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www.dionex.com/foodnotebook Related Dionex Applications Literature Dionex has an extensive library of methods and techniques for determining a wide variety of analytes important to the . Below is a selected list of applications covered in this brochure. For more information, please visit www.dionex.com and click on Industrial/Food and Beverages on the sidebar under

Applications. All of the literature below can be found by clicking Literature and Manuals under Training and Corporate Headquarters Support on the sidebar, or by contacting your local Dionex representative. Dionex Corporation 1228 Titan Way P.O. Box 3603 Literature Sunnyvale, CA 94088-3603 Tel: (408) 737-0700 Contaminant Matrix Resource Fax: (408) 730-9403 Fried and baked AN 409: Fast Determination of in Food Samples Using Accelerated Acrylamide Solvent Extraction Followed by Ion Chromatography with UV or MS Detection Worldwide Sales and Service juice AN 82: Analysis of Fruit Juice Adulterated with Medium Invert from Beets North America U.S./Canada (847) 295-7500 Poster: Fast and Effective Determination of in Grains or Food Using Aflatoxins Grains and seeds Accelerated Solvent Extraction Followed by HPLC South America Liquid food AN 165: Determination of Benzoate in Liquid Food Products by Reagent-Free Brazil (55) 11 3731 5140 Benzoate products Ion Chromatography Europe AN 182: Determination of Biogenic Amines in Alcoholic Beverages by Ion Austria (43) 1 616 51 25 Biogenic amines Beer, wine Chromatography with Suppressed Conductivity and Integrated Pulsed Benelux (31) 20 683 9768 Amperometric Detection (32) 3 353 42 94 AN 183: Determination of Biogenic Amines in Fermented and Non-Fermented Denmark (45) 36 36 90 90 Biogenic amines Meats, cheese Foods Using Ion Chromatography with Suppressed Conductivity and Integrated France (33) 1 39 30 01 10 Pulsed Amperometric Detection Germany (49) 6126 991 0 AU 162: Determination of Biogenic Amines in Fruit, Vegetables, and Chocolate Ireland (353) 1 644 0064 Fruit, vegetables, Biogenic amines Using Ion Chromatography with Suppressed Conductivity and Integrated Pulsed Italy (39) 02 51 62 1267 and chocolate Amperometric Detection Sweden (46) 8 473 3380 Iodide Milk AN 37: Determination of Iodide in Milk Products Switzerland (41) 62 205 9966 United Kingdom (44) 1276 691722 AN 221: Rapid Determination of in Liquid Milk and Milk Powder by Melamine Milk HPLC on the Acclaim Mixed-Mode WCX-1 Column with UV Detection Asia Pacific AN 112: Determination of Nitrate and Nitrite in Meat Using High-Performance Australia (61) 2 9420 5233 Nitrate and nitrite Meats Ion-Exchange Chromatography China (852) 2428 3282 Organochlorine AN 349: Rapid Determination of Organochlorine in Animal Feed India (91) 22 2764 2735 Animal feed pesticides Using Accelerated Solvent Extraction Japan (81) 6 6885 1213 Korea (82) 2 2653 2580 Organophosphorus AN 343: Determination of Pesticides in Large-Volume Food Samples Using , vegetables pesticides Accelerated Solvent Extraction Singapore (65) 6289 1190 Taiwan (886) 2 8751 6655 AN 356: Determination of in Vegetation Samples Using Accelerated Perchlorate Vegetation Solvent Extraction and Ion Chromatography Fruits, vegetables, Pesticides AN 332: Accelerated Solvent Extraction of Residues in Food Products grains www.dionex.com AN 196: Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Edible Polycyclic aromatic Edible oils Oils by Donor-Acceptor Complex Chromatography (DACC)-HPLC with hydrocarbons (PAHs) Fluorescence Detection

