (tas. analyte classes in the same method, And is the grass greener? txp.tp/1015/jana). or perhaps test for pesticide residues I’ve seen a lot of changes over my career at the same time as collecting data for – and many of the big ones came from How quickly will it be adopted? characterization or authentication. instrument manufacturers. I think that’s It won’t happen immediately, of course. Similarly, there is a growing interest in one of the reasons I recently decided Introduction of new technology is an looking for environmental contaminants – to make a pretty big change for myself evolutionary process. The bigger research I’ve looked at the uptake of pharmaceuticals when I joined Thermo Fisher Scientific. laboratories are often the first adopters; in plants caused by the use of treated Luckily, people from my old world still they often want to investigate the sewage effluent on land, for example. It’s talk to me, even though I’ve crossed over potential of the technology – and also surprising how many pathways exist for to the “other side”. And that’s important push extra development. The smaller labs contaminants to get into food. And let’s – I made some great friends over the years will follow. Years ago, we were one of the not forget food contact materials – John on the conference circuit and beyond. first labs to use an LC-MS/MS method, Gilbert goes into much more detail on Now, I’ve been on both sides of the and I remember giving a presentation on page 28, but it is yet another separate world fence – and I consider myself a mediator the multi-residue analysis of about 30 of contaminant analysis. The real driver for of sorts. In my current role, I can make pesticides. People couldn’t believe it could moving in this direction is the capability sure we are communicating effectively be a robust, routine technique – now of the instrumentation available. with our customers and perhaps facilitate everyone’s using LC-MS/MS. It’s hard to Another trend I see developing is the kinds of collaborations I enjoyed in believe that the same won’t happen with using full-scan instruments to detect my previous life. I’m very happy to be GC-HRAM technology. You can take markers to help food manufacturers where I am at this exciting time, and as your sample; do the quantification, the ensure product consistency from a for whether the grass is greener – well, identification – and the screening – all quality control point of view. With that would be telling... in one single analytical run. global food trade, raw ingredients come As with any new technique, affordability from many different sources and are Video interview with Richard Fussell: will be perhaps the biggest barrier. But that difficult to track. The use of chemicals tas.txp.to/1015/Fussell too will change. As Alexander Makarov varies over the world – as do the potential To find out more: thermoscientific.com/ notes on page 48, Orbitrap technology is routes of contamination. I believe food QExactiveGC

www.theanalyticalscientist.com 52 Solutions

Solutions

Real analytical problems Collaborative expertise Supercharging Novel applications Correlative Microscopy

Equipping scanning electron microscopes with Raman imaging to create a 2014 Innovation Award-winning universal microscopy solution.

By Olaf Hollricher

The problem Efforts to combine different high- resolution imaging techniques to provide the most comprehensive material property characterization are on the increase. For example, it is possible to show the structure of a sample with scanning electron microscopy (SEM) and determine its molecular composition with a Raman microscope. As these methods require separate instruments, an inevitable complication is sample transfer and re-identification of the investigated area. Is there a way to dispense with this tedious procedure and replace it with a simple – ideally, one-click – operation?

Background Correlative microscopy involves using two Figure 1. RISE microscopy investigation of a thin section of a drill core from the Äspö Hard Rock or more microscopy technologies on the Laboratory (Oskarshamn, Sweden). Top: The RISE image is a composite of the SEM (bottom right) same sample area. Over the past decade, and Raman images. The Raman spectra indicate epidote (red), plagioclase (green), and quartz the need to describe nanometer-scale (brown) as well as four additional, unspecified minerals (top right). The elemental composition of the samples in full detail has elevated the material was determined with EDX (top left: Ca, Fe, Al: grey; Si, O: orange; N: green). Bottom: importance of this combined approach. Comparing the light image (left) with the SEM image (right) of the sample reveals that the images High-performance analytical techniques look completely different though they are of exactly the same area. relevant to correlative microscopy include, Image parameters: 100 μm x 100 μm, 150 x 150 pixels = 22,500 spectra, Integration time: 0.08 sec/ among others, optical microscopy, spectrum. Sample courtesy of Christiane Heim, Geoscience Centre, University of Göttingen, Germany. SEM, atomic force microscopy (AFM), tomography, energy dispersive X-ray (SIMS). Linking the data sets enables the a more detailed understanding of the (EDX), focused ion beam (FIB) and correlation of structural, morphological material investigated. secondary ion mass spectrometry and chemical information, which provides Correlative microscopy may appear

