EU Regulation 396/2005: Pesticide Residue Testing and the Critical Role of QuEChERS Evaporation in Food Safety

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 4th May 2026? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application note by<strong> Shimadzu, </strong>presentation by <strong>MDCW / JEOL</strong> and technical note by <strong>Thermo Fisher Scientific!</strong></p><h3><strong>1. MDCW / JEOL: Flow-Modulated GCxGC-QMS Analysis Without Splitting Off the GC Flow</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/O_16_Jensen_11e29d5022.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>This presentation by Kirk Jensen (JEOL USA) explores the feasibility of performing <strong>flow-modulated comprehensive two-dimensional gas chromatography (GC×GC) coupled with quadrupole mass spectrometry (QMS)</strong> without splitting the GC flow, which is traditionally required to protect MS systems from high carrier gas flows. The core concept builds on GC×GC, where compounds are separated using a primary and secondary column connected via a modulator, significantly increasing separation power compared to one-dimensional GC. The presentation contrasts <strong>thermal modulation</strong> (offering sharper peaks and higher theoretical sensitivity but requiring cryogenic cooling) with <strong>flow modulation</strong>, which avoids cryogens, handles volatile analytes well, and is more flexible, but typically demands higher gas flows that standard MS systems cannot tolerate .</p><p>To address this limitation, the study utilizes the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=24&amp;search=JMS-Q1600GC"><strong>JEOL JMS-Q1600GC</strong></a><strong> UltraQuad quadrupole GC-MS system</strong>, which can accept unusually high carrier gas flows (up to ~20 mL/min), enabling direct coupling with a <strong>SepSolve INSIGHT flow modulator</strong> without splitting the effluent . The analytical setup includes dual GC columns (e.g., Zebron ZB-5MSplus for the first dimension and BPX50 for the second), high secondary flow rates (~25 mL/min), and electron ionization (EI) MS detection. Additional system components include optional FID detection, bleed line control, and ChromeSpace software for data processing . This configuration allows full analyte transfer into the MS, eliminating the need for flow splitting and potentially improving detection efficiency.</p><p>Experimental results demonstrate the applicability of this approach to complex mixtures, including a <strong>pesticide mixture containing over 200 compounds</strong> and real-world samples such as perfumes and fuels. The GC×GC-MS system produced detailed two-dimensional chromatograms with high spectral quality, enabling the correct identification of approximately 120 compounds despite relatively moderate spectral match factors . Comparisons at different flow rates (e.g., 25 vs. 50 mL/min) showed that spectral integrity and compound identification remain robust, indicating that higher flow operation does not significantly compromise MS performance.</p><p>In conclusion, the work demonstrates that <strong>flow-modulated GC×GC-QMS without flow splitting is feasible</strong>, provided that the MS system can tolerate high carrier gas flows. While further optimization is needed (e.g., column selection, inlet pressure, and separation conditions), the approach offers a practical alternative to thermal modulation by eliminating cryogens and simplifying operation. Future work will focus on improving sensitivity, optimizing separations, and exploring alternative carrier gases such as hydrogen to reduce costs and expand applicability</p></div></div></div></div></div></div></section><h3><strong>2. Shimadzu: Detailed Hydrocarbon Analysis by Nexis GC-2030 Using ASTM D6730</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00863_en_eb633bc741.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>Detailed compositional analysis of gasoline in accordance with ASTM D6730 is feasible using the Nexis GC-2030.&nbsp;</li><li>By employing PONAsolution, a PONA/DHA analysis software, laborious identification tasks can be reduced, and quantitation calculations and report generation can be performed automatically.</li></ul><p>ASTM D6730 specifies the analysis of hydrocarbons in gasoline and oxygenates such as ethanol, methyl tert-butyl ether (MTBE), and ethyl tert-butyl ether (ETBE) over a boiling point range up to 225 ̊C. Identification and quantification of individual compounds in gasoline are critically important for refinery process control and product quality assurance. In this application news, we report compositional analysis of gasoline conforming to ASTM D6730 using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexis+GC-2030"><strong>Nexis GC-2030 gas chromatograph</strong></a>. Gasoline typically comprises over 100 hydrocarbons, making identification tasks highly complex; however, PONAsolution, a PONA/DHA analysissoftware,simplifies this process.