<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 23rd June 2025? 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>posters by <strong>Agilent Technologies / ASMS </strong>and<strong> Thermo Fisher Scientific / ASMS </strong>and presentation by<strong> William &amp; Mary / MDCW!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Improved Determination of Polychlorinated Biphenyl Compounds by US EPA Method 1628</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_5977c_pcb_hydroinert_column_asms_2025_mp_360_en_agilent_8db06d5b24.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>Polychlorinated Biphenyl (PCBs) and the Environment&nbsp;</strong></h5><p>Polychlorinated Biphenyls (PCBs) are synthesized compounds that belong to the chlorinated hydrocarbon family of compounds. PCBs were used in a variety of industrial applications such as electrical components, plasticizers and pigments/dyes, until they were banned in 1979 by the Toxic Substances Control Act (TSCA)<sup>1</sup> . PCBs are considered to persistent organic pollutants (POPs) as they do not easily degrade in the environment. PCBs can be found in the air, water, and soil and have been known to bioaccumulate in marine life.</p><p>The EPA has recently developed a low-resolution mass spectrometry method that can calibrate 65 PCBs congeners and screens for all 209 using labeled PCB compounds for direct and indirect quantitation<sup>2</sup> . The 65 congeners are targeted for calibration and quantitation due to specific factors described in the method<sup>2</sup> . As with most EPA methods, the prescribed methodology utilizes helium as a carrier gas. The recommended column for this analysis makes adequate separation and quantitation more challenging. To achieve separation that meets the method criteria, the run time is over 40 minutes long. By using a column better suited for PCB congener separation and hydrogen as the carrier gas, superior separation can be achieved in under 20 minutes, resolving previously co-eluting analytes.</p><h4><strong>Experimental&nbsp;</strong></h4><h5><strong>System configuration using hydrogen carrier gas&nbsp;</strong></h5><p>The Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890%2F5977C+GC%2FMSD"><strong>8890/5977C GC/MSD</strong></a> equipped with the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=HydroInert+Ion+source"><strong>HydroInert Ion source</strong></a> was operated in selective ion monitoring (SIM) mode for this analysis.</p><h4><strong>Conclusions</strong></h4><h5><strong>Faster Analysis, Superior Separation Achieved&nbsp;</strong></h5><ul><li>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=DB-XLB+column"><strong>DB-XLB column</strong></a> offers enhanced selectivity for PCB congeners, resulting in previously co-eluting congeners to separate.&nbsp;</li><li>Selectivity is easily achieved operating the MSD in SIM mode.&nbsp;</li><li>The method meets the 10ppb detection limit for all the quantified compounds.</li><li>The HydroInert ion source allows hydrogen carrier gas to be used for more rapid analysis.</li></ul><h3><strong>2. Shimadzu: Simultaneous Analysis of Synthetic Musk Compounds in Water Using a Triple Quadrupole GC-MS System</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_09_ssk_020_en_4ae628cef8.pdf"><strong>Full PDF for download</strong></a></li></ul><p><strong>User Benefits:</strong></p><ul><li>Using a GC-MS/MS, synthetic musk compounds in water can be accurately quantified with high sensitivity.</li><li>Supporting effective environmental monitoring in water and risk assessment using GC-MS/MS</li></ul><p>Synthetic musk compounds (SMCs) are synthetic organic substances designed as substitutes for natural musk and are widely used in various household products. During everyday activities such as showering and washing, these compounds are released into wastewater. However, current wastewater treatment processes cannot completely remove SMCs, allowing them to enter aquatic ecosystems. As highly bio-accumulative organic compounds, SMCs can cause both acute and chronic toxicity in aquatic organisms. They are also known to cause endocrine disruption when accumulated in the human body1-3) . Due to these potential risks, continuous monitoring of SMCs in water is essential. The main analytical methods for detecting SMCs in water include liquid-liquid extraction (LLE), solid-phase extraction (SPE), and solid-phase microextraction (SPME). Liquid-liquid extraction method requires a large amount of solvent and long preparation time but has the advantage of simultaneously extracting multiple organic compounds 4) . In this application news, 15 types of SMCs in water were simultaneously analyzed using the gas chromatography method with liquid-liquid extraction method.</p><h4><strong>Analytical conditions</strong></h4><p>In this newsletter, SMCs in water were analyzed using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-TQ8050+NX"><strong>GCMSTQ8050 NX</strong></a> of SHIMADZU (Figure 1). The instrumental detailed analytical conditions of instrument and the MRM conditions for each compound were shown in Table 1 and 2, respectively.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>The simultaneous analysis of 15 SMCs in water was performed using the SHIMADZU GCMS-8050 NX system. The coefficient of determination(R2) of the calibration curve for all SMCs were 0.99 or higher. The LOD and LOQ were ranged from 0.003 to 0.020 ng/mL and 0.01 to 0.07 ng/mL, respectively. The recovery test results were between 86.3 % and 106.4 %, with a relative standard deviation (RSD) of 0.7 % to 4.2 %. This analytical method, using a GC-MS/MS system, provided reliable quantitative results for 15 synthetic musk compounds in water samples and demonstrated high sensitivity and efficiency.</p><h3><strong>3. Thermo Fisher Scientific / ASMS: Performance evaluation of GC-MS/MS for Dioxin analysis with amendments to EU Regulations 644/2017 and 771/2017 for food and feed&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PO_298_ASMS_25_performance_evaluation_GC_MS_MS_dioxin_analysis_po298_na_en_8721a5f8dc.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Polychlorinated dibenzo-p-dioxins/furans (PCDD/F), or dioxins, are persistent organic pollutants (POPs) that can accumulate within food chains due to their chemical stability and high fat solubility, posing health risks to humans through food consumption<sup>1</sup> . Current regulations monitor food and feed for dioxins, with maximal allowable levels for PDCC/Fs in feedstuffs at the pg•g-1 concentration range<sup>2</sup> . However, a recent review process has proposed a reduction of up to 40% in these levels by 2024 for certain feed items, such as animal/milk/egg fats (1.0 pg•g-1), fish oil (3.5 pg•g-1), and fish feed (1.0 pg•g-1)<sup>3</sup> . Since 2014, the European Commission has permitted the use of gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) for food and feed analysis as an alternative to GC-high resolution mass spectrometry (HRMS)<sup>4,5</sup> . With the proposed reduction in maximum limits, the performance of current instrumentation to achieve these targeted limits must be assessed.</p><p>Laboratories face challenges in maintaining consistent sensitivity to detect trace levels of dioxins in complex food matrices and in reporting various regulatory requirements for PCDD/ F analysis<sup>6,7</sup> . This study used the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/485"><strong>Thermo ScientificTM TSQTM 9610 triple quadrupole GC-MS/ MS</strong></a> system with the NeverVentTM advanced electron ionization (AEI) source to demonstrate compliance with the proposed regulatory limits for PCDD/F in food and feed samples. The aim was to ensure consistency with previously determined concentrations of PCDD/F in food and feed matrices and meet current compliance with the EU regulations.</p><h4><strong>Materials and methods</strong></h4><p>Data was acquired, processed, and reported using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Thermo Scientific Chromeleon Chromatography Data System (CDS) software</strong></a>, version 7.3. Integrated instrument control ensures full automated setup of the Dioxin analytical workflow through the eWorkflow which provides optimized instrument / quantification methods, view settings for time efficient data evaluation and customizable report templates. Isotopic dilution quantification is performed automatically in real time with the incorporated custom variable and formula functionality eliminating the need for exporting to external software packages.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>The results of these comprehensive experiments demonstrate that the TSQ 9610GC-MS/MS system, configured with the NeverVent AEI source and controlled using Chromeleon CDS software together with the Dioxin eWorkflow, can deliver reliable regulatory compliant performance for the quantification and confirmation ofPCDD/Fs food and feedstuffs:&nbsp;</p><ul><li>Fentogram level sensitivity performance for ultra trace level determination of PCDD/F within food and feed samples&nbsp;</li><li>Check standard performance was within quantitation and ion ratio thresholds for regulatory method compliance at femtogram levels.&nbsp;</li><li>Accurate and precise quantitation at both current and newly adopted maximum limits for PCDD/F in food and feed.&nbsp;</li><li>Chromeleon CDS software, version 7.3, provides an integrated platform, with the ability to automatically setup, easily acquire, process and report compliant data in a fully regulated environment, eliminating the need for using external spreadsheet programs.&nbsp;</li><li>Chromeleon eWorkflows, available from Thermo Scientific also provide error-free execution of each analysis to meet standard operating procedure (SOP) requirements, further simplifying the user</li></ul><h3><strong>4. William &amp; Mary / MDCW: Method optimization of fingermark residue using comprehensive two-dimensional gas chromatography&nbsp;</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/FL_07_Macturk_MDCW_2025_Oral_Presentation_4c2c820f98.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Fingermarks—smudged or incomplete fingerprints—may lack value for direct identification but can still offer critical information through their chemical residue. This study explores the potential of nontargeted chemical analysis of fingermark residue to determine donor characteristics such as sex and age. Using comprehensive two-dimensional gas chromatography (GC×GC), the team sought to enhance analytical resolution and method efficiency.</p><h4><strong>Experimental Approach</strong></h4><p>Researchers first collected fingermark residue using cotton swab extraction, followed by centrifugation and sample preparation. A GC×GC method was optimized by adjusting parameters like modulation period, hot pulse time, oven hold times, and ramp rate. Multiple method configurations were tested for chromatographic resolution, and the optimized helium-based method was later translated for use with hydrogen carrier gas using modeling tools.</p><h4><strong>Results</strong></h4><p>Method optimization led to significant improvements in peak separation, enabling identification of various compound classes including sterols, fatty acid methyl esters, fatty alcohols, and steroids. Additionally, unexpected anthropogenic substances such as sunscreen agents and plasticizers were detected. Hydrogen-based methods were able to achieve comparable separation quality, with the “H₂ Translate” method offering the highest number of identifiable peaks.</p><h4><strong>Conclusion</strong></h4><p>This study demonstrates that nontargeted GC×GC analysis is effective for resolving both endogenous and exogenous compounds in fingermark residue. The optimized methods not only improve forensic chemical profiling but also support a successful transition from helium to hydrogen as a carrier gas—promoting sustainability without compromising analytical performance.</p>