the Analytical Scientist advantageous, but it has substantial of obtaining complete images. The technical challenges, which makes problem with only acquiring a single experiments cumbersome. Moreover, Raman spectrum is that you never know shuttling from one microscope to another from exactly which point in the SEM may affect the sample’s integrity. However, image the spectrum was taken. Even the primary problem is precise retrieval of after a flawlessly executed calibration, a sample’s area of interest, which means the focus can move due to thermal drift you have to rely on fiducial marks or and charging effects. These effects can feature recognition. Both procedures are easily result in a displacement of 5 µm or painstaking and time-consuming. more; a distance greater than generally Integrating multiple technologies acceptable in correlative studies. in a single platform to create a hybrid However, now we can overlay an image system has been a distinct step in the linking measurements precisely and right direction. For inspecting biological reliably, and this provides an expedient samples, for example, the combination of method for alleviating drift. fluorescence microscopy and SEM has proven useful. In materials science and The solution geology, however, different combinations One day Jaruslav Jiruse, head of R&D of optical microscopy with AFM, SEM at the SEM manufacturer Tescan (Brno, and EDX are popular. Czech Republic) called me to ask if SEM is a very powerful technique for WITec would participate in developing investigating almost any sample that a “universal SEM” that combined several can endure a vacuum environment and different analysis techniques with the it is able to zoom continuously from a imaging capabilities of SEM. The field-of-view up to 100 mm in diameter potential of Raman in combination with down to a resolution of approximately SEM was immediately apparent to me, 1 nm. Despite its extremely high so I was more than happy to agree to the resolution it also has a remarkable collaboration (especially given our strong depth-of-field, giving images that track record in correlative microscopy; have great clarity and 3D texture. for example, our Raman-AFM product SEM, however, does not reveal the was introduced in 2003). In April 2012, composition of a sample and, therefore, we officially began our three-year project EDX is often incorporated to identify (UniverSEM) funded by the EU within elemental constituents. Although the FP7 framework. useful, EDX cannot offer insight into Russian novelist and historian the arrangement and coordination of the Aleksandr Solzhenitsyn once said, “The detected atoms and their chemical bonds solution is always simple, one must only – that particular characterization is best find it”. His words are so pertinent to accomplished with Raman spectroscopy. research and development – and they Every compound has a unique Raman made us think carefully about the spectrum, thus displaying “chemical challenges we were about to face when fingerprints” within the investigated combining SEM and Raman microscopy. material. This method is non-destructive Firstly, during SEM imaging the and doesn’t require labeling or other secondary electrons scattered from sample preparation. the sample are detected by extremely Although a combination Raman/SEM light-sensitive photomultipliers, which product was already available, it could are incompatible with the bright lasers only perform Raman measurements at required for Raman imaging. Clearly, individual points and wasn’t capable we could not apply the techniques 54 Solutions