</p><h4><strong>PONAsolution</strong></h4><p>PONAsolution Ver.6 provides retention index libraries for each relevant standard (ASTM D6730, D6729, D5134, D6733). Identification of n-alkanes automatically corrects the retention times of the remaining several hundred components, thus streamlining the identification process. When only a specific retention region requires adjustment, the two-point identification function is useful (Fig. 1). In the two-point identification procedure, reference and sample chromatograms are compared while assigning corresponding peaks. First, click on an identified component mark in the reference data (Fig. 1, a), then click the matching sample peak (Fig. 1, b). Repeat this for a second pair of peaks. The retention times of components between these two anchor points are then automatically corrected.</p><h4><strong>Conclusion</strong></h4><p>Compositional analysis of gasoline in accordance with ASTM D6730 was performed. The combination of SH PONA Tuning Column and SH-1 PONA main column enabled separation of compounds with closely spaced retention times. Moreover, use of PONAsolution software greatly simplifies complex identification tasks.</p><h3><strong>3. Thermo Fisher Scientific: Fiber optic probes add flexibility to Raman chemical analysis</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/drx3_flex_tech_note_tn54708_bebb56b870.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Fourier Transform Infrared Spectroscopy (FTIR) and Raman Spectroscopy are non-destructive analytical techniques that rely on the interaction of electromagnetic radiation with molecular vibrations to provide information about the chemical composition and structure of a sample. Despite their similarities, there are some distinct differences between the two techniques. In principle, FTIR is based on the absorption of infrared radiation by molecules and measures changes in dipole moment during molecular vibrations. Raman spectroscopy, on the other hand, is based on the inelastic scattering of monochromatic light and measures changes in polarizability during molecular vibrations.&nbsp;</p><p>When applied to bulk chemical analysis, both FTIR and Raman spectroscopy can be used to analyze solids, liquids, and gases, but the nature of Raman spectroscopy lends some unique sampling advantages. Additionally, Raman often requires little to no sample preparation. Presented herein are application examples that highlight some of the sampling advantages of Raman spectroscopy. All the spectral data in this technical note were collected using a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2238"><strong>Thermo Scientific™ DXR3 Flex Raman Spectrometer</strong></a> equipped with a fiber optic probe. (Fiber optics are readily available for Raman spectroscopy because of the use of visible and NIR light and do not require the exotic materials associated with FTIR fiber optics.) Preliminary tests for all samples were carried out using both 532 nm and 785 nm excitations, and it was determined that the 785 nm laser set gave an overall better balance between fluorescence and Raman scattering efficiency.</p><h4><strong>Summary&nbsp;</strong></h4><p>In this technical note, the analyses of a variety of samples by Raman spectroscopy are demonstrated. All samples were analyzed without sample preparation.&nbsp;</p><ul><li>Precise and localized analysis at the focal point of the Raman-exciting laser allows sampling through glass bottles, blister packaging and plastic containers, which eliminates possible cross contamination and analyst exposure to hazardous materials. The contributions from the packaging and containers depend on the type of container material, the container thickness, and the materials’ chemical compositional complexity, but these contributions can be readily subtracted out when needed.&nbsp;</li><li>Water is a weak Raman scatterer. Raman therefore has reduced water sensitivity, making it a preferred technique for aqueous solution analysis over FTIR. As demonstrated in the analysis of an energy drink, the Raman bands from water can be subtracted from the spectrum of the aqueous solution, leading to the identification of the components of the solution.&nbsp;</li><li>Raman spectroscopy is well suited for the analysis of inorganic materials, especially in identifying the crystal phases and polymorphs, as demonstrated by the analyses of minerals and pigments in a painting.&nbsp;</li><li>Fiber optic probes provide flexibility and ease of maneuverability. This is particularly advantageous when analyzing samples that are difficult to access or manipulate, such as large containers, geological samples and paintings</li></ul><p>The DXR3 Flex has multiple sampling options available. A properly configured fiber-optic probe is arguably the most versatile accessory for the analysis of bulk solids and liquids. The advantages, both from those inherent to Raman spectroscopy and those resulting from the use of fiber optic probe, provide opportunities for a wide variety of different applications when using the DXR3 Flex Raman Spectrometer.</p>