News from LabRulezGCMS Library - Week 26, 2025

GC–MS as a valuable tool for analysing cannabinoid-containing gummies and identifying the synthetic process used for their production

<p><strong>In the week of June 30, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.</strong></p><blockquote><p><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></p><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>4 500 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. Agilent Technologies: From Insights to Outcomes: Real-World Optimization of Lab Operations Using CrossLab Connect Digital Services</strong></h5><ul><li>Already taken place Monday, June 30, 2025</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5256">Registration</a></li></ul><p>Discover how labs capitalize on utilization and service data with CrossLab Connect. Case studies show how informed decisions drive cost savings, productivity gains, and sustainability progress.</p><h5><strong>2. Agilent Technologies: Go Beyond Limits in Pesticide Analysis: Watch, Ask, Connect with Agilent</strong></h5><ul><li>Already taken place Monday, June 30, 2025</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5262">Registration</a></li></ul><p>Watch the webinars, submit your question and join us for live Q&amp;A session on June 30 to consult directly with Agilent experts and gain practical insights on pesticide analysis.</p><h5><strong>3. Agilent Technologies: Optimizing Laboratory Procurement with Digital Services: Take Control of Your Laboratory Spend with Agilent CrossLab Connect</strong></h5><ul><li>Tuesday, July 1, 2025, 16:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5257">Registration</a></li></ul><p>Learn how labs use CrossLab Connect to optimize CapEx &amp; OpEx, avoid unnecessary instrument purchases, and fine-tune service coverage using risk-based, data-driven insights and real case studies.</p><h5><strong>4. Wasson-ECE Instrumentation: Data Handling Software: OpenLab Chemstation vs OpenLab CDS</strong></h5><ul><li>Tuesday, July 1, 2025, 21:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5276">Registration</a></li></ul><p>Explore how OpenLab CDS enhances chromatography workflows by integrating features from ChemStation, EZChrom, and MassHunter to boost usability, productivity, and user experience.</p><h5><strong>5. Agilent Technologies: Biopharmaceutical Raw Material Verification with Handheld Vaya Raman Spectrometer</strong></h5><ul><li>Thursday, July 3, 2025, 20:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/2770">Registration</a></li></ul><p>The Agilent Vaya handheld Raman spectrometer increases raw material identification throughput without increasing costs by reducing the need for sampling.</p>

