Analytix Issue 3 • 2010 New Generation of Organic CRM • Organic CRMs • Chromogenic Media for MiBi • Inorganic Custom Standards • Derivatization reagents for Pharmaceuticals • Bioethanol analysis • ISO/IEC 17025 accreditation of HYDRANAL® service lab 2 New Generation of Organic CRM Dear Colleague, It has now been sixty years since Fluka® was in Buchs, our lab received ISO/IEC 17025 accreditation for founded in 1950 in the middle of St. Gallen, qNMR analysis. As a relative primary method, qNMR off ers Switzerland. After the addition of new facilities outstanding opportunities for the exact determination of Editorial in Buchs in the Rhine Valley, Fluka established the purity of organic substances. The new class of organic itself as one of the leading producers and suppli- TraceCERT® standards is traceable to NIST references and will ers of research chemicals, reagents and stand- be characterized not only by qNMR, but also by additional ards. In 1989, Fluka joined the Sigma-Aldrich analytical techniques including HPLC, GC and other meth- Corporation and eventually changed its name ods. Amino acids and PAHs have been selected to be the fi rst to Sigma-Aldrich Switzerland. Today, within the CRM which are certified by this multi-step approach, but impressive Sigma-Aldrich product portfolio, many more substances of high relevance to the analytical Fluka is the brand representing high-quality community will follow soon. reagents and standards for analytical chemistry. Michael Weber Happy birthday, Fluka brand, with 60 years of exceptional Manager R&D/Innovation Europe Hence, it is a pleasure to present a new service service, meeting the needs of the world-wide scientific tool as well as a new class of certifi ed standards community! which are now launched under the Fluka brand. With the introduction of the new web- based dynamic Custom Standards Platform (sigma-aldrich.com/csp) we provide the Michael Weber capability to compose your individual inor- Manager R&D/Innovation Europe ganic custom standard within minutes. You [email protected] can actually choose between multi-elemental standards for spectroscopy as well as anion and cation mixtures for ion chromatography. The whole process from specifying the com- position of your individual standard to the submission of your request is a fast and easy online experience. And of course, all these cus- tom standards are produced and certified under double accreditation following both ISO/IEC 17025 and ISO Guide 34. Try it! As a second highlight, we are introducing the fi rst series of a new generation of organic Certi- fied Reference Materials for calibration and validation of chromatography or for other ana- lytical applications. After the implementation of high-precision quantifi cation with 1H-NMR Analytix is published fi ve times per year by Sigma-Aldrich Chemie GmbH, MarCom Europe, Industriestrasse 25, CH-9471 Buchs SG, Switzerland Publisher: Sigma-Aldrich Marketing Communications Europe Publication director: Ingo Haag, PhD Editor: Daniel Vogler sigma-aldrich.com/analytix 3 Feature Article Chromatography 4 Launch of a New Generation of Organic 13 Enantiomeric Purities of Pharmaceuticals Certified Reference Materials Using Carbohydrate-based Isothiocyanates First Series of Products Includes 21 Amino Acids 18 Analysis of Bioethanol – Detection of Chloride and Sulfate with Dication and Microbiology Trication Solutions of Contents Table 7 Overview of Chromogenic Media Chromogenic media offer a range of benefits for Titration the enumeration, detection, and identification of 20 Increasing Reliability and Value of Analytical microorganisms. Results ISO/IEC 17025 accreditation of HYDRANAL® Standards service lab 10 New Dynamic Platform for Inorganic Custom Standards Monthly Savings Program 12 Certified Reference Materials for Spectroscopy 22 35% Off – Volumetric Titration Reagents New Product Corner 23 Analytical Standards of Alkylresorcinols 23 New Standards for Regulated Food Dyes sigma-aldrich.com/analytix 4 Launch of a New Generation of Organic Certified Reference Materials First Series of Products Includes 21 Amino Acids Alexander Rück, Senior Scientist R&D Europe [email protected] Christine Hellriegel, Senior Scientist R&D Europe [email protected] Matthias Nold, Product Manager Analytical Standards [email protected] We are pleased to present a fi rst series of the new product line accepted reference materials are readily available (e.g. from of organic TraceCERT® certifi ed standards. These certifi ed NIST and other metrological institutes), it is a significant reference materials (CRMs) are produced and certifi ed in a challenge to establish traceability for organic reference double accredited laboratory fulfi lling both ISO/IEC 17025 materials. and ISO Guide 