Dried fruit, wine, AN 54: Determination of Sulfite in Food and Beverages by Ion-Exclusion Sulfite Dionex products are designed, bottled juices Chromatography with Pulsed Amperometric Detection developed, and manufactured AN 353: Rapid Determination of Sulfonamide Residues in Animal Tissue and under an ISO 9001 Quality System. Sulfonamides Animal tissue Infant Food Containing Animal Products Using Accelerated Solvent Extraction Grains (wheat AN 350: Extraction of Zearalenone from Wheat and Corn by Accelerated Zearalenone and corn) Solvent Extraction MSQ and MSQ Plus are trademarks of Thermo Fisher Scientific. All All TN 208: Methods Optimization in Accelerated Solvent Extraction Venture is a trademark of W. R. Grace and Co. TN 209: Accelerated Solvent Extraction Sample Preparation Techniques for Food DCMSLink, Reagent-Free, and RFIC are trademarks and Acclaim, ASE, ASRS, All All and Animal Feed Samples AutoSuppression, AutoTrace, CarboPac, Chromeleon, CSRS, IonPac, and UltiMate are registered trademarks of Dionex Corporation. TN 210: Accelerated Solvent Extraction Techniques for In-Line Selective All All Removal of Interferences © 2009 Dionex Corporation LPN 2135-02 PDF 08/09 Printed in U.S.A.

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Global Supply, Local Concern

Increasingly global food supply chains have raised concerns about food safety. Products are grown and processed in widely differing environments under a variety of regulatory frameworks, travel thousands of miles, are kept in various storage conditions, experience temperature fluctuations that may affect shelf life, and are handled by many different people. At any point in this process, products can be contaminated or may become unfit for consumption.

Contaminants may originate from agricultural Food contaminant analysis poses several Fortunately, with Dionex technology many of sources, such as pesticides, animal growth challenges. Usually, the contaminant must be these food contaminants can be extracted hormones, or antibiotics; environmental isolated from the food matrix before it can be and identified reliably and quickly before they sources, such as water and air pollutants; analyzed. The proper separation technique, reach the table. Dionex has worked with or from food production processes, via medium, and mobile phase/gradient must industry and regulatory agencies to develop or adulteration. Food be identified, depending on the suspected extraction, sample preparation, IC, and HPLC contaminants may cause acute effects contaminants. Finally, a detection method solutions for the determination of a broad ranging from mild rash, light headache, or sensitive to the suspected contaminants range of food contaminants. to more serious diseases like , must be used. auto-immune diseases, thyroid problems, and even death. Health effects of exposure to contaminants may become apparent only after years of prolonged exposure.

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www.dionex.com/foodnotebook System Solutions

Solvent and Solid-Phase Extraction Ion Chromatography Liquid Chromatography Solid food samples (e.g., grains, fruits, Since the development of ion chromatography The Dionex UltiMate® 3000 series of liquid vegetables, meats) require sample (IC) analysis over 30 years ago, Dionex has chromatography systems are ideal for preparation before analysis. Common pioneered the development of IC systems, the analysis of organic contaminants, for extraction techniques, such as Soxhlet and media, and applications. Whether you are example polycyclic aromatic hydrocarbons sonication, are slow and use high solvent running a few food samples for process or pesticides. Choose from a wide variety volumes. Additional cleanup steps are often development or have a heavy workload of of modules, detectors, and configurations to required after these extraction techniques, samples for QC and regulatory compliance, adapt the instrument to your applications and adding additional time, labor, and cost. whether your analytical task is simple or needs. From semipreparative to analytical complex, Dionex has the right system for you. to nano scale applications, and from basic Dionex Accelerated Solvent Extraction (ASE®) systems to the Rapid Separation LC systems systems use elevated temperatures and • Starter line and basic systems for straightforward and repetitive analyses for UHPLC, there is a system solution that is pressures to extract analytes quickly and right for you. efficiently. Adsorbants mixed with the • Reagent-Free™ systems reduce eluent and sample or placed in the extraction cell regenerant preparation • Excellent retention time precision, detector automate cleanup of interferents, further • Dual systems allow double throughput, sensitivity, linearity, and drift reducing time, effort, and solvent usage. simultaneous analysis, and complex • x2 dual systems for multidimensional The AutoTrace® SPE instrument automates methods separations extraction and concentration of liquid • Suppressed conductivity, pulsed • Rapid Separation LC (RSLC) systems for samples. amperometry, UV-vis, fluorescence, and fast, high flow-rate, ultrahigh-pressure MS detectors applications • Extraction of sample sizes from 1 to 100 g in minutes • Ion-exchange, ion-exclusion, carbohydrate, • Biocompatible systems available for and amino acid columns sensitive samples • Automation reduces operator time and labor • Concentrator, polishing, and trap columns • Reversed-phase, ion-exchange, for on-line sample preparation and trace mixed-mode (HILIC, reversed-phase, • Dramatic solvent reduction analyte determination and ion-exchange combinations), and • Handles acidic and alkaline matrices • Integrated control and data processing monolith columns ® • Wide range of applications with Chromeleon software • Diode array, multi-wavelength, • Approved for use by the US EPA fluorescence, and MS detectors • Integrated control and data processing with Chromeleon software

