Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 4th August 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you poster by Agilent Technologies / ASMS, application note by Shimadzu, presentation by PSL RESEARCH UNIVERSITY / MDCW and technical note by Thermo Fisher Scientific!<h3>1. Agilent Technologies / ASMS: Investigation and Profiling of the Aroma Components by GC-SICRIT-QTOF&nbsp;</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_6546_gc_sicrit_qtof_aroma_component_asms_2025_thp_157_en_agilent_3b0b61094d.pdf">Full PDF for download</a></li></ul>Volatile aroma components possess significant value in flavor research. Conventional GC-MS analysis, reliant on the NIST library, is more adept at identifying known components. In contrast, LC-QTOF which exhibits strong identification capabilities, demonstrates limited ionization efficiency for volatile substances.GC-SICRIT-QTOF, a hybrid technique, synergizes the separation capabilities of GC for volatiles, the ionization strength of SICRIT for alkenes and enols, and the powerful identification capacity of QTOF, highly suitable for the detection and profile of volatile aroma components.<h4>Experimental</h4><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6546+Q-TOF">Agilent 6546 Q-TOF</a> Mass Spectrometer</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=53&amp;search=SICRIT+ion+source">SICRIT ion source </a>(Plasmion GmbH, Germany</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8860+GC">Agilent 8860 GC System</a></li></ul><h4>Results and Discussion</h4><h5>Target Extraction and Confirmation&nbsp;</h5>Without sample preparation, volatile aroma components can be directly analyzed 6546 QTOF equipped with the SICRIT ion source, obtain MS and Auto MS/MS spectra within 1 min. For example, in positive ion mode, we can observe [M+H]+ and [M+NH4 ]+ ions for common organic solvents such as water, alcohol, acetonitrile and so on. If we spike ethanol vapor to nitrogen gas, less than 0.1% can be detected with 10e4~5 intensity (Figure 1).&nbsp;It is also possible to find volatilizable components in complex mixtures. Figure 2 shows some examples. Butanediol is a major component in essence. Besides of alcohol, it is also possible to find esters in Chinese liquor. Alkenes and enols are main aroma components in Sichuan pepper. Their formulas are proved by accurate mass and isotope patterns.<h5>GC Coupling for isomers separation</h5>&nbsp;Pepper samples contain many isomers with the same formula but different aromas. We use 8860 GC to separate these isomers, combined with SICRIT-QTOF for ionization and acquiring mass spectra. The system demonstrates a robust response to the volatile gas components of Sichuan pepper, with a significant number of signals observed in the total ion chromatogram (TIC, Figure 3).&nbsp;For the known volatile components, the GC-SICRIT-QTOF system can identify many isomers by quasi-molecular ion extraction. For example, C10H16, includes myrcene with peppery aroma, limonene with the flavor and fragrance of oranges, sabinene with woody and spicy aroma. RT, MS and MS/MS spectra can be used for identification by the support of reference and PCDL database.&nbsp;<h4>Conclusions</h4>GC-SICRIT-QTOF is a powerful tool for volatile aroma component analysis. It combines the separation capabilities of GC, the ionization strength of SICRIT for low polar components, and the identification power of QTOF.&nbsp;Compare to GC-MS, this system shows quasi-molecular ions, which can be used in identification and discover new component using non-targeted extraction. Soft ionization is also suitable for fast screening and profiling without preparation.&nbsp;GC-SICRIT-QTOF facilitates the analysis of complex mixtures. It was demonstrated in the research of Sichuan pepper, including the target extraction, unknown analysis and profiling. It will contribute to the development of new food products, fragrances, and other applications in the flavor industry.<h3>2. PSL RESEARCH UNIVERSITY / MDCW: TOWARDS A BETTER UNDERSTANDING OF THE BODY VOLATOLOME: FOCUS ON ENDOGENOUS PARAMETERS INFLUENCING BODY VOLATOLOME COMPOSITION&nbsp;</h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/FL_06_BOUDADR_FL_06_b8fc54d8f5.pdf">Full PDF for download</a></li></ul>The human body emits a wide range of volatile organic compounds (VOCs), collectively known as the body volatolome. This study aimed to better understand how endogenous parameters—such as age, sex, and anatomical sampling site—influence the composition of these compounds. Using skin sampling devices (SkinVOCs®) and comprehensive GC×GC-TOF-MS, researchers profiled VOCs from different body areas of volunteers while controlling for exogenous factors like deodorants or perfumes.Principal Component Analysis (PCA) and Partial Least Squares Discriminant Analysis (PLS-DA) revealed clear distinctions in VOC profiles based on sampling site and age. For instance, armpit VOCs showed age-dependent differences, particularly in the levels of steroids and known odor-active molecules like E-3-methyl-2-hexenoic acid. Interestingly, left-right body symmetry was confirmed, suggesting that bilateral samples from the same person can be used as replicates. Some molecules were identified as gender-specific, and although some trends contradicted literature findings, most supported age and sex influence on volatolome composition.The study concludes that age- and gender-matched sampling is essential in clinical volatolomics research to avoid confounding variables. These findings pave the way for developing personalized diagnostics and deeper understanding of skin VOCs in health and disease.