2014 just two years after the project was accepted for funding by the EU. As the SEM and Raman components are essentially two systems using the same vacuum chamber, we didn’t have to make any compromises regarding the respective imaging capabilities. The microscope achieves a lateral resolution of 360 nm and acquires complete Raman images with tens of thousands of data points that can be perfectly superimposed over the SEM image. 2015 Winners This is a huge improvement over separate Andreas Seidel-Morgenstern (left) instruments, with shuttling executed and Peter H. Seeberger (right), at the push of a button and sample orientation preserved consistently. The Who Figure 2. RISE microscopy characterization of rutile and anatase, two modifications of TiO2. The new microscope enables software- SEM image (left) shows the size and structure of the crystals. According to their Raman spectra driven quick and convenient switching (right), rutile (red) could be easily distinguished from anatase (blue). Image parameters: 12 μm x 12 between Raman imaging and SEM, will be the μm, 150 x 150 pixels = 22,500 spectra, Integration time: 0.037 sec/spectrum. transformation of the Raman spectra into an image, and the ability to overlay Nominations winner in simultaneously. Secondly, the space the SEM column, freeing space for both images to produce a RISE image. for the inside the chamber and surrounding other detectors. After SEM imaging, To explore and substantiate the the SEM column is very limited; SEMs the sample is simply transferred to the capabilities of RISE microscopy we 2016 Humanity in 2016? resemble abstract hedgehogs because Raman position using the SEM stage. identified and imaged 2D materials, Science Award all the tools orbiting the SEM column The numerical aperture of the objective including (but not limited to) graphene are now open aim toward the same point: the sample. can be optimized as the space above and molybdenum disulphide (MoS2), This is critically important because the the sample is not shared with other mineral phases in sections of a drilling resolution of an optical microscope is detectors. And you can use a compact core, and polymorphs of titanium directly linked to its numerical aperture scanner because it only has to handle the dioxide (TiO2). – the light cone angle of the objective objective and not samples of varying size We believe that correlative microscopy Analytical science has the power to change human lives for the better, but rarely receives the same available for excitation and detection. and weight. – exemplified by our RISE technology For a high-resolution objective, this The modular nature of WITec Raman – will be of great benefit in solving fanfare as other scientific disciplines. The Humanity in Science Award was launched to recognize angle is about 140 degrees, leaving microscopes allowed us to overcome many scientific questions when a single and reward a recent breakthrough in analytical science that has truly made the world a better place. precious little real estate for the SEM the third and final challenge: excitation technology is insufficient. Others seem The 2016 award will be presented on May 10 in Munich, Germany. column itself, much less other detectors. sources and spectrometers are coupled to to agree: Photonics Media and the Thirdly, a fully equipped Raman the instrument by flexible optical fibers, International Society for Optics and Could the grand winner be someone you know? Nominate an analytical science project with a microscope needs several excitation meaning that they can be placed far Photonics has recognized RISE with humanitarian impact now at www.humanityinscienceaward.com sources (lasers) and spectrometers that from the SEM chamber whilst always their Photonics PRISM Award 2015 weigh more than an SEM chamber’s preserving alignment. In a system with as being the preceding year’s most flanges can support (that is if space was “X” mirrors, there will “X” sources of innovative development in metrology Why enter? available for attachment, which it isn’t!). misalignment. Moreover, modern fibers instrumentation. And it took a podium Ÿ $25,000 grand prize We found Solzhenitsyn’s simple allow very efficient coupling of light, as spot in The Analytical Scientist’s Ÿ solution to the first two problems by they are more transparent than air. Innovation Awards in December of the All-expenses paid trip to Analytica 2016 placing only the objective and scanner same year (https://theanalyticalscientist. Ÿ Opportunity to tour Phenomenex headquarters in Torrance, California inside the vacuum chamber and changing Beyond the solution com/issues/1214/return-of-the-tasias/). the scanning procedure – we scan the We named the new technology “RISE” Nominations close on November 27, 2015 - Good luck! objective rather than the sample. The (Raman imaging with scanning electron Olaf Hollricher is R&D Director at WITec, location of the objective is offset from microscopy) and presented it at Analytica Ulm, Germany. humanityinscienceaward @humanityaward [email protected] the Analytical Scientist 2015 Winners Andreas Seidel-Morgenstern (left) and Peter H. Seeberger (right), Who will be the Nominations winner in for the 2016 Humanity in 2016? Science Award are now open

Analytical science has the power to change human lives for the better, but rarely receives the same fanfare as other scientific disciplines. The Humanity in Science Award was launched to recognize and reward a recent breakthrough in analytical science that has truly made the world a better place. The 2016 award will be presented on May 10 in Munich, Germany. Could the grand winner be someone you know? Nominate an analytical science project with a humanitarian impact now at www.humanityinscienceaward.com

Why enter?