ASE and AutoTrace Series ICS Series UltiMate Series Accelerated Solvent and IC/RFIC™ Analytical Systems HPLC/RSLC Analytical Systems Solid-Phase Extractions page 3 Agricultural Chemicals

Agricultural chemicals are used to increase crop yields, control weeds and pests, and to prevent diseases to crops and livestock. These chemicals include pesticides, , plant growth regulators, growth hormones, and veterinary drugs/antibiotics. Many of these substances pose health risks to humans and livestock, and can build up in the environment or in foods. Dionex provides applications and systems for the extraction and determination of a variety of agricultural chemicals.

Pesticide Extraction from Crops Pesticide Analysis Peaks: (10 µg/L each) Some pesticides that pose severe health or N-methylcarbamates and 1. sulfoxide 7. Propoxur 2. Aldicarb sulfone 8. Carbofuran environmental risks have been banned in N-methylcarbamoyloximes are among the 3. Oxamyl 9. Carbaryl many countries around the world, but are most widely used pesticides in the world. 4. Methomyl 10. 1-Naphthol 5. 3-Hydroxy carbofuran 11. Methiocarb still used in other countries. Build up of legal Gas chromatographic analysis has proven 60 6. Aldicarb 12. BDMC

pesticides in foods can also pose a health unsuccessful due to degradation of the 4 risk to humans and animals, with the severity analyte compounds during vaporization. 2 3 9 depending on the type of pesticide and the Postcolumn derivatization with fluorescence mV 1 10 5 6 length of exposure. Dionex ASE systems can detection after a reversed-phase HPLC 78 be used for the extraction of pesticides, such separation delivers highly sensitive 1112 as organophosphates, organochlorides, and determinations of carbamate compounds. carbamates, from solid and semisolid food When even more sensitivity is required, -5.9 510152023.8 samples rapidly, and with far less solvent than the Dionex UltiMate 3000 system and Minutes 24088-01 Soxhlet or sonication. Chromeleon software can be combined with an MS/MS system solution using the Chromatogram of a standard mixture of 10 Link™ carbamates plus two reference compounds (peaks DCMS software plug-in to provide a 10 and 12) separated using an UltiMate 3000 powerful alternative. system and Acclaim® 120 C18 column.