Webinars LabRulezGCMS Week 27/2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 30th June 2025? 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 other document by <strong>Agilent Technologies </strong>and<strong> </strong>posters by<strong> Shimadzu / ASMS, Thermo Fisher Scientific / ASMS </strong>and <strong>Waters / ASMS</strong>!</p><h3><strong>1. Agilent Technologies: Understanding Solvent Focusing Gas Chromatography and How it can be Optimized for Splitless Injections&nbsp;</strong></h3><ul><li>Other document (white paper)</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/wp_solvent_focusing_gc_5994_8387en_agilent_7911ade217.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Discussions of the basic mechanism of gas chromatography (GC), samples can start as a liquid, solid, or a gas. These samples, when not in gas phase, are converted into a vapor made up of solvent and analytes that are then separated using a GC column. The type of film or stationary phase used in the column helps to separate the compounds of a sample mixture. Meanwhile, the role of the gaseous mobile phase is to move compounds through the column without chemically interacting with them.1 With splitless injections, almost the entire sample is transferred onto the column head, making it ideal for trace level analysis, but more susceptible to solvent interactions due to the large volume of solvent also introduced to the column. It is important to understand all the variables and how to optimize them to successfully perform splitless injections, including the role of the sample solvent and related solvent effects.</p><h4><strong>Sample preparation and solvent selection</strong></h4><p>Prior to efficient sample preparation methods for the analysis of pesticides, a guard column was used to help protect the analytical column from heavy matrix or nonvolatile analytes. The primary method of sample preparation used was solvent dilution in hexane or dichloromethane, which potentially passed through a filter, and then injected directly into the inlet and analyzed on a 5% phenyl phase type column. This can be referred to as the dilute and shoot method. As dichloromethane and hexane are both compatible solvents with a 5% phenyl phase, the guard column was only needed to protect the analytical column from matrix, and not from adverse&nbsp;wettability.&nbsp;</p><p>With the adoption of more involved sample preparation techniques, traditionally used in liquid chromatography, samples typically finish their preparation in the polar solvent acetonitrile. For GC analysis solvent exchange is employed, which is the process of drying down a sample in one solvent under nitrogen gas and reconstituting it in another solvent such as hexane. This procedure is performed to ensure proper interactions between solvent and column phase. Since these cleaned up samples contained less matrix, the need for a guard column was decreased.6 Gradually the requirement for solvent exchanges was decreased to decrease the overall sample preparation time, but this left the prepared samples in a final solvent of acetonitrile.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>For a gas chromatography analysis to be successful there are many factors to be considered. These factors include injection speed, solvent choice, installation of the column, and the column phase selection. Solvent selection is important in more decisions than determining which solvent will dissolve analytes. Solvent selection can impact vaporization volume in the liner, as well as impact reconcentration at the head of the GC column.&nbsp;</p><p>Splitless&nbsp;injections will be more affected by solvent selection, as there will be a greater amount of solvent introduced to the column and greater interactions between the solvent and column phase. If the solvent and column phase are mismatched, there will be an increase in the flooded zone, and a subsequent impact to the peak shape of analytes. To mitigate the problem of using a polar solvent with a nonpolar column, a guard column can be used to help refocus the solvent and analytes at the head of the analytical column and improve analyte peak shape.</p><h3><strong>2. Shimadzu / ASMS: PFAS in Bottled Water: A Simple Approach Using HS-SPME GC/MS/MS for Volatile Contaminant Analysis</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_25_TP_312_a610778a69.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Concerns about per- and polyfluoroalkyl substances (PFAS) contamination in bottled water, linked to significant health risks, are growing. The Food and Drug Administration (FDA) has published plans surveying bottled water for PFAS in 2024-2025. While Liquid Chromatography/Mass Spectrometry (LC/MS) is the primary analytical method for PFAS, it struggles to analyze certain PFAS related compounds like fluorotelomer alcohols (FTOHs), perfluoroalkyl iodides (PFIs), and (n:2) fluorotelomer iodides (FTIs). Gas Chromatography/Mass Spectrometry (GC/MS) offers a complementary approach for volatile PFAS. This study utilizes Head-Space Solid Phase Microextraction Triple Quadrupole Gas Chromatography/Mass Spectrometry (HS-SPME GC/MS/MS) to analyze PFAS in bottled water. This technique offers several advantages, including minimal sample preparation, making it a valuable tool for comprehensive PFAS analysis.</p><h4><strong>Methods</strong></h4><p>A volatile PFAS analysis method was developed on a Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-TQ8040+NX"><strong>GCMS-TQ8040 NX</strong></a> with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=AOC-6000+Plus"><strong>AOC-6000 Plus</strong></a> multifunctional autosampler equipped with a solid phase microextraction (SPME) module (Figure 1).&nbsp;</p><p>Thirteen PFAS target compounds were included in the Multiple Reaction Monitoring (MRM) method. The PFAS chemical classes were perfluoroalkyl iodides (PFIs), (n:2) fluorotelomer iodides (FTIs), (n:2) fluorotelomer acrylates (FTACs), (n:2) fluorotelomer methacrylates (FTMACs), (n:2) fluorotelomer alcohols (FTOHs) and perfluoroalkane sulfonamides (FASAs). Internal standards (IS) FTOHs, FASAs and FTAC mass-labelled compounds were added to each vial prior to extraction. Concentrations of the target compounds were calculated using isotope dilution.&nbsp;</p><p>An internal calibration curve was prepared in 10 mL of reagent water at concentrations of 2000, 1000, 500, 100, 50, 10, 2.5 and 1 ng/L. The IS were spiked at 100 ng/L to each calibrator. Sodium Chloride (NaCl) was added to each vial to achieve a final salinity concentration of 2% NaCl (w/v). These calibrators were vortex for 30 seconds and then placed on the AOC-6000 Plus autosampler rack for analysis.&nbsp;</p><p>The optimized parameters of the HS-SPME GC/MS method for the targeted PFAS are listed in table 1. Quantitative and reference ions for each PFAS target are listed in table 2. The associated internal standard used for each compound is also listed in table 2.&nbsp;</p><p>A laboratory control sample (LCS) was analyzed to determine the general performance of the method in a clean matrix. The bottled water samples were analyzed to determine the effect of matrix on method performance. The type of bottled water analyzed was purified water.</p><h4><strong>Conclusion</strong></h4><p>The PFAS family includes thousands of compounds across diverse chemical classes, making comprehensive analysis challenging and often necessitating multiple analytical techniques. LC-MS is widely used and well-established for PFAS analysis but is less effective for detecting certain compounds - particularly volatile PFAS. In contrast, GC-MS excels at analyzing volatile PFAS and serves as a valuable complement to LC-MS, offering a more complete and balanced approach to PFAS detection. By extending the range of detectable compounds, GC-MS helps overcome PFAS analysis limitations previously imposed by instrumentation constraints. This study demonstrates the strong performance of an HS-SPME GC/MS/MS method for measuring volatile PFAS in bottled water. The application presents a simple, rapid, robust, precise, and accurate workflow that significantly improves the ability to detect a broader spectrum of PFAS compounds in bottled water.