News from LabRulezGCMS Library - Week 19, 2026

<p><strong>🎤Francis Femi Oloy</strong></p><p><strong>In this episode of Concentrating on Chromatography, David speaks with Francis Femi Oloy about using chromatography to uncover hidden pollutants in real-world water systems.</strong></p><p>Femi’s team analyzed polychlorinated biphenyls (PCBs) in six major rivers in southwestern Nigeria — compounds that were banned decades ago but still persist in the environment. Using a workflow that many analytical labs will recognize — liquid–liquid extraction, cleanup, rotary evaporation, nitrogen blowdown, and GC-ECD detection — they quantified 25 PCB congeners at trace levels and linked the results to ecological and human health risk.</p><h4><strong>In this conversation, we cover:</strong></h4><ul><li>Why legacy pollutants like PCBs still show up today</li><li>Choosing GC-ECD vs LC-MS for halogenated compounds</li><li>Liquid–liquid extraction and matrix cleanup strategies</li><li>Why sample concentration is critical for dilute environmental samples</li><li>How rotovap + nitrogen blowdown work together without losing volatile analytes</li><li>Seasonal trends (why wet season levels were higher)</li><li>Translating concentration data into meaningful risk assessments</li></ul><h3><strong>Video Transcription</strong></h3><section><div><div><div><div><div><div><p><strong>Persistent organic pollutants</strong> such as polychlorinated biphenyls (<strong>PCBs</strong>) remain a significant environmental concern despite decades of regulatory restrictions. In this interview, Francais Femi Oloy discusses the environmental and analytical challenges associated with monitoring PCB contamination in rivers of southwestern Nigeria, a rapidly industrializing region where urban growth, industrial activity, agriculture, and dense populations intersect with extensive aquatic systems.</p><p>Oloy explains that his interest in environmental contaminant analysis emerged from observing unexplained health problems and environmental degradation while growing up in Nigeria. This motivated his transition into organic and environmental chemistry, with a focus on identifying pollutants present in drinking water, agricultural soils, and food systems. Southwestern Nigeria, particularly the Lagos region, represents a critical environmental monitoring area due to intense industrial development, shipping activity, and widespread human dependence on rivers for domestic use, agriculture, and fishing.</p><p>Although PCBs are considered “<strong>legacy pollutants</strong>” and are no longer intentionally produced, the interview highlights why they continue to persist in aquatic environments. Old electrical transformers and aging industrial equipment still contain PCB residues, while historical contamination stored in river sediments can become remobilized during flooding, dredging, or sediment disturbance. Because PCBs are hydrophobic and resistant to degradation, they preferentially accumulate in sediments and bioaccumulate through aquatic food chains, creating long-term environmental and human exposure risks.</p><p>A major focus of the discussion centers on the analytical workflow used for PCB determination in environmental water samples. Composite river water samples were collected in amber glass bottles to avoid contamination and photodegradation, preserved with sodium azide to minimize microbial activity, and stored under cooled conditions prior to extraction. The analytical protocol employed <strong>liquid–liquid extraction</strong> using dichloromethane (DCM) and hexane to recover both polar and nonpolar PCB congeners. Oloy emphasizes that liquid–liquid extraction was selected over solid-phase extraction (SPE) because of concerns about congener retention within sorbent materials and clogging issues associated with large-volume environmental samples.