page 4 Antibiotic Extraction and Analysis The ASE systems are ideal for extraction Peaks: 1. Sulfadiazine (SDZ) of sulfonamides from meats, with high 2. Sulfathiazole (STZ) Veterinary drugs and antibiotics are used recoveries. Although milk does not require 3. Sulfapyridine (SPD) in the animal breeding industry to treat, 4. Sulfamerazine (SMR) extraction, samples can be notoriously 5. Sulfamethazine (SMZ) prevent, and control diseases caused by 6. Sulfachloropyridazine (SCP) difficult to analyze, due to the complexity of viruses, bacteria, protozoa, and fungi. 7. Sulfadimethoxine (SDM) the matrix. Standard sulfonamide separation 8. Sulfaquinoxzline (SQX) Unfortunately, some of these drugs are also *. Theobromine procedures require two injections with 40 added to animal feed to stimulate growth 1 different mobile phases to resolve all eight 2 3 4 5 and produce leaner meat. In humans, C 6 7 8 compounds commonly found in milk. With a these drugs can cause an allergic reaction, Dionex HPLC system, Acclaim 120 C18 column, mAU bacterial resistance to antibiotics, and even B gradient separation, and UV-vis detection, * cancer. Regulatory agencies have established sulfonamide antibiotic residues in milk or maximum contamination levels for a variety meat extracts can be determined easily in a 0 A of antibiotics, and some have been banned single injection. for use in livestock or feed. Testing of crops, animal products, and feed is essential to Tetracyclines are wide-spectrum antibiotics 5 10 15 20 25 Minutes protect humans from exposure. commonly used for infections in humans 21533 and livestock. Animal studies show that Gradient separation of A) sulfonamide standards, Sulfonamides are used as veterinary tetracycline can cross the placental barrier, B) a milk sample, and C) a milk sample spiked with antibiotics, both to combat infection sulfonamides, performed using an UltiMate 3000 and can have toxic effects on developing and to promote growth. Some livestock system and Acclaim 120 C18 column with UV fetuses. Long-term exposure in humans may detection at 265 nm. Samples prepared according companies have abused these drugs to also to the development of antibiotic- to AOAC method 993.92. increase growth and profits. American resistant strains of bacteria. Tetracycline and European regulatory agencies have contaminants in a pork sample are rapidly and established maximum residue levels (MRLs) Peaks: 1. Oxytetracycline easily quantified using a Dionex HPLC system 2. Tetracycline for veterinary antibiotics in meat and and UV detection. 3. Chlortetracycline milk products. 4. Doxycycline 18 1 2 4 3 C

mAU B

A 0

0 1 2 3 4 5 6 7 Minutes 21534

Gradient separation of A) tetracycline standards, B) a pork sample, and C) a pork muscle sample spiked with tetracyclines, performed using an UltiMate 3000 system and Acclaim 120 C18 column with UV detection at 360 nm.

page 5 Environmental Contaminants

Environmental contaminants can be either natural or man-made, and are present in the water, air, and soil. Some are biological byproducts of bacteria or fungi that may come into contact with foods during growth or storage. These chemical contaminants include perchlorate, nitrate, polycyclic aromatic hydrocarbons (PAH), polychlorinated biphenyls (PCB), dioxins, lead, , , polybrominated diphenyl ether (PBDE), , , and biogenic amines as well as many others.