Ÿ $25,000 grand prize

Ÿ All-expenses paid trip to Analytica 2016 Ÿ Opportunity to tour Phenomenex headquarters in Torrance, California Nominations close on November 27, 2015 - Good luck!

humanityinscienceaward @humanityaward [email protected] 56  Application Note x10 2 1.1 1 0.9 0.8 0.7 0.6 Trace LC-MS Analyses 0.5 0.4 of Hormones in 0.3 0.2 Potable Water and in 0.1 0 -0.1 Ultrapure Water 6.2 6.226.24 6.26 6.28 6.3 6.326.34 6.36 6.38 6.4 6.426.44 6.46 6.48 6.5 6.526.54 6.56 6.58 6.6 6.626.64 6.66 Counts (%) vs. Acquisition Time (min) Anastasia Khvataeva-Domanov1, Matias Figure 1. MRM chromatogram (ESI+) of estradiol in potable water and after purification using Kopperi2, Jevgeni Parshintsev2, Patrik Milli-Q® systems. Appelblad3 and Stephane Mabic1 Hormone Concentation (ng/L) 1 Millipore S.A.S., Lab Solutions, Lab Water, rue Jacques Tap water After purification Monod, 78280 St.-Quentin-en-Yvelines, France Estradiol (France, Spain) 265.40 ND 2University of Helsinki, Faculty of Science, Department 297.92 ND of Chemistry, Laboratory of Analytical Chemistry, P.O. Box 55, 00014 University of Helsinki, Finland Androsterone (France, Spain) 515.33 ND 3EMD Millipore, Lab Solutions, Advanced Analytics, 1635 ND Froesundaviks Alle 1, 169 03 Solna, Sweden Corticosterone (China) 14.91 ND

Hormones are examples of contaminants Table 1. Hormone concentrations in laboratory potable water and the product ultrapure water* of emerging concern (CEC) that have been * All data reported are one-time, one-location data and are not representative of water in the various detected in environmental and drinking countries where samples were taken. waters around the world in trace amounts (1, 2). Even at very low concentrations, CECs analyses, androstenedione, androsterone, Conclusion could potentially exert ecotoxicological corticosterone, cortisone, estradiol, estrone, Trace levels of hormones were detected effects (3). progesterone, OH-progesterone, and in laboratory potable water samples using Liquid chromatography-mass testosterone were analysed by standard LC-MS/MS. After the potable water was spectrometry (LC-MS) is frequently used addition method in potable water as well as in purified using Milli-Q® water purification for trace hormone analysis to address Milli-Q® water produced from potable water systems, the hormones were no longer concerns on environmental health and using Elix® + Milli-Q® Advantage A10 detected. Milli-Q® water purification systems safety. These methods have very low water purification systems (China and Spain) produce ultrapure water suitable for trace detection limits, making it critical to and a Milli-Q® Integral water purification LC-MS analyses in environmental research. avoid, or at least minimize, contamination system (France). 1-liter samples were enriched during the experimental process. Indeed, by SPE prior to LC-MS/MS and analyzed References components of the LC-MS instrument; the in triplicate using an Agilent 1290 Infinity® 1. M.J. Capdeville, and H. Budzinsk, TrAC Trend mass spectrometer (4); sample handling HPLC coupled to an Agilent® 6420 Triple Anal Chem 30, 586–606 (2011). and manipulation (1); as well as the reagents Quadrupole LC-MS system (ESI+, MRM), 2. S.A., Snyder, E.C. Wert, H. Lei, P. Westerhoff, and solvents used in the analyses, can all and using a Purospher® STAR RP-18 and Y. Yoon, Removal of EDCs and Pharmaceuti- contribute to contamination issues. endcapped (2 µm) Hibar® HR 50-2.1 column cals in Drinking and Reuse Treatment Processes. Water plays an important role in LC-MS, (EMD Millipore). (AWWA Research Foundation, 2007). where it is used extensively in the workflow. Table 1 summarizes the results of the 3. C.J. Sinclair, W. Beinum, C. Adams, R. Bevan, It is essential that the detected analytes come LC-MS/MS experiment. Of the three L. Levy, S. Parsons, et al. Final Report for from the samples, and not from the water potable water samples analyzed, estradiol Drinking Water Inspectorate. York: Food and used in various steps of the experiment (such and androsterone were detected in potable Environment Research Agency, (2010). http://dwi. as in the preparation of samples, standards, water in laboratories in France and Spain, defra.gov.uk/research/completed-research/reports/ blanks, and eluents; or rinsing/flushing of while corticosterone was detected in the DWI70-2-232.pdf the HPLC and MS systems). potable water sample from the Chinese 4. M. Oehme, U. Berger, S. Brombacher, F. Kuhn, To evaluate the risk of hormone laboratory. Figure 1 shows the MRM and S. Kolliker, TrAC Trend Anal Chem, 21, detection in the blanks and its effect on chromatogram of estradiol. 322-331 (2002). www.merckmillipore.com Application Note  57