<h3>3. Shimadzu: Multiresidue Pesticides Analysis in Cumin Seeds Using GCMS-TQ8040 NX&nbsp;</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_06_saip_gc_041_en_d646a1cd78.pdf">Full PDF for download</a></li></ul>Cumin (Cuminum cyminum) has been used as a natural medicine for over 2000 years. It shows anti-inflammatory property and supports the immune system. Cumin seeds (Figure 1) have been widely used as a spice in many food preparations. To fulfil the high-demand of such spices, pesticides are widely used. But their overuse may cause acute and permanent health problems in humans. Therefore, to protect human health, the European Union has set maximum residue limits (MRLs) for the presence of pesticides in cumin seeds[1]. Thus, increasing the importance of having analytical method for determination of residual pesticides present in it.This study reports a validated method for the determination of 169 pesticides in cumin seeds of Indian origin using Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ8040+NX">GCMS-TQ8040 NX</a> (Figure 2). The multi-residue extraction was performed using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=QuEChERS+extraction+method">QuEChERS extraction method</a>[2].<h4>Materials and Methods&nbsp;</h4>The reference standards for this study were procured from Restek with below catalogue number: GC multi-residue pesticides kit – 32562 Cumin seeds procured from local market, were used to prepare matrix-matched calibration standards and spiked samples. This method is validated for criteria as mentioned in SANTE Guidelines[3]. <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ8040+NX">GCMS-TQ8040 NX</a>, manufactured by Shimadzu Corporation Japan, was used to quantify residual pesticides in cumin seeds sample.<h4>Conclusion&nbsp;</h4>A validated method was developed as per SANTE guidelines for determination of 169 pesticidesin cumin seeds. QuEChERS’ extraction was used for quantifying residual pesticides in this complex spice matrix containing essential oils, cuminaldehyde, pigments etc. The instrumental MRM method was effortlessly created using Smart Pesticides Database. The combination of highly sensitive Shimadzu GC-MS/MS and reliable method showed reproducibility &lt; 20% (as per SANTE guidelines) at LOQ levels. This enables its use in testing laboratories for multi-residue analysis in cumin seeds.<h3>4. Thermo Fisher Scientific: What is the benefit of high mass resolving power on the Orbitrap Exploris GC Series?&nbsp;</h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/sl_003312_gc_hram_orbitrap_exploris_240_targeted_gc_sl003312_na_en_8f86e0d919.pdf">Full PDF for download</a></li></ul><h4>Why do I need high mass resolving power from Orbitrap technology?&nbsp;</h4><ul><li>Resolve target analytes from interfering compounds and matrix ions of similar mass.&nbsp;</li><li>Achieve sub-ppm mass accuracy to give data certainty in compound identification.&nbsp;</li><li>Sub-ppm mass accuracy enables narrow mass extraction windows (± 5 ppm) to give high selectivity, which in turn makes peak detection algorithms efficient.&nbsp;</li><li>Easily increase scope of analysis through full scan accurate mass data acquisition (Figure 1).&nbsp;</li><li>Quickly and confidently propose elemental compositions for the identification of unknown features.&nbsp;</li><li>Retrospective data processing of samples long after data acquisition.&nbsp;</li><li>Have high mass resolving power and sensitivity. No compromise.&nbsp;</li></ul>With resolving power of up to 240,000 and consistent sub-ppm mass accuracy, the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/473">Thermo Scientific™ Orbitrap Exploris™ GC 240 mass spectrometer</a> is a unique laboratory tool for targeted and discovery workflows, where screening, quantitation, compound identification, and structural elucidation applications are required.&nbsp;High-resolution Orbitrap mass spectrometry has been available with both liquid and gas chromatography for many years and has proven to be a highly valuable analytical technique.1-4 More recently, the technology in gas chromatography moved to join the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/472">Thermo Scientific Orbitrap Exploris Mass Spectrometer</a> series. This new platform of a benchtop hybrid quadrupoleOrbitrap mass spectrometer opens up research opportunities in a system with a significantly reduced footprint, saving both energy and raw materials. The benchtop hybrid quadrupole-Orbitrap mass spectrometer provides new possibilities for increased mass accuracy, sensitivity, and selectivity for GC-amenable compounds. Figure 2 shows how the resolving power is in the ideal range for volatile small molecules, with resolving power increasing with lowering m/z.