Mycotoxins are regulated in many countries. Analysis 494 methods for aflatoxins commonly include A Mycotoxins are mild to fatal Soxhlet extraction and solid-phase extraction produced by fungi, and develop in a wide (SPE) cleanup prior to separation and B1 variety of crops during growth or storage, determination using HPLC. Dionex automates mV B2 including grains, tree nuts, ground nuts, and these sample prep steps by combining G1 oil seeds. Symptoms of exposure include extraction with an ASE system followed by allergic reactions, diarrhea and nausea, on-line SPE-LC using an UltiMate 3000 HPLC -83 kidney damage, immunosuppression, system, a Venture™ AF SPE immunoaffinity 494 nerve damage, and even death. Many of B column, and an Acclaim 120 C18 analytical these have also been identified as column. This method saves time, labor, and . Over 400 mycotoxins have solvent and yields high recoveries and the mV been identified and, based on toxicity and B1 low detection limits (< 2 ppb) required by the B2 occurrence, aflatoxins, vomitoxin, fumonisin, European Commission and the US FDA. zearalenone, and T-2 are of primary -83 concern. Contamination by - Zearalenone (ZON) is a mycotoxin produced 19 22 24 26 29 Minutes producing fungi is unavoidable, so a variety by the Fusarium fungus. ZON can be found 25425-01 of crops have to be monitored to make sure in a wide variety of plants and soils, and can Determination of aflatoxins extracted from that production and storage conditions do not have negative health effects on animals and A) almonds and B) corn using an ASE system. allow toxins to accumulate above humans. Traditional methods for extracting Samples were prepared using on-line SPE, separated acceptable limits. ZON from soils or animal feed include wrist using an Acclaim 120 C18 column, and detected using fluorescence. Levels of B1 were shaking or blending. These methods normally Aflatoxins are produced by the fungus above 20 µg/kg for both samples, higher than take 30–60 min per sample with constant regulatory maximums in Europe and the US. Aspergillus that grows in soil and decaying lab technician attendance. The ASE system vegetation. These toxins are highly reduces the extraction time to approximately carcinogenic, and the presence of the 15 min per sample and uses only 25–35 mL aflatoxins designated B1, B2, G1, and G2 of solvent.

page 6 Environmental Contaminants

Biogenic Amines Perchlorate A B Biogenic amines, such as cadaverine, Perchlorate is a naturally occurring mineral Peaks: 1. Putrescine 0.65 9.5 mg/kg 2. Cadaverine — 3.1 putrescine, spermidine, histamine, found in nitrate fertilizers, and a manmade 3. Histamine — 1.6 phenyethylamine, agmatine, and tyramine, chemical used as an ingredient for solid 4. Agmatine 8.2 6.9 5. Spermidine 7.6 14.3 are low molecular weight organic bases rocket propellant, explosives and industrial 6. Spermine 46.6 32.1 commonly present in living organisms, where processes like rubber manufacturing. This 0.65

they are responsible for many essential contaminant interferes with the iodide uptake 6 functions. In general, the consumption of into the thyroid gland, and can disrupt neuro- biogenic amines does not present a health logical development in fetuses and children. µS hazard, but at high concentrations these 1 4 5 Perchlorate in irrigation water can build up in compounds can lead to serious health effects. a variety of crops, such as lettuce, spinach, A: Stored at 4 °C for 2 weeks Determination of these compounds in fresh 0.30 melons, and grains. Sample preparation 0.65 and processed food is of interest not only for perchlorate analysis typically involves because of their toxicity, but also because of 6 high speed blending and ultrasonication 1 their use as spoilage indicators. µS 2 extraction, but these techniques are not 3 4 5 Many biogenic amines can be detected efficient enough to extract tightly bound ions, using conductivity detection, but some such as perchlorate, from complex vegetation B: Stored at 25 °C for 2 weeks 0.30 do not have a charge after separation, or other biosolid matrices. Additional cleanup 0 10 20 30 40 and thus are non-conductive. Uncharged steps, such as SPE, are also usually required. Minutes 24117 amines can be detected using integrated An ASE system can extract perchlorate from Biogenic amines in sausage after storage at A) 4 °C pulsed amperometric detection (IPAD) or UV biosamples in approximately 15 min, and and B) 25 °C, separated using an IonPac CS18 detection. Suppressed conductivity provides additional cleanup steps are not required column and detected using suppressed conductivity. superior detection limits, and IPAD provides when in-cell adsorbants are used. Because Increases in putrescine, cadaverine, histamine, and spermidine indicate spoilage. the ability to determine a wider range of the extraction solvent is water, methods analytes. The Dionex ICS-3000 system can be developed for analysis of perchlorate in water configured with all three detectors, in series are easily applicable. Peak: 1. Perchlorate 10 ng/g or in parallel, to determine 10 biogenic amines 25 Extraction recoveries from fruits, vegetables, in a single injection on an IonPac® CS18 and grains range from 89 to 110% for column. Biogenic amines can be determined quantities as low as 10 ppb (ng/g). Minimum in alcoholic beverages, meats and cheeses, detection limits using an IonPac AS16 column vegetables, and even chocolate. Mass and suppressed conductivity detection are spectrometry can also be used to identify µS A <2.0 µg/kg for perchlorate extracted from biogenic amines in cases where interferents spinach, melon, and corn. are present. B 1