Determination of Lactose in Lactose-free Products Using HPAEC-PAD

In many European countries, Figure 1. Calibration curve for the lactose concentrations in the range of 21.8 µg/L to 1090.0 µg/L the limit of lactose in lactose- and results for method performance free labelled products has been lowered from 100 to 10 mg/100 g product in recent years (1).

Mareike Margraf and Dr. Kate Monks

Special methods and systems are needed because classical determination of sugars in food products with RI detection is far too insensitive for this case. An HPLC method that easily reaches the required limit of detection (LOD) by using high-performance anion-exchange chromatography coupled to pulsed amperometric detection (HPAEC-PAD) is presented. After calibration, several Figure 2. Chromatograms of food samples (red) with an overlay of the sugar standard (blue), food products were analysed to determine samples: A: Chicken skewers, B: Meatloaf, C: “Paprika Lyoner” sausage, D: Nuremburg sausages. the lactose content. Calculated lactose concentrations and content per 100 grams also shown. Method: The system consists of a KNAUER AZURA analytical HPLC The analysis of four food samples from principle was quite specific for sugars system coupled to a DECADE II typical German food (Figure 2) shows and only showed very little interference electrochemical detector. A biocompatible that three of them were lactose-free even by matrix peaks. Using the AZURA HPLC system was used in order to eliminate according to the new lactose limits given analytical system combined with the the necessity of regular passivation. by the EU. The chicken skewers sample DECADE II electrochemical detector, The mobile phase (30 mM NaOH) was contained substantial amounts of lactose the analysis of lactose in lactose-free continuously sparged with helium to keep and could not be sold as lactose-free. The labelled products can be carried out in a it inert. The applied anion exchange column chromatograms show only little interfering robust and reproducible manner. (RCX-10, 7 µm, 250 x 4.6 mm) was stored matrix peaks, so that the analytes could be in the tempered section of the DECADE well separated and identified. Reference II detector. The isocratic separation was 1. EFSA Journal 2010; 8(9):1777 http://www. carried out at 2ml/min and 30°C (column Conclusion efsa.europa.eu/de/scdocs/doc/1777.pdf and flow cell). Injection volume was 50 µl. The presented method of HPAEC-PAD Results: A mixture of three sugars was on a KNAUER HPLC system proved to analysed exemplarily and calibration was be well-suited to determine low limits of carried out for lactose (Figure 1). sugars in food products. The detection

www.knauer.net The Bioanalytical Trendsetter

Sitting Down With…Robert (Bob) Kennedy, Distinguished Professor and Chair of Chemistry at the University of Michigan, Ann Arbor, USA, and Chair of the forthcoming HPLC 2016 conference in San Francisco. Sitting Down With  59