</p><p>Following extraction, concentration and cleanup represented critical analytical stages due to the trace-level occurrence and volatility of PCBs. Silica and alumina cleanup procedures were used to remove matrix interferences prior to instrumental analysis. The concentration workflow combined rotary evaporation for bulk solvent reduction with nitrogen blowdown for final volume reduction to less than 1 mL, while carefully avoiding excessive temperature or complete dryness to minimize analyte loss. Oloy repeatedly stresses that improper concentration procedures are among the most common causes of analytical failure in PCB analysis.</p><p>For instrumental determination, the study utilized <strong>gas chromatography coupled with electron capture detection (GC-ECD)</strong> rather than LC-MS or GC-MS. According to Oloy, GC was preferred because PCBs are sufficiently volatile for gas chromatographic separation, while ECD provided superior sensitivity and selectivity for chlorinated compounds at environmentally relevant concentrations. The interview also discusses analytical validation strategies, including the use of surrogate standards to assess <strong>recoveries,</strong> which ranged from approximately <strong>85% to 114%</strong>, and signal-to-noise-based determination of detection limits.</p><p>The study further examined <strong>seasonal variations in PCB concentrations</strong>, revealing <strong>higher levels during the wet season</strong>. This observation was attributed to rainfall-driven runoff from contaminated infrastructure, sediment resuspension, and lower temperatures that reduce volatilization losses. To communicate toxicological relevance beyond simple concentration reporting, the researchers also calculated <strong>toxic equivalency values (TEQs)</strong>, converting mixtures of PCB congeners into biologically meaningful toxicity estimates comparable to dioxin toxicity metrics.</p><p>Beyond environmental monitoring, Oloy highlights broader research interests focused on <strong>pollutant remediation and sustainable environmental protection</strong>. His group is also involved in developing catalytic materials capable of degrading or removing persistent contaminants from environmental systems. Throughout the discussion, he emphasizes that analytical chemistry plays a central role not only in detecting pollutants, but also in enabling prevention, remediation, and long-term environmental management strategies.</p></div></div></div></div></div></div></section><blockquote><p><strong>This text has been automatically transcribed from a video presentation using AI technology. It may contain inaccuracies and is not guaranteed to be 100% correct.</strong></p></blockquote><blockquote><h4><strong>Concentrating on Chromatography Podcast</strong></h4><p>Dive into the frontiers of chromatography, mass spectrometry, and sample preparation with host David Oliva. Each episode features candid conversations with leading researchers, industry innovators, and passionate scientists who are shaping the future of analytical chemistry. From decoding PFAS detection challenges to exploring the latest in AI-assisted liquid chromatography, this show uncovers practical workflows, sustainability breakthroughs, and the real-world impact of separation science. Whether you’re a chromatographer, lab professional, or researcher you'll discover inspiring content!</p><p>You can find <strong>Concentrating on Chromatography Podcast </strong>in podcast apps:</p><ul><li><a target="_blank" rel="noopener noreferrer" href="https://open.spotify.com/show/1wZg67rCjoGju4yhqxI3tL"><strong>Spotify</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://podcasts.apple.com/tz/podcast/concentrating-on-chromatography/id1788429185"><strong>Apple podcast</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://podscan.fm/podcasts/concentrating-on-chromatography"><strong>podscan</strong></a></li></ul><p>and on <a target="_blank" rel="noopener noreferrer" href="https://www.youtube.com/@ChromatographyTalk/videos"><strong>YouTube channel</strong></a></p></blockquote>

Tracking Toxic PCBs in River Water using Gas Chromatography–Electron Capture Detection

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The Fitness for Purpose of Analytical Methods

The third edition of Eurachem’s flagship guide provides updated, practical guidance on method validation, verification, sampling, and fitness for purpose, aligned with ISO/IEC 17025:2017.