0 17 20 25 30 35 Minutes 22991-01

Perchlorate extracted from A) spinach and B) spinach spiked with 10 ng/g perchlorate, separated using an IonPac AS16 column and detected using suppressed conductivity.

page 7 Food Additive Contaminants

Food additive contaminants are chemicals that are intentionally added to a product during the manufacturing process. Many chemicals are added for valid reasons, and need to be monitored to assure they are added according to their usage and specifications, to detect contamination of chemical feed stocks, and for labeling purposes due to potential allergic reactions for consumers. Some examples of these types of chemicals would be nitrate, nitrite, sulfite, and benzoate. In some cases, however, dangerous or banned chemicals are used to save cost or mislead the consumer. From a safety and regulatory standpoint, unauthorized and banned chemicals need to be detected to assure they are not being used for food products. Examples include melamine and Sudan dyes.

Sulfites occur naturally in almost all wines Melamine Peaks: 1. Melamine 50 µg/L and are added to wines as , to Melamine, a common component of 2. Cyanuric acid 200 prevent spoilage and oxidation. Sulfites are plastic manufacturing, and cyanuric acid, a often used as preservatives in foods, such 450 compound often used for pool chlorination, 1 as dried fruits and vegetables. Both the EU are closely related chemicals that are and the US FDA require that foods containing non-toxic by themselves. However, when sulfites be labeled, and the US FDA has combined these components form a toxic, banned the use of sulfites in certain foods, insoluble crystal that causes kidney stones such as fresh fruits and vegetables. Ion- mAU and can lead to renal failure. Because exclusion chromatography and pulsed melamine has a high nitrogen content, it has amperometric detection can be used to been added to low-quality wheat gluten, quantify sulfite in wine and dried foods for animal feed, and milk products to make them regulatory and labeling compliance. A appear higher in protein. Numerous children B 2 and pets have become ill and some have died Nitrate and Nitrite 0 because of food products adulterated with Nitrate and nitrite are usually added to melamine and contaminated with cyanuric 0.0 2.5 5.0 7.5 10.0 processed meat products to protect against Minutes acid. Melamine and cyanuric acid can be 24324 that can cause food separated using an Acclaim Mixed-Mode poisoning, such as . A) Melamine and B) cyanuric acid standards, separated WAX-1 or WCX-1 column and determined by using an Acclaim Mixed-Mode WAX-1 column and However, nitrite can react with secondary UV absorption (LC/UV and IC/UV), or mass detected using UV at 210 nm. amines in food products or in the digestive spectrometry (LCMS) for increased specificity system to form nitrosoamines, a class and sensitivity. of carcinogenic compounds. Nitrate, Peaks: 1. Mannitol – Sulfites although more stable than nitrite, can act 2. Sulfite 10.4 mg/L as a reservoir for nitrite. Also, nitrate can Sulfites are used in foods to preserve the look 120 readily be converted into nitrite by microbial 2 and taste and to prevent spoilage. However, reduction. Thus, both nitrate and nitrite must excessive concentrations can trigger allergic be monitored to ensure the quality and safety reactions in some people, causing breathing of meat products. nC difficulty in minutes after ingestion. 1

0 0 612 Minutes 11853-03

Determination of sulfite in apricots by ion-exclusion chromatography, separated using an IonPac ICE-AS1 column and detected using pulsed amperometry.