</p><h3><strong>3. Thermo Fisher Scientific / ASMS: Large-scale targeted biomarker analysis of volatile organic compounds in breath by TD-GC-MS&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PO_456_ASMS_25_large_scale_targeted_biomarker_analysis_po456_na_en_910bf58c57.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Breath analysis of volatile organic compounds (VOCs) is emerging as a promising tool in non-invasive disease diagnostics. While untargeted methods dominate current workflows, they often lack reproducibility and specificity. This study introduces a fully integrated, large-scale targeted workflow for VOC biomarker quantification using TD-GC-MS, aiming to support the development of Owlstone Medical’s Breath Biopsy VOC Atlas® and broader breathomics applications.</p><h4><strong>Materials and Methods</strong></h4><p>Breath samples were collected using the ReCIVA® Breath Sampler and CASPER® air supply to reduce ambient contamination. Samples were analyzed with a <strong>Markes </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=7&amp;search=TD100xr+thermal+desorber"><strong>TD100xr thermal desorber</strong></a><strong> </strong>coupled to a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/18"><strong>Thermo Scientific Orbitrap Q Exactive GC-MS system</strong></a>, known as the Breath Biopsy OMNI® method. A total of 200 VOC targets were monitored, using 36 deuterated internal standards. All data acquisition and analysis were performed in <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Chromeleon CDS software</strong></a> in a secure, cloud-based enterprise environment.</p><h4><strong>Results</strong></h4><p>The workflow includes automated system suitability and intelligent run controls (SST/IRC) to avoid the loss of valuable patient samples. High-confidence compound identification was achieved using composite scoring, ion ratio matching, and HRAM spectral libraries. Method validation across two independent breath sample cohorts demonstrated strong precision, with over 70% of VOCs meeting the &lt;20% RSD threshold across studies and sequences.</p><h4><strong>Conclusion</strong></h4><p>This targeted TD-GC-MS workflow provides a robust, compliant, and scalable solution for high-confidence breath biomarker analysis. The integration of cloud-based Chromeleon CDS, automated QC protocols, and HRAM detection supports reproducible, high-throughput studies that are essential for advancing clinical breathomics and precision medicine.</p><h3><strong>4. Waters / ASMS: GC-APCI-MS/MS Analysis of Polychlorinated Dibenzo-p-dioxins and Furans to Revised US EPA1613 Guidelines</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008849_81ffe9aec9.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In response to the U.S. EPA’s 2024 update of Method 1613 for the analysis of PCDD/Fs in wastewater, this study evaluates the performance of an alternative workflow using tandem quadrupole mass spectrometry (MS/MS) with APCI instead of traditional high-resolution mass spectrometry (HRMS). The goal was to demonstrate that such a system can meet all critical quality control (QC) metrics required by the revised method.</p><h4><strong>Materials and Methods</strong></h4><p>Analysis was carried out using a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/55"><strong>Waters Xevo TQ-XS tandem quadrupole MS</strong></a><strong> </strong>with an APGC™ source, coupled to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890+GC"><strong>Agilent 8890 GC</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=8&amp;search=CIS-4+PTV"><strong>Gerstel CIS-4 PTV injector</strong></a>, with <strong>autosampling via </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=PAL+3+RSI"><strong>PAL 3 RSI</strong></a>. Chromatographic separation used a Restek Rtx-Dioxin2 column. Calibration standards from Wellington Laboratories were diluted to test both linearity and detection limits, and internal QC metrics were adapted to accommodate the MS/MS platform.</p><h4><strong>Results</strong></h4><p>The adapted workflow successfully replicated key EPA1613 QC checks, including relative response factors, isotopic ratios (±15%), and detection limits. The system showed excellent mass accuracy and resolution, verified through an automated Python-based script. Ionization suppression events were detected and visualized, aiding sample quality assessment. Signal-to-noise ratio evaluation, even in low-noise MS/MS traces, was possible after modifying detector settings.</p><h4><strong>Conclusion</strong></h4><p>This work proves that a GC-APCI-MS/MS system can fully comply with revised EPA1613 guidelines. The platform demonstrated robust quantitative performance, reproducibility, and reliable QC monitoring. It represents a valid and cost-effective alternative to HRMS for regulatory dioxin and furan analysis in environmental samples.</p>

News from LabRulezGCMS Library - Week 27, 2025

NDMA in macrolides: GC-MS/MS method for its detection and study of its formation

<p><strong>In the week of July 7, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.</strong></p><blockquote><p><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></p><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>4 500 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. Wasson-ECE Instrumentation: Introduction to the Micro GC, Use of Autosamplers with the uGC</strong></h5><ul><li>Tuesday, July 8, 2025, 21:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5304">Registration</a></li></ul><p>Do you know about Wasson-ECE’s MicroGCs? Join us for an introduction to Micro-GCs and their use with autosamplers.</p><h5><strong>2. Agilent Technologies: Cutting through pesticide residues and heavy metals</strong></h5><ul><li>Wednesday, July 9, 2025, 06:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4868">Registration</a></li></ul><p>This webinar focuses on pesticides and heavy metals detection, along with performing elemental speciation in dairy products by LC/MS/MS, GC/MS/MS, and ICP-MS techniques.</p><h5><strong>3. Separation Science: From Peaks to Insights: Navigating Environmental Analysis with Weck Laboratories using GC/MS/MS Instrumentation</strong></h5><ul><li>Wednesday, July 9, 2025, 11:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5259">Registration</a></li></ul><p>Discover the benefits of using triple quadrupole GC/MS in high-throughput environmental testing workflows.</p><h5><strong>4. Metrohm: Amplifying the Invisible: Advanced Spectroelectrochemistry with EC-SERS</strong></h5><ul><li>Wednesday, July 9, 2025, 19:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5285">Registration</a></li></ul><p>Learn how Raman spectroelectrochemistry empowers time-resolved redox analysis by combining spectroscopy with electrochemistry—featuring SERS and real-world research applications.</p><h5><strong>5. Thermo Fisher Scientific: MOSH MOAH Analysis Made Clear: Strategies for Diverse Matrices</strong></h5><ul><li>Thursday, July 10, 2025, 08:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5305">Registration</a></li></ul><p>Join our upcoming webinar to learn from our experts about advanced MOSH/MOAH analysis techniques designed to tackle diverse matrices with exceptional efficiency and precision.</p><h5><strong>6. Agilent Technologies: Surface Measurement and Beyond – Nondestructive Testing with Handheld FTIR and SORS Raman Spectroscopy</strong></h5><ul><li>Thursday, July 10, 2025, 11:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5298">Registration</a></li></ul><p>Join us for an engaging webinar! Agilent portable SORS Raman and FTIR systems are simplifying in situ chemical analysis.</p>