<h3><strong>The Fitness for Purpose of Analytical Methods: A Laboratory Guide to Method Validation and Related Topics: Third edition (2025)</strong></h3><p><strong>Author: </strong>H. Cantwell</p><p>This guide was first issued in 1998 and the second edition published in 2014. Over the years it has been one of the most popular of the Eurachem guides. Since the release of the first edition, however, there have been many changes in terminology, working practices, reference documents and requirements. This third edition, produced by the Eurachem Method Validation Working Group, forms a thorough revision of the 2014 edition.</p><p>This third edition includes a section on sampling and sample handling as <strong>ISO/IEC 17025:2017</strong> introduced a focus on sampling associated with the testing or calibration being carried out by the laboratory and further guidance on assessing the calibration function has been included. The Guide is also now supported by a number of supplementary guidance documents – please see the section on supplementary guidance below.</p><h4><strong>Contents</strong></h4><p>This third edition includes guidance on:</p><ul><li>The importance of fitness for purpose;</li><li>The concept of method validation and verification;</li><li>How a method validation or verification study should be performed and how much should be done;</li><li>Sampling and sample handling in relation to method validation;</li><li>A thorough explanation of the various validation parameters (performance characteristics) and related topics;</li><li>Follow-up on the validation study (reporting, use of performance data in Internal Quality Control);</li><li>Documentation of analytical methods.</li></ul><p>Annexes also describe the statistical basis of detection limits and analysis of variance for precision studies, and add a check list to aid users in selecting and determining the validity of a test kit.</p><p>In preparing this guidance, the Working Group has aimed at the right balance between giving a solid theoretical background for method validation studies and providing practical guidelines on how to plan, perform and evaluate such studies in the laboratories.</p><p>The approach is generic in the sense that the Guide does not focus on particular fields of application (food, environment, pharmaceuticals etc.). However, the guide includes references to a number of specific guides in fields where different practices have been developed and become common.</p><p>The guide also includes a full bibliography. Further literature references on method validation can be found in the section "Validation of analytical methods" in the Reading list on this website.</p>

Terminology in Analytical Measurement: Introduction to VIM 3

This Eurachem guide introduces VIM 3 terminology relevant to analytical laboratories, explaining key metrological concepts for chemical, biological, and clinical measurements with practical examples.

<h3><strong>Terminology in Analytical Measurement: Introduction to VIM 3 (Second Edition 2023)</strong></h3><p><strong>Author: </strong>V. J. Barwick (Ed.)</p><h4><strong>Contents</strong></h4><p>This guide has been produced by members of the Eurachem Education and Training Working Group and others co-opted to the Project group for this task.</p><p>In the world of metrology – the science of measurement and its application – there is a language which has to be learned. The International Vocabulary of Metrology (VIM) was produced to provide a common language, primarily for physical measurements. The VIM 3 is a consistent set of concepts each described by a unique term, the ‘label’ of the concept. VIM 3 is applicable across all scientific disciplines thus making it relevant to those involved in performing measurements in chemistry and biology. Consistent definitions of concepts with their associated terms and symbols are essential if analysts and customers across the globe are to understand each other.</p><p>This Eurachem Guide discusses a selection of the concepts in VIM 3, focusing on those most likely to be encountered in analytical laboratories. It aims to cover chemical, biological and clinical measurements and gives examples over and above those in the notes accompanying the definitions in VIM 3. The guide is intended for laboratory staff, accreditation bodies, for those commissioning measurements and for those using measurement results. Lecturers and trainers may also find this guide useful when teaching aspects of metrology.</p><p>In this second edition the scope and structure, and the terms and concepts discussed, remain unchanged from the first edition. However, all sections have been reviewed and, where necessary, the text has been revised to improve clarity and ensure consistency with current international guidance at the time of publication.</p>

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Tracking Toxic PCBs in River Water using Gas Chromatography–Electron Capture Detection

EU Regulation 396/2005: Pesticide Residue Testing and the Critical Role of QuEChERS Evaporation in Food Safety

News from LabRulezGCMS Library - Week 19, 2026