page 8 Food Additive Contaminants

using an IonPac AS18 column and suppressed Sudan Dyes Peaks: 1. conductivity detection can determine and 2. Sudan II The Sudan dyes have been linked to increased quantify benzoate in a variety of liquid 3. Sudan III cancer risks, and are now banned in most 300 4. Sudan IV food samples. Carbonated beverages often 5. Oil Red O (2 peaks) countries around the world. However, some contain benzoate, as well as other additives. suppliers still turn to these substances to The Acclaim Mixed-Mode WAX-1 column and enhance their products’ visual appeal, in spite UV detection can be used to simultaneously mAU of the prohibition, because of low cost and determine benzoate, citrate, , 3 4 easy availability. Sudan dye contamination 1 2 , and other additives for B 5 discovered in 2005 led to the UK's biggest A assurance. 0 food recall ever. Sudan dyes can be 0 2 4 6 8 10 12 determined quickly and easily using an HPLC Alternative Ingredients Minutes 21787-01 system with an Acclaim 120 C18 column and Determination of sudan dyes in paprika, separated using absorbance detection. Unscrupulous manufacturers may replace quality ingredients with cheaper alternatives an Acclaim 120 C18 column and detected using UV at 500 nm. Benzoate to cut costs and increase profits. This can be dangerous for consumers with food allergies, Since the early 1900s, benzoate has been particularly if all of the ingredients are not used worldwide as a , due to Peaks: 1. Chloride – listed on the label as required by law in 2. Benzoate 0.05 % its antimicrobial properties, low toxicity, most countries. Examples include the use 1 and absence of taste. Although the US 10 of beet medium invert sugar in orange juice, FDA lists benzoate as generally recognized and the addition of coffee husks, cereals, or as safe (GRAS), the maximum permitted caramelized to instant coffees. These concentration is 0.1%. The European Union adulterants can be detected by determining limits benzoate to 0.015% in soft drinks and full oligosaccharide or carbohydrate profiles 0.2% in all other foods. Ion chromatography using IC with the CarboPac® PA-100 column µS and pulsed amperometric detection.

2

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Determination of benzoate in , separated using an IonPac AS18 column and detected using suppressed conductivity.

page 9 Process Contaminants

Processing contaminants are generated during the processing cycle of a product. They are formed when a chemical reaction takes place between the food and processing (e.g., disinfection, fermentation, heating, canning, or grilling). Examples of these contaminants include acrylamide, PAHs, oxyhalides, and haloacetic acids.

Acrylamide Polycyclic Aromatic Hydrocarbons Peaks: 1. Acrylamide 1.56 mg/kg Acrylamide is a genotoxic compound found in Edible Oils in fried or baked goods. It is produced when Numerous polycyclic aromatic hydrocarbons 100 asparagine reacts with reducing sugars, such (PAHs) are carcinogenic, making their as fructose or glucose, or carbonyl compounds. presence in foods and the environment a Browning while cooking produces acylamide, health concern. PAHs occur in charbroiled as does overcooking. The acrylamide content and dried foods, and may form in edible oils mAU 1 in some samples, such as hash browns, potato by pyrolytic processes, such as incomplete chips, or French fries, can be particularly high, combustion of organic substances. PAHs in as much as several mg/kg. foods can also result from environmental contamination. –10 Sample preparation methods for acrylamide 02Minutes 5 determination often use multiple cleanup steps, Oils are difficult to analyze, because the 18772-01 such as liquid extraction, centrifugation, matrix quickly clogs columns and equipment. Determination of acrylamide in potato chips after and SPE. Automated extraction using an Most methods for PAH determination in oils extraction using an ASE system. Extract separated ASE system decreases the time, labor, and require complex liquid-liquid extractions, using an IonPac ICE-AS1 column and detected solvent required to prepare samples for cleanup columns, evaporation, and/or SPE. using UV at 202 nm. analysis. Acrylamide can be separated using These manual steps are time, labor, and ion-exclusion chromatography or reversed- solvent intensive. The dual capabilities of the Peaks: (20 µg/kg each) phase LC, and determined by UV or mass UltiMate 3000 system allow automation of 1. Phenanthrene 8. Benzo[k]fluoranthene spectrometric detection. Dionex provides 2. Anthracene 9. Benzo[a]pyrene SPE and matrix elimination, greatly reducing 3. Fluoranthene 10. Dibenzo[a,h]anthracene solutions for the application of preference. the effort and resources required to analyze 4. Pyrene 11. Benzo[g,h,i]perylene 5. Benzo[a]anthracene 12. Indeno[1,2,3-cd]pyrene these carcinogens while increasing the 6. Chrysene 13. Benzo[b]crysene (added as I.S.) recovery and reproducibility of the method. 7. Benzo[b]fluoranthene 140 8