Webinars LabRulezGCMS Week 28/2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 7th July 2025? 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 posters by <strong>Agilent Technologies / ASMS, Shimadzu / ASMS, </strong>presentation by<strong> Liège University / MDCW </strong>and technical note by<strong> Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Analysis of Allergens in Fragrance Samples Using a Comprehensive GCxGC in Combination with a High-Resolution Mass Spectrometry&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_gc_gc_7250_allergens_asms_2025_mp_353_en_agilent_3459141f12.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Fragrances are highly complex mixtures that combine natural and synthetic components. Analytical separation of these samples on a single GC column results in coelution of isomers and structurally similar compounds which produce similar spectral fragmentation patterns. This significantly complicates identification and quantitative analysis of individual components of the fragrances. Here we demonstrate a power of a comprehensive GCxGC approach combined with high resolution MS for identification and quantitative analysis of 64 allergens in fragrances. With added confidence in compound identification provided by accurate mass, this approach also streamlines a non-targeted analysis of the fragrances to determine their composition.</p><h4><strong>Experimental</strong></h4><p>The samples were separated on an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC"><strong>8890 GC</strong></a> using a comprehensive GCxGC configuration with a reverse flow modulator (RFM). The non-polar/mid-polar column set was used and comprised of a 20m x 0.1mm x 0.1um DB-1ms column (100% Dimethylpolysiloxane) coupled to a 5m x 0.25mm x 0.15um DB-17ms column (equivalent to (50%-phenyl)- methylpolysiloxane). Optimized instrumental parameters are shown in Table 1.</p><p>The data were acquired using the high-resolution <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7250+GC%2FQ-TOF"><strong>7250 GC/Q-TOF</strong></a> at data rate of 50 Hz. For compound identification the Unknown Analysis tool of <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+Quantitative+Analysis"><strong>MassHunter Quantitative Analysis</strong></a> software version 12.1 and the GC Image software version 2024 R3 were used. The linear retention indices (RIs) were used to increase confidence in compound identification. Statistical analysis was performed in Mass Profiler Professional (MPP) software version 15.1.</p><h4><strong>Results and Discussion</strong></h4><h5><strong>GCxGC Configuration&nbsp;</strong></h5><p>A GCxGC RFM method was developed to achieve an optimal chromatographic separation of all the allergens while also ensuring adequate sensitivity and carrier gas flow to the MS. GCxGC RFM setup included two detectors: the Q-TOF MS and the FID. The configuration provided an optimal flow to the MS of 1.3 mL/min (11.8% of total flow) maintaining a constant split between FID and MS throughout the entire oven temperature ramp. The configuration is shown in Figure 2.</p><h4><strong>Conclusions</strong></h4><ul><li>Allergens in fragrance samples have been analyzed using comprehensive GCxGC combined with the highresolution GC/Q-TOF and RFM.&nbsp;</li><li>Fragrances with different types of aroma were analyzed using the GCxGC/HRMS combined with statistical analysis to identify the major differentiating compounds that may contribute to the particular type of scent.</li></ul><h3><strong>2. Liège University / MDCW: Coupling of Vac-HS-SPME and GC×GC-qMS for simultaneous 5-HMF quantification and volatile profiling in honey</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/FL_01_Honey_Eggermont_D_c3a35d2053.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The presentation by D. Eggermont et al. explores a novel analytical approach for assessing honey quality and authenticity. The method focuses on the simultaneous quantification of 5-hydroxymethylfurfural (5-HMF)—a key marker of honey freshness, heat exposure, and compliance with EU regulations—and the untargeted profiling of semi-volatile organic compounds (sVOCs).</p><p>The core of the method is <strong>vacuum-assisted headspace solid-phase microextraction (Vac-HS-SPME)</strong>, which improves extraction efficiency for low and semi-volatiles by reducing gas-phase resistance and accelerating mass transfer. This is followed by <strong>comprehensive two-dimensional gas chromatography coupled with quadrupole mass spectrometry (GC×GC-qMS)</strong>, enabling high-resolution separation and detection of both derivatised 5-HMF and various sVOCs such as benzaldehyde, furfuralcohol, phenylethanol, and menthofuran.</p><p><strong>Instrumentation used in the method includes:</strong></p><ul><li><strong>SPME fiber:</strong> DVB/CAR/PDMS (1 cm)</li><li><strong>Thermal desorption and focusing:</strong> Markes and SepSolve</li><li><strong>GC×GC system: </strong>Shimadzu platform with apolar × polar column set</li><li><strong>Mass spectrometer:</strong> Quadrupole MS operated in SIM mode for targeted 5-HMF quantification and full scan for volatile profiling</li></ul><p>The method was rigorously validated (LoQ 4.7 µg/g, LoD 1.6 µg/g, recovery 98%, precision RSD 21%) and compared against HPLC-UV as the official method, showing comparable results with lower sample amounts and fewer preparation steps. Additionally, the technique aligns with green analytical chemistry principles due to its miniaturization, low solvent use, and energy efficiency. This makes it a promising tool for routine honey analysis and food quality control.</p><h3><strong>3. Shimadzu / ASMS: Advancing PFAS Detection in Drinking Water: GC-MS as a Complementary Technique to LC-MS for Closing PFAS Mass Balance</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_25_WP_133_fcfd7e41b2.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Analysis of per- and polyfluoroalkyl substances (PFAS) in the environment is pivotal. There are several standardized PFAS methods, such as EPA 533, 537.1 8327, 1633, OTM-45 and OTM 50. Most of these methods are based on Liquid Chromatography/Mass Spectrometry (LC/MS) techniques. However, LC/MS is not suitable to analyze all PFAS compounds because of the diverse physico-chemical properties of chemicals within the PFAS family. Gas Chromatography/Mass Spectrometry (GC/MS) as a complementary technique can address volatile PFAS compounds that are challenging to analyze by LC/MS. In this study, a Head-Space Solid Phase Microextraction Triple Quadrupole Gas Chromatography/Mass Spectrometry analytical method is used to analyze PFAS in drinking water. This technique has advantages of analyzing volatile PFAS in water with minimum sample preparation procedure.</p><h4><strong>Methods</strong></h4><p>A volatile PFAS analysis method was developed on a Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ8040"><strong>GCMS-TQ8040</strong></a> NX with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=AOC-6000+Plus"><strong>AOC-6000 Plus</strong></a> multifunctional autosampler equipped with a solid phase microextraction (SPME) module (Figure 1).&nbsp;</p><p>Thirteen PFAS target compounds were included in the Multiple Reaction Monitoring (MRM) method. The PFAS chemical classes were perfluoroalkyl iodides (PFIs), (n:2) fluorotelomer iodides (FTIs), (n:2) fluorotelomer acrylates (FTACs), (n:2) fluorotelomer methacrylates (FTMACs), (n:2) fluorotelomer alcohols (FTOHs) and perfluoroalkane sulfonamides (FASAs). Internal standards (IS) FTOHs, FASAs and FTAC mass-labelled compounds were added to each vial prior to extraction. Concentrations of the target compounds were calculated using isotope dilution.&nbsp;</p><p>An internal calibration curve was prepared in 10 mL of reagent water at concentrations of 2000, 1000, 500, 100, 50, 10, 2.5 and 1 ng/L. The IS were spiked at 100 ng/L to each calibrator. Sodium Chloride (NaCl) was added to each vial to achieve a final salinity concentration of 2% NaCl (w/v). These calibrators were vortex for 30 seconds and then placed on the AOC-6000 Plus autosampler rack for analysis.</p><p>The optimized parameters of the HSSPME GC/MS method for the targeted PFAS are listed in table 1. Quantifier and qualifier ions for each PFAS target are listed in table 2. The associated internal standard used for each compound is also listed in table 2.&nbsp;</p><p>A laboratory control sample (LCS) was analyzed to determine the general performance of the method in a clean matrix. Drinking water analyzed in the study were from a private well and an utility with surface water as its source.</p><h4><strong>Conclusion</strong></h4><p>This study demonstrated the satisfactory performance of a HS-SPME GC/MS/MS method to measure PFAS in drinking water. The PFAS family is vast, comprising thousands of different compounds across various chemical classes. Due to this diversity, multiple analytical instruments are necessary to effectively analyze PFAS. While LC-MS is widely recognized for its ability to analyze many PFAS compounds, it is not always practical for measuring certain PFAS. This has led to a gap in the environmental mass balance, especially when it comes to measuring volatile PFAS compounds. Fortunately, unlike LC-MS, GC-MS is well-suited for analyzing volatile PFAS compounds. GC-MS complements LC-MS-based PFAS methods, providing a more comprehensive analytical solution. By expanding the PFAS target list, GC-MS helps close gaps in the PFAS environmental mass balance. The method used in this study demonstrated quantitative capability in analyzing nanogram per liter PFAS compounds in an LCS and matrix influenced drinking water samples.</p><h3><strong>4. Thermo Fisher Scientific: Method transfer to the EXTREVA ASE Accelerated Solvent Extractor&nbsp;</strong></h3><ul><li>Technical note (White paper)</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/wp_001751_sp_extreva_ase_method_transfer_wp001751_en_c7884e1151/wp-001751-sp-extreva-ase-method-transfer-wp001751-en.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=EXTREVA+ASE"><strong>EXTREVA™ ASE™</strong></a> Accelerated Solvent Extractor (Figure 1) is a system based on many proprietary technologies including gas-assisted solvent extraction and parallel accelerated solvent extraction. This fully automated system combines the extraction and evaporation capabilities in one instrument, and it can be conveniently used for extracting and concentrating/evaporating extracts from up to 16 solid and semi-solid samples per batch (i.e., 4 sequences of 4 sample cells in parallel). The EXTREVA ASE system combines elevated temperatures and pressurized gas with liquid solvents to achieve fast and efficient collection of analytes from various matrices. The system can use up to six different extraction solvents (or mixtures of them) and extract up to four cells in parallel. The gas-assisted solvent extraction comprises delivering a mixture of extraction solvents and nitrogen gas to the stainless-steel cell to reach the working pressure of 200 psi (~14 bar). The combined effect of temperature and pressure greatly increases the efficiency of the extraction process, significantly reducing the amount of time and solvent required for extraction when compared to traditional techniques such as Soxhlet. The enrichment/concentration process starts immediately after the completion of the extraction step without any analyst interaction, if no offline cleanup of extract needed. The extracts can be evaporated to dryness or concentrated in 2 mL vials to volumes as low as 0.3 mL, with the final volume controlled by artificial intelligence machine vision (Figure 2). Succinctly, the EXTREVA ASE system automates extraction, in-cell clean up, and evaporation, which frees up the analyst’s time for other, more demanding tasks.</p><p>A schematic diagram of the EXTREVA ASE Accelerated Solvent Extractor is shown in Figure 2. This white paper describes the method transfer from a Thermo Scientific™ Dionex™ ASE 350 Accelerated Solvent Extractor to the EXTREVA ASE system, and provides instructions for new EXTREVA ASE system methods.</p><h4><strong>Which options to choose for a particular application?&nbsp;</strong></h4><p>The EXTREVA ASE system workflows comprise three main options: extraction only, evaporation only, or extraction and evaporation combined (integrated) depending on the option of the instrument.&nbsp;</p><p><strong>1. Extraction only:</strong> No evaporation. After extraction, the analyst may perform an offline cleanup, and, subsequently, perform sample enrichment. If evaporation is performed after cleanup, the analyst needs to manually load cells and evaporation bottles back onto the EXTREVA ASE system as per the evaporation workflow below.&nbsp;</p><p><strong>2. Evaporation only:</strong> Evaporation has two modes of operation: evaporation to dryness or evaporation to a fixed volume. When evaporating to a fixed volume, the minimum and maximum volumes are 0.3 and 1.6 mL, respectively. When evaporating to dryness, automatic end point detection is not available; therefore, the analyst needs to optimize evaporation conditions, such as temperature, vacuum and nitrogen gas flow, in order to complete this process in the minimum amount of time while meeting analysis requirements.&nbsp;</p><p><strong>3. Extraction and evaporation combined (integrated):</strong> Extraction followed by evaporation either to dryness (such as fat extraction) or fixed volume (such as PAH, OCP, and PCB) can be pursued based on the need of a particular application or target analytes.</p>