How are you managing all of your chemistry was one of the best routes). I current responsibilities? was also fascinated by the mathematical It’s pretty crazy right now. Being side – the patterns that emerge from the “We’ve tended to chair of the department is a full-time Periodic Table and the stoichiometry job – and chairing HPLC 2016 is also of reactions; I thought it was cool that focus on problems taking a good bit of my time. And, of you could calculate chemical reactions course, I have my research group to in that way. that demand the run. Thankfully, I have a lot of support – and I’m trying to delegate things as But you never made it into development of new much as I can. Once I get HPLC 2016 veterinary school... under control, I can cut back a little No. As an undergraduate (in Gainesville, analytical methods.” bit – 10-hour days, evening work and Florida), I decided to pursue a PhD in no rest at the weekend loses its appeal chemistry. I found research to be my pretty quickly! chief interest – making new molecules, or analytical methods. For example, discovering new things about molecules, making measurements in the brain and How did you become HPLC making measurements were all very neurotransmitters, where sampling 2016 chair? appealing. And I really enjoyed what I probes provide minute samples – but Simple – I was asked. And though was doing in the organic lab, using all lots of them. It drove us to think I wasn’t looking for more work, I’ve the different instruments (NMR and about how we perform sensitive and enjoyed so many conferences over the GC). I should also thank John Dorsey high-throughput measurements, years – and truly recognize that they help (now at Florida State University) for which led us to microfluidics and high- the wider analytical community – so I analytical chemistry courses that further sensitivity mass spectrometry (HSMS) thought it was about time to give a little triggered my interest. and a variety of fluorescence-based something back. When it was time to go to graduate detection methods. One thing that will make next school, I chose the University of North Another example is how cell year’s event great is the location: San Carolina at Chapel Hill. I remember biochemistry drives secretion, which Francisco. It’s a wonderful city and talking to Jim Jorgensen who told me he brought us to metabolomics using there is a lot going on in biotech and had an idea for a new project to analyze HPLC-MS, CE-MS, capillary LC- biopharmaceutical spaces. We’ll have an single cells. I thought that was the MS, and MALDI-MS. We wanted to emphasis on those fields at the event, coolest thing ever. Then as a post-doc, I push further and began collaborating which will make it quite special. Another worked with Mark Wightman who was with Jim Jorgensen on developing ultra- theme of the conference is personalized doing bioanalytical work. high pressure liquid chromatography medicine; expect to see some excellent Making measurements in biological (UHPLC) for metabolomics. And, speakers from this growing field. I’m systems has continued to be a big focus while all that was going on, we began really excited and looking forward to it. for me – and very fortunately it’s become developing microfluidic tools for studying Everyone reading this needs to put June a prominent trend overall. Indeed, the beta cells and measuring insulin and 19 to 24 2016 in their diaries and plan US National Institutes of Health and glucagon secretion from them. to attend this special event! National Science Foundation are very When you get an idea for a question, supportive of developing new analytical ideally it’s one where the instrumentation How did you get into science? tools to study biology – so they are is not yet available or fully developed so I was always interested in science and recognizing these trends for proteomics, you can start to think about developing I can remember being particularly metabolomics and so on. And, of course, a solution. I suppose I’m a separation interested in biology as a child. I’d that’s related to the advancement of scientist – but we’ve had projects in watch natural history shows and was analytical instrumentation. electrochemistry, fluorescence and MS. very interested in images of embryos In reality, I try to find the best technique developing. But, as I got older, I chose How do you make your group stand for the job or develop a new one. chemistry for practical reasons; I was out from the crowd? doing well at it in school and I wanted We’ve tended to focus on problems For more about HPLC 2016, to get into veterinary school (and that demand the development of new visit: www.hplc2016.org

www.theanalyticalscientist.com not the Identification of Extractable and Leachable container-closure impurities is challenging. High risk leachable compounds can lead to product withdrawal or costly delays to market. Whether you are testing drug delivery devices or food packaging materials, Thermo Scientific™ has unique capabilities for fast, confident identification and quantitation of organic and elemental impurities. Visit our website to find out how we can help you to identify all leachable suspects. usual suspects

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