2 6 9 5 mV

7 10 1 4 11 3 12 13

–20 25 30 35 40 45 50 55 60 Minutes 25267-01

Determination of PAH standards in an olive oil matrix using automated on-line matrix elimination. The overlay of seven runs shows the reproducibility of the automated SPE and the separation. page 10 of bromate despite interferences from the

Disinfection By-Products Chlorite

matrix. However, waters with high ionic- Bromate Bottled water is considered a food product strength matrices, especially mineral waters, by many regulatory agencies, such as the can overload even the highest-capacity US FDA and the European Commission. columns, leading to band broadening or even All drinking water must be disinfected, to 0.5 total masking of the bromate peak. Dionex remove microorganisms and ensure it is has developed a two-dimensional IC method safe to drink. However, reactions between that automatically preconcentrates the disinfectants and organic matter in water water sample, eliminates the matrix using can produce carcinogenic by-products, such µS

a 4 mm column, and resolves the bromate Chlorate as bromate, oxyhalides, and haloacetic peak on a 2 mm column with a different acids, that are dangerous even at trace column chemistry. This not only prevents concentrations. Trace analysis of drinking interference, but it increases sensitivity by water can be difficult because of the high using a smaller diameter column and provides 0.2 concentrations of other ions that are often 0 5101520 25 30 verification by using two different column found in water. Dionex has developed a Minutes 24076-01 chemistries. number of different columns and methods Determination of chlorate, chlorite (1.0 µg/L each), and to facilitate determination of these Haloacetic Acids bromate (0.5 µg/L) in a water sample using a high- contaminants. capacity 4 mm IonPac AS19 column and suppressed Haloacetic acids (HAAs) are formed when conductivity detection. Oxyhalides and Bromate chlorine disinfectants react with organic acids. Many of these acids are suspected The bromate is formed in water Peaks: 1. MCAA carcinogens. Five HAAs are regulated in 3 when naturally occurring bromide reacts 7500 2. MBAA much of the world, and some regulatory – 3. DCAA – Br with ozone used for disinfection. Chlorate 6500 Cl 4. BCAA bodies require monitoring of other HAAs. NO – 3 5. DBAA and chlorite are produced by chlorine dioxide – CO 2 Many of these compounds can be determined 5500 3 6. TCAA and chloramine disinfectants. High-capacity 2– Intensity, cps SO 7. BDCAA using conductivity detection, but mass 4 IC columns and conductivity detection can 4500 8. CDBAA spectrometry is the best detection method for 9. TBAA be used to determine low levels of chlorate, 3500 5 6 determining the most HAAs simultaneously. 4 7 chlorite, and bromate in drinking water with 2500 Dionex developed the IonPac AS24 column 2 moderate to low ionic-strength matrices. 8 specifically for the separation of HAAs before 1500 Br– 9 Postcolumn derivatization and UV detection 1 detection using MS. allows determination of very low levels 500 0 51015202530354045505560 Minutes 25675-01

Determination of haloacetic acids (1.0 µg/L each) in a water sample using an IonPac AS24 column and ESI- MS/MS detection. The green areas designate the times during which the matrix ions were diverted to waste.

page 11