News from LabRulezGCMS Library - Week 28, 2025

<p><strong>A pressurized liquid extraction and GC/MS (PLE-GC/MS) method was developed for quantifying seven model contaminants in recycled HDPE, selected based on EFSA and FDA recommendations. The method showed low detection limits, good repeatability, and high accuracy. Extraction was optimized using acetone at 100 °C for 6 min.</strong></p><p>This method was applied in a challenge test to evaluate an innovative HDPE recycling process using limonene for polymer dissolution and precipitation. The results confirmed high cleaning efficiency, demonstrating both the effectiveness of the recycling process and the suitability of the PLE-GC/MS method for such evaluations.</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986"><strong>Pressurized liquid extraction and GC/MS determination of model contaminants in HDPE - Application to recycling of post-consumer polyolefins using limonene</strong></a></h4><p>Javier Blázquez-Martín, Jorge García-Barrasa, María Teresa Tena&nbsp;</p><p>Journal of Chromatography A, Volume 1745, 2025, 465749</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1016/j.chroma.2025.465749">https://doi.org/10.1016/j.chroma.2025.465749</a></p><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/"><strong>CC-BY 4.0</strong></a></h6></blockquote><p><strong>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.</strong></p><p>World plastic production reached 400.3 million tonnes in 2022. Of the total, the production of polyolefins from fossil sources accounted for 45.2 %. The most produced polyolefins were polypropylene (PP) and polyethylene (PE: linear low density (LLDPE), low density (LDPE), medium density (MDPE) and high density (HDPE)) [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0001"><span>1</span></a>], with main applications in the packing industry [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0002"><span>2</span></a>].</p><p>Of the 17.9 million tonnes of post-consumer packaging waste collected in the European Union in 2020, 46 % was recycled, 37 % was used for energy recovery and 17 % ended up in landfills [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0003"><span>3</span></a>]. This metric cannot be applied to polyolefins and is mainly due to the high recyclability of poly(ethylene terephthalate) (PET). HDPE recycling rates fall to 10 to 15 % in Europe [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0004"><span>4</span></a>]. As for other polymers (LDPE, PP and PS), recycling is limited as well [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0004"><span>4</span></a>].</p><p>A wide variety of extraction methods has been proposed for extracting additives and contaminants from plastics, such as total dissolution [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0022"><span>22</span></a>], solvent extraction [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0022"><span>22</span></a>], supercritical fluid extraction [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0023"><span>23</span></a>], pressurized liquid extraction [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0023"><span>[23]</span></a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0024"><span>[24]</span></a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0025"><span>[25]</span></a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0026"><span>[26]</span></a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0027"><span>[27]</span></a>] or microwave-assisted extraction [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0028"><span>28</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0029"><span>29</span></a>]. Pressurized liquid extraction is a technique that achieves higher efficiencies and lower operating times by using organic solvents at high pressures, allowing working with temperatures higher than the selected solvent's boiling point, which increases the diffusion and desorption of compounds from the polymer, as well as increasing compound solubility.</p><p>The analysis of the PE extracts has been carried out by gas chromatography/mass spectrometry (GC/MS) [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0022"><span>22</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0025"><span>25</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0026"><span>26</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0028"><span>28</span></a>], GC with a flame ionization detector (FID) [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0025"><span>25</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0026"><span>26</span></a>] or a thermoionic selective detector (TSD) [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0026"><span>26</span></a>], headspace solid phase microextraction and GC/MS [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0022"><span>22</span></a>], liquid chromatography (LC) with UV–Vis [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0023"><span>23</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0024"><span>24</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0027"><span>27</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0029"><span>29</span></a>] and MS detection [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0024"><span>24</span></a>]. GC is the preferred technique for volatile and low molecular weight compounds. Due to the volatile nature of some compounds of interest, and to allow a simultaneous detection, GC/MS was chosen for this study.</p><p>The aim of this work was to develop, optimize and validate a PLE and GC/MS-based method for the determination of seven model contaminants (proposed by the EFSA), as well as to demonstrate the cleaning efficiency of a recycling process intended for PE from different waste sources based on the dissolution-precipitation method with limonene by analysing artificially contaminated HDPE samples in a challenge test. The development of this method is of utmost importance since, to our knowledge, there are no validated procedures published for surrogates of challenge tests.</p><h4><strong>2. Materials and methods</strong></h4><h5><strong>2.4. FTIR characterization</strong></h5><p>FTIR characterization was performed to determine whether treated and untreated HDPE presented differences in its characteristic bands, as well as to determine the presence of residual limonene after the treatment. To carry out the measurements, a Perkin-Elmer FTIR spectrometer (Waltham, MA, USA) equipped with an ATR accessory was used. Resolution of 4 cm<sup>-1</sup>, 4 scans per measurement and room temperature were the selected conditions. Vibrational bands for HDPE and limonene have been assigned according to Da Silva and Wiebeck [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0031"><span>31</span></a>] and Schulz et al. [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0032"><span>32</span></a>] and can be found in Table S1 of the supplementary material.</p><h5><strong>2.5. Pressurized liquid extraction</strong></h5><p>A Dionex ASE 200 pressurized liquid extractor (Sunnyvale, CA, USA) with a solvent controller was used for the extraction process. 0.5 g of PC-HDPE flakes were placed into 11 mL extraction cells with sea sand filling up the void volume inside the cells. Extractions were carried out at 10.3 MPa (1500 psi) using acetone as solvent. Temperature varied from 60 to 100 °C, setting an upper limit below HDPE's melting point (120–130 °C) to prevent polymer melting. The extraction time varied from 2 to 10 min. The use of one, two, three and four extraction cycles was studied as well. The flush volume was 60 % and purge time was set at 60 s. A preheating step of 5 min was used. Acetone extracts containing the surrogates were transferred into volumetric flasks and made up with acetone to 50 mL after the addition of 1.25 mL of an internal standard solution. Aliquots of each extract were filtered through a 0.22 µm nylon syringe filter prior to GC analysis.</p><h5><strong>2.6. Chromatographic conditions</strong></h5><p>An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890+GC"><strong>Agilent 8890 gas chromatograph </strong></a>coupled to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=5977B"><strong>Agilent 5977B single quadrupole mass spectrometer</strong></a> and an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7693A+autosampler"><strong>Agilent 7693A autosampler</strong></a> were used for GC analysis. The chromatographic column was an Agilent HP-5 ms (30 m x 250 µm x 0.25 µm) with a 5 % phenyl 95 % dimethylpolysiloxane phase.</p><p>The oven program started at 35 °C, holding for 0.5 min before raising the temperature to 60 °C at a rate of 10 °C min<sup>-1</sup>. Temperature was raised again to 280 °C at a rate of 70 °C min<sup>-1</sup> and maintained for 1.8 min.</p><div><p>Injection was done at 380 °C with an Agilent 5190–2293 4 mm I.D. liner in splitless-split mode (0.05 min in splitless mode). The carrier gas was helium at 1.0 mL min<sup>-1</sup>. MS detection was carried out by electronic impact, with an ionization source heated at 230 °C with a voltage of 70 eV. The quadrupole temperature was 150 °C. Chromatograms were registered in SIM mode. Chromatographic parameters for each compound are listed in <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#tbl0001"><span>Table 1</span></a>.</p><h4><strong>3. Results and discussion</strong></h4><h5><strong>3.1. GC/MS determination of surrogates</strong></h5><p>The analyte separation by GC was studied using surrogate standard solutions prepared in three different solvents: isopropanol, acetone and diethyl ether. Isopropanol was chosen first as it had been previously used for pressurized liquid extraction of additives in polyethylene [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0024"><span>24</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0025"><span>25</span></a>]. In addition, it is considered as a green solvent [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0033"><span>33</span></a>], but it was discarded because it has a higher boiling point than chloroform and, therefore, interfered with its detection.</p><p>Diethyl ether and acetone proved to be better candidates as they did not interfere with the detection of any of the surrogates. However, diethyl ether's lower boiling point led to the evaporation of standard solutions even under cooling conditions, so acetone was chosen to prepare the surrogate solutions for the GC/MS analysis. Acetone is considered a green solvent as well [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#bib0033"><span>33</span></a>].</p><div><p>Due to the extensive range of boiling points (from 62 °C for chloroform to 443 °C for methyl stearate), both a high injection temperature (380 °C) and a low oven start temperature (35 °C) were needed. A non-polar low-bleed column was used to carry out the separation. A chromatogram of a solution containing 1000 µg <span>L</span><sup>-1</sup> of each surrogate in acetone is shown in <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#fig0001"><span>Fig. 1</span></a>. <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#tbl0001"><span>Table 1</span></a> shows the model contaminants, their physical properties and the chromatographic parameters for its detection.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Journal_of_Chromatography_A_Volume_1745_2025_465749_Fig_1_GCMS_SIM_chromatogram_of_a_standard_solution_containing_1_000_g_L_1_of_each_surrogate_53d33c9fd8.jpg" alt="Journal of Chromatography A, Volume 1745, 2025, 465749: Fig. 1. GC/MS SIM chromatogram of a standard solution containing 1,000 µg L-1 of each surrogate. 1: chloroform. 2: deuterated toluene. 3: toluene. 4: deuterated chlorobenzene and chlorobenzene. 5: methyl salicylate. 6: phenyl cyclohexane. 7: deuterated benzophenone and benzophenone. 8: methyl stearate." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Journal_of_Chromatography_A_Volume_1745_2025_465749_Fig_1_GCMS_SIM_chromatogram_of_a_standard_solution_containing_1_000_g_L_1_of_each_surrogate_53d33c9fd8.jpg 245w," sizes="100vw" width="1501" height="900"></p></div><h5><strong>3.4. Recycling method based on dissolution-precipitation</strong></h5><p>The analytical method developed was used in the evaluation of the cleaning efficiency of a recycling method based on the dissolution-precipitation of post-consumer HDPE using limonene as the dissolution solvent which is a greener alternative to the commonly used toluene or xylene. The addition of an antisolvent to precipitate the polymer was deemed unnecessary, as the polymer precipitated by cooling down the mixture.</p><p>Both the PC-HDPE flakes and the recycled polymer were characterized by FTIR. Attention was put to find characteristic signals of the polymer and residual solvents. Of the PC-HDPE samples analysed, only HDPE characteristic bands were found. For the ultra-cleaned HDPE, the characteristic bands of the polymer were found along bands for limonene, which meant that residues of the solvent remained after the ultra-cleaning method.</p><p>To ensure the absence of any residues of limonene in the precipitated polymer, a drying step was carried out. A soft temperature of 40 °C was chosen to prevent the polymer from degrading. Aliquots of a treated sample being dried in an oven were taken at different time intervals and stored in closed glass vials at room temperature until characterization. The IR spectrum of each aliquot was registered to analyze the trends of limonene characteristic bands over time of drying.</p><div><p>The IR spectrums were registered six times for the aliquot taken at <i>t</i> = 0 h and three times for the rest of the aliquots. For each spectrum, the signal areas of limonene's characteristic bands were obtained. The variation of mean signal area over time is shown in Fig. S4 of the supplementary material. At 9 days, no signals were found. A comparison of spectrums of ultra-cleaned HDPE with 0 and 9 days of drying at 40 °C is shown in <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325000986#fig0003"><span>Fig. 3</span></a>. No differences in HDPE bands were found between the contaminated and ultra-cleaned polymer.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/JO_6_BE_2_1_7fccd4305a.jpg" alt="Journal of Chromatography A, Volume 1745, 2025, 465749: Fig. 3. FTIR spectrums of ultra-cleaned just after cleaning (A) and after 9 days of drying at 40 °C (B). Band assignment can be found in Table S1 of the supplementary material." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_JO_6_BE_2_1_7fccd4305a.jpg 103w," sizes="100vw" width="987" height="1500"></p></div><h4><strong>4. Conclusions</strong></h4><p>A PLE-GC/MS method for the determination of seven model contaminants in post-consumer and recycled HDPE was optimized, validated and applied to the evaluation of a novel recycling method based on the dissolution and precipitation of PC-HDPE with limonene.</p><p>GC/MS allowed the quantification of the model contaminants in a single analysis, using acetone as solvent. LODs suitable for the low concentrations expected in the recycled material were achieved. The PLE conditions were optimized with a central composite design, with the compromise values allowing a fast and automated extraction process.</p><p>This method was applied to evaluate the cleaning efficiency of a novel recycling method using limonene, following EFSA recommendations to carry out a challenge test. High cleaning efficiencies were achieved for all surrogates, proving the suitability of limonene and the dissolution-precipitation process to recycle PC-HDPE.</p><p>Moreover, the proposed analytical method allowed an easy, fast analysis of HDPE samples both before and after recycling, regardless of original application of the material, proving its adequate use during the evaluation of other novel recycling methods, whether they are mechanical, chemical or alternative processes. Lastly, the use of green and bio-based solvents, lower temperatures and shorter analysis times reduced the impact on the environment.</p></div>