34, using quantitative NMR for content determination with direct traceability to NIST references Conventionally, the purity of a substance is determined by and the SI base unit kg. The double accreditation represents means of GC or HPLC and the content is calculated by sub- the highest achievable level of reliability and therefore tracting water content, residue solvents and inorganic earns the label of the “gold standard” among CRM impurities from the measured chromatographic purity. producers. However, since every chemical substance has its own char- acteristic UV-absorption behaviour, direct traceability is Feature Article Feature The new product class of organic CRMs for use as internal only possible if an internationally accepted reference stand- standards for qNMR has been presented in the previous ard is available for the compound in question. This is not issue of Analytix. Here, we introduce our fi rst product line of necessary if a relative primary analytical method such as organic CRMs for use as chromatography standards. quantitative NMR (qNMR) is used. With qNMR technology, traceability between completely different organic com- Since the use of certifi ed reference materials is becoming pounds can be achieved since the NMR signal intensity is in increasingly important, especially in the areas of food & direct relation to the numbers of protons involved. beverage analysis as well as in environmental analysis, the first two series of CRMs include amino acids (which are WIS presented here) and polyaromatic hydrocarbons (PAH) S S (which we will present in the next issue of Analytix). C R N M O I Why certified reference materials? -P T R UC To ensure the reliability of analytical results, the quality of the OD reference material used for calibration of the instruments is crucial. Certified reference materials are most trustworthy STS 490 SRMS 001 since they fulfi l several requirements: ISO 17025 ISO Guide 34 • They must be traceable to an internationally accepted reference (e.g. from NIST, BAM or SI) Double accreditation for CRM production using qNMR • The certified value must have a properly calculated In the R&D lab of Sigma-Aldrich Buchs (Switzerland) a new uncertainty Bruker Avance III 600 MHz Ultrashield NMR spectrometer • They must be shown to be sufficiently homogeneous was recently installed and the instrument performance was • The stability of the material must be carefully determined optimized for the high-resolution quantifi cation of organic substances. By the end of 2009, the new NMR lab was fully If a manufacturer is accredited to ISO Guide 34 (“General accredited under both ISO/IEC 17025 and ISO Guide 34 for requirements for the competence of reference material the certification of organic reference materials using producers”) and also according to ISO/IEC 17025 (“General 1H qNMR. Quantitative NMR is a non-destructive technique requirements for the competence of testing and calibration that demonstrates many advantages over other analytical laboratories”), then the fulfi llment of all these requirements methods: it requires easy sample preparation; analysis is is guaranteed. fast; it provides full structural information; data about impu- rities or isomers are available; and it is less time consuming For more than two years now, the Buchs site of than many other analytical techniques, since it requires no Sigma-Aldrich in Switzerland has held this “gold standard” equilibration time. for the production of inorganic TraceCERT standard solu- tions (sigma-aldrich.com/inorganiccrm) for AAS, ICP and IC. While for inorganic materials internationally sigma-aldrich.com/organicCRM 5 1H qNMR is marked by its linearity, Once having selected a suitable starting material, a defi ned specifi city and robustness regard- number of subsamples are taken from diff erent positions ing most parameter settings. The within the bulk material. From those samples, some are most outstanding attribute of stored at room temperature for periodical stability tests in 1H qNMR is that it may be consid- order to get data on aging of the material. Other samples ered a primary ratio method are stored at higher temperature for stress tests, helping to because it does not need a stand- ensure stability at even extreme transportation conditions. ard reference of the same material. Further samples go into quality control for chromatography, The NMR spectrum of a solution LC-MS or other standard techniques if required. However, 10 shows all soluble organic sub- subsamples are taken for homogeneity assessment and stances present, with the peak area content determination by qNMR. Therefore, it is necessary being directly proportional to the that a reference standard has certain required properties in amount of nuclei