Pressurized liquid extraction and GC/MS determination of model contaminants in HDPE - Application to recycling of post-consumer polyolefins using limonene

<p><strong>In the week of July 14, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.</strong></p><blockquote><p><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></p><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>4 500 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. Agilent Technologies: Recycled Plastics in Food Packaging: Testing and Standards in India’s rPET Mandate</strong></h5><ul><li>Wednesday, July 16, 2025, 07:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5306">Registration</a></li></ul><p>Explore India’s rPET packaging regulations and testing methods using GC/MS, ICP-MS, and LC/MS. Ensure safety and compliance in recycled plastics for food contact with expert insights and case studies.</p><h5><strong>2. Shimadzu Corporation: Guide To Aroma Analysis: Discover The Latest GCMS Solutions</strong></h5><ul><li>Thursday, July 17, 2025, 09:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5277">Registration</a></li></ul><p>Explore how Shimadzu’s advanced GC-MS systems, Aroma Database, along with other innovative solutions can streamline conventional aroma analysis with accuracy.</p><h5><strong>3. Thermo Fisher Scientific: Targeted MS quantitation - Controlled and accessed from anywhere</strong></h5><ul><li>Thursday, July 17, 2025, 16:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5232">Registration</a></li></ul><p>Join our webinar to learn how Chromeleon 7.4 software provides MS labs with advanced tools for their targeted quantitation workflows by combining the powerful network and compliance capabilities.</p><h5><strong>4. Agilent Technologies: Part 2: Characterizing catalysts using an UV-VIS/NIR system with the Praying Mantis diffuse reflectance accessory</strong></h5><ul><li>Thursday, July 17, 2025, 20:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4926">Registration</a></li></ul><p>In Part 2 of this workshop, we look at performing measurements on the Cary 5000 UV-VIS/NIR Spectrophotometer with the Praying Mantis accessory from Specac/Harrick.</p>

Webinars LabRulezGCMS Week 29/2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 14th July 2025? 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 posters by <strong>Agilent Technologies / ASMS, Shimadzu / ASMS, </strong>presentation by<strong> Liège University / MDCW </strong>and technical note by<strong> Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Optimizing Hydrogen Carrier Gas on GC/MS Using the HydroInert EI Source and 5Q Columns&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_gc_gc_5q_columns_ei_source_asms_2025_mp_358_en_agilent_c5cf1876f0.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Hydrogen is widely recognized for its benefits in gas chromatography (GC), including cost-effective generation in the lab, rapid chromatography, and higher sample throughput. However, its reactivity can lead to hydrogenation and dechlorination reactions in the mass spectrometer electron ionization (EI) source, complicating its application in many scenarios. To address these issues, Agilent has developed a specially designed extractor source for the Inert Plus GC/MSD and triple quadrupole GC/MS systems, enhancing performance with hydrogen carrier gas. The Agilent HydroInert source maintains mass spectral fidelity and allows users to utilize existing helium-based mass spectral libraries.</p><p>This study investigates how the 5Q series of columns impact the performance and durability of the HydroInert source tune. The study involved cycling through 10,000 oven temperature ramps without any injections to assess the effects of column bleed from the 5Q phase. Furthermore, the study examined how the combination of sample matrix and column bleed from the 5Q phase affects source longevity.</p><h4><strong>Experimental</strong></h4><h5><strong>HydroInert Functionality with 5Q Columns (no Injection)&nbsp;</strong></h5><p>An experiment was designed to investigate the effects of ultra low bleed columns (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?instrumentationItems=19&amp;manufacturerItems=1&amp;search=HP-5Q"><strong>HP-5Q</strong></a>) on the functionality of the HydroInert source over time. A method simulating a large oven temperature ramp cycle (Table 1) over 12 minutes was created. The syringe was removed from the ALS tower to simulate injections, but to isolate the source of siloxanes to column bleed from the HP-5Q only. 10,000 injections were executed, and a system tune was performed every 100 injection to monitor source parameter shifts.</p><p>The Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7000E"><strong>7000E</strong></a> was run in SCAN mode, scanning from 50-450 m/z during each run. Air leaks were detected and immediately remedied when found to ensure the experiment was free from oxides. Liner and septum were not changed during this experiment.</p><h4><strong>Results and Discussion</strong></h4><h5><strong>HydroInert Functionality with 5Q Columns (no Injection)&nbsp;</strong></h5><p>Results of the effects of 10,000 oven temperature cycles on the HydroInert source tune parameters are shown in Figure 2. Repeller and ion body voltages are set automatically by the tune algorithm to maximize the transference of ion on the 7000E. Throughout the 10,000 injections the ion body voltage remained stable. The EM voltage gain across 10,000 injections was as expected. The source was in use for 120,000 minutes during this study and data was being collected throughout the duration of the study in SCAN mode. During this study, three leaks were detected at the MS transfer line and were corrected as soon as they were detected. The leaks are reflected in the spike in O2 percentage. A new ion body will typically have a voltage of 16-22 V on a HydroInert source. When an ion body begins to lose functionality the ion body voltage will begin to rise to compensate for the loss. Eventually the ion body voltage tops out at 29-30 V and the tune begins to show lower abundance of tune ions, until the source fails to tune. In the current study the ion body voltage was set by the tune algorithm between 19-24 V. This is a stable and normal operating range for the ion body. It is important to remember that a single elevated ion body tune is not cause for concern, there needs to be a trend of elevation over time. The overall purpose of this first study was to examine what baseline changes would occur to the HydroInert tune parameters when using a 5Q column in leak free conditions. Water and oxygen are known to speed the liberation of column bleed, which in turn reduces the functionality of the HydroInert source. This study shows that under leak free conditions, with a 5Q column, the HydroInert source can function optimally for an extended period. This study adds to a growing body of evidence that has demonstrated one of the main factors in HydroInert longevity is leak state of the system.</p><h4><strong>Conclusions</strong></h4><p>Agilent HydroInert source longevity is dependent on application and method conditions. However, by using the best practices highlighted above, the longevity of HydroInert parts can be prolonged. The HydroInert source cannot be mechanically or chemically cleaned, thus when source parts show reduced functionality, replacement of the recommended parts is required to restore functionality. Replacement intervals will be method and application dependent.</p><h3><strong>2. Liège University / MDCW: MOSH&amp;MOAH in food ingredients and additives and the advantages of using LC/GC×GC(-FID/TOFMS) for their analysis&nbsp;</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/FL_02_2025_MDCW_AG_MOSH_MOAH_additives_a05df36b39.pdf"><strong>Full PDF for download</strong></a></li></ul><p>This presentation by Aleksandra Gorska and colleagues (Gembloux Agro-Bio Tech) addresses the analysis of MOSH (mineral oil saturated hydrocarbons) and MOAH (mineral oil aromatic hydrocarbons) in food ingredients and additives, particularly those derived from oils and fats. These contaminants are widespread in the food chain due to packaging, lubricants, or storage conditions. While MOSH can accumulate in human tissues, MOAH—especially those with three or more aromatic rings—pose genotoxic risks. The European Food Safety Authority (EFSA) has recently emphasized a lack of data on such impurities in food additives.</p><p>To fill this gap, the researchers developed and applied an advanced analytical workflow based on <strong>HPLC-GC×GC-FID/TOFMS</strong>, replacing the traditional HPLC-GC-FID approach. This multidimensional technique combines high-resolution separation with both flame ionization detection (FID) and time-of-flight mass spectrometry (TOFMS), allowing detailed structural characterization, efficient removal of interfering compounds, and the ability to separate MOAH by the number of aromatic rings.</p><p>Key benefits of the HPLC-GC×GC-FID/TOFMS system include clearer chromatograms with structured elution patterns, improved purification and separation of complex MOAH profiles, and identification of contamination markers such as DIPN (indicating migration from recycled packaging). Additionally, the system enables <strong>simultaneous quantification of MOAH and polycyclic aromatic hydrocarbons (PAHs)</strong>, which have distinct analytical requirements and toxicological profiles.</p><p>The study concludes that, despite its complexity, the HPLC-GC×GC-FID/TOFMS technique provides substantial analytical advantages and aligns with EFSA’s recommendations. It offers a powerful tool for ensuring food safety in products containing oil- or fat-derived additives, enabling more accurate risk assessments and source tracking of contamination.</p><h3><strong>3. Shimadzu / ASMS: Highly sensitive and efficient analysis of aroma components using trapped Headspace GC-MS&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_2025_MP_352_97902375e7.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The aroma composition of foods has been the subject of considerable research in recent years. It is well known that the presence of volatile compounds and their composition determine the specific aroma of foods and the flavor of the resulting products. Static headspace technique enables high sensitivity analysis of volatile compounds, normally extracting 1 mL of headspace. But in situations where it is necessary to evaluate the total chemical profile, it is known that components in small quantities also affect the overall aroma. Thus, the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=HS-20+NX"><strong>HS-20 NX</strong></a> was used running in "Trap mode", where by using trapped headspace sampling, it is possible to extract much more volume and analyze, not only the majority components, but all the compounds with high sensitivity.&nbsp;</p><p>The system used to achieve the highest sensitivity is the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=HS-20+NX"><strong>HS-20 NX</strong></a> coupled to the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-QP2020+NX"><strong>GCMS-QP2020 NX</strong></a> single quadrupole mass spectrometer.</p><h4><strong>Results and Discussion</strong></h4><p>After the incubation time, the acquisitions were done by loop mode and trap mode with 3- and 5-times sample concentration. In this way, it is possible to analyze, via trap, the presence of compounds at trace levels, which cannot be observed when analyzed in loop mode. 18 compounds could be identified in the sample when analyzed in loop mode, whereas in trap mode, 35 were identified.</p><p>Some components such as benzene acetaldehyde, gammacaprolactone, methyl butyrate, o-guaiacol, that have a decisive influence on the overall aroma and flavor were detected only in the trap mode, due to their low concentrations in the sample. Even concentrating the sample 5-times in the trap, it was possible to detect these compounds that require greater sensitivity along with compounds present in high concentrations in the sample, such as butanoic acid, acetic acid, and others, without losing analysis efficiency.</p><h4><strong>Conclusion</strong></h4><p>The improvement in analysis sensitivity when using trap mode can be observed when comparing the area for some components with a major impact on the overall aroma but present in small quantities. When concentrating the sample 3-times in the trap, the peak intensities increased from 351.17 to 1401.08%. And it was still possible to have a significant increase of another 168%, on average, by concentrating the sample 5-times. The peak intensities increased from 521.48 to 2517.86% compared to loop mode analysis.&nbsp;<br>These analyses demonstrate that trapped headspace can be used to determine an overall aroma profile in a single analysis and with a single trapping material. The trapped headspace sampler enables ultra sensitivity analysis, identifying compounds at low concentrations which were undetectable with conventional headspace samplers.</p><h3><strong>4. Thermo Fisher Scientific: Data-driven GC and GC-MS instrument monitoring with SmartStatus intelligent software</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/tn_001883_gc_ms_gc_ms_ms_smartstatus_tn001883_na_en_99ce72eef2/tn-001883-gc-ms-gc-ms-ms-smartstatus-tn001883-na-en.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Rising costs can significantly impact an analytical laboratory’s profit margin, and it is crucial to maintain productivity and ensure maximum asset utilization to stay competitive. To balance increased overhead costs, including analytical gases and staff pay, laboratories must ensure that analytical instrumentation consistently produces results, without interruption. Re-analyzing entire runs due to drops in sensitivity, unnecessary downtime, and underutilization of consumables is expensive and time consuming.&nbsp;</p><p>Thermo Scientific™ SmartStatus™ instrument tracking can help laboratories realize additional cost savings. This is done by using data-driven insights to accurately determine when to perform maintenance and replace consumables and parts, so that the system consistently runs smoothly for all samples and meets specifications in the initial analysis. This ensures that consumables and parts are replaced on the correct schedule and avoids excess instrument downtime.&nbsp;</p><p>SmartStatus instrument tracking is an intelligent instrument health software that allows users to track key aspects of their GC-MS system. It is available as standard on the Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/483"><strong>TRACE™ 1600 GC series,</strong></a> Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/487"><strong>AI/AS 1610 liquid autosampler</strong></a>, Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/484"><strong>ISQ™ 7610 GC-MS series</strong></a>, and the Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/485"><strong>TSQ™ 9610 GC-MS/MS series</strong></a>. In this technical note, the new SmartStatus instrument tracking capabilities are highlighted with examples of how it can enable analytical laboratories to keep instruments producing consistent results.</p><h4><strong>SmartStatus software overview&nbsp;</strong></h4><p>SmartStatus intelligent software, available within Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Chromeleon™ Chromatography Data System (CDS)</strong></a>, allows monitoring of the entire analytical system including Thermo Scientific™ autosamplers, GC, GC detectors (FID and TCD), and mass spectrometers (MS). Hundreds of key instrument parameters are monitored by SmartStatus software, which provides real-time data and insights informing the user to potential problems before they arise to ensure maximum instrument uptime. This allows users to make informed decisions on which parts of the analytical system require attention and when. By performing preventative maintenance using data-driven guidance, optimal instrument performance is sustained day in and day out. Figure 1 shows the SmartStatus software overview page for a TSQ 9610 triple quadrupole MS coupled to a TRACE 1610 GC and AI/AS 1610 liquid autosampler. This overview page allows a user to quickly determine if the system is ready to run or requires attention.&nbsp;</p><p>For more information on instrument status, there is a detailed view for each part of the system. This next level view shows how many injections have been performed for the various GC consumables, the lifetime of the MS detector and filament, and when the last tune was performed. Figure 2 shows an example of the GC and MS parameters and how they are monitored. Each parameter is represented as a counter gauge. As the usage increases, the gauge changes color to quickly notify the user of any maintenance that is required or will be needed soon. This allows users to plan maintenance in advance to fit it around their schedule and workload. SmartStatus instrument tracking can be monitored directly in Chromeleon CDS, and consumables usage can also be monitored directly on the TRACE 1610 GC touch screen through the dedicated instrument health icon, as shown in Figure 3.</p><p>The ISQ 7610 GC-MS and the TSQ 9610 GC-MS/MS detector lifetime is monitored using a predictive algorithm. This assesses the voltages on the detector and predicts the lifetime remaining on the system so that preventative maintenance can be planned. As the ISQ 7610 GC-MS and TSQ 9610 GC-MS/MS are equipped with the XLXR™ electron multiplier detector as standard, the lifetime of the detector is several years.1 By monitoring the detector intelligently, users can avoid unnecessary downtime. Figure 4 shows monitoring of the detector within SmartStatus software.</p>

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News from LabRulezGCMS Library - Week 29, 2025

Webinars LabRulezGCMS Week 29/2025

Pressurized liquid extraction and GC/MS determination of model contaminants in HDPE - Application to recycling of post-consumer polyolefins using limonene

News from LabRulezGCMS Library - Week 28, 2025

Webinars LabRulezGCMS Week 28/2025

NDMA in macrolides: GC-MS/MS method for its detection and study of its formation

News from LabRulezGCMS Library - Week 27, 2025

Webinars LabRulezGCMS Week 27/2025

GC–MS as a valuable tool for analysing cannabinoid-containing gummies and identifying the synthetic process used for their production

News from LabRulezGCMS Library - Week 26, 2025

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