<h4>The impact of mass resolution on selectivity for targeted analysis&nbsp;</h4>High-resolution, accurate-mass (HR/AM) experiments typically provide a full scan analysis of a sample, and for small molecule analyses, the scan range is typically 50–600 Da. Orbitrap technology provides the required selectivity to resolve the target compound from other compounds or from matrix ions of similar mass. For targeted compound analysis, the accurate mass of the diagnostic ion is extracted with a narrow mass extraction window (typically &lt; 5 ppm). This narrow window is possible only when the instrument provides sufficient mass accuracy, for which high mass resolving power is essential. However, when two mass profiles overlap, the measured mass profile is the sum of the two individual profiles. This overlap results in the incorrect assignment of the mass of the target compound. The problem is demonstrated in Figure 3, where a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/421">QuEChERS</a> leek extract in acetonitrile was analyzed four times at resolving powers of 15K, 30K, 60K, and 120K (m/z 200).&nbsp;Being able to separate two compounds that are close in mass is one of the significant advantages of high-resolution accurate mass. This is demonstrated in Figures 4A-C where the compounds flurenol methyl ester C15H12O3 m/z = 240.0781 and dimetilan C10H16N4O3 m/z = 240.1217 were analyzed at equal intensity at three different resolving power levels of 30,000, 60,000, and 240,000. The zoomed spectra show excellent separation at all resolution levels, with improvements at 60K and 240K showing the clear benefits. When analyzed at 10:1 ratio (Figure 5), there is still good separation and mass accuracy. The latter reflects the real world where compounds will be at varying intensities, and it is essential that mass accuracy is maintained to make confident identifications.

News from LabRulezGCMS Library - Week 32, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 11th August 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you poster by Agilent Technologies / ASMS, application note by Shimadzu and technical note by Thermo Fisher Scientific!<h3>1. Agilent Technologies / ASMS: Fully Automated Workflow for Volatile PFAS Analysis in Food Contact Materials Using GC-Triple Quadrupole</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_7010d_pal_autusampler_pfas_asms_2025_tp_456_en_agilent_50ffdde82b.pdf">Full PDF for download</a></li></ul>The analysis of per- and polyfluoroalkyl substances (PFAS) in food contact materials (FCMs) is crucial due to potential health and environmental concerns. Increased PFAS testing is needed to meet public demands and new regulations. Gas Chromatography coupled with Triple Quadrupole Mass Spectrometry (GC/TQ) offers a robust and sensitive method for detecting volatile PFAS. However, manual sample preparation could pose a bottleneck, impacting lab productivity. This study presents a robust and fully automated method using the PAL3 platform with GC/TQ for quantifying more than 30 volatile PFAS in FCMs, such as paper coffee cups. The automation approach minimizes human error, improving reliability and reproducibility for routine analysis and safety assessments of PFAS in FCMs.<h4>Experimental</h4><h5>Automated Sample Preparation&nbsp;</h5>The integrated 120 cm <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=PAL3">PAL3 Series 2 RTC autosampler</a>, paired with the Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7010D+GC%2FMS">7010D GC/TQ</a>, facilitated a fully automated PFAS quantitation workflow using a paper cup matrix. It served as an automated liquid handling platform for preparing calibration standards, extracting samples, and injecting them into the GC/TQ system, equipped with essential tools and modules.<h5>GCMS Instrumentation&nbsp;</h5>The 7010D GC/TQ with HES 2.0 ion source was coupled to an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC">8890 GC</a> system equipped with an MMI inlet and splitless liner (p/n 5190-2293). SWARM autotune optimized the instrument settings. The Agilent 8890 GC, operated in pulsed splitless mode with a splitless inlet liner, was used for analysis. The PAL3-GC/TQ system, managed by <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+Acquisition+software">MassHunter Acquisition 13.0 software</a>, provided an integrated single-software experience. <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter+Optimizer">MassHunter Optimizer</a> was used to obtain MRM transitions for 34 targets, along with collision energies1 . Instrument operating conditions and parameters are given in the table below<h4>Conclusions</h4><ul><li>This study demonstrated a robust, fully automated method for analyzing volatile PFAS in FCMs using the PAL3 Series 2 RTC autosampler and Agilent 7010D GC/TQ system.&nbsp;</li><li>Method detection limits (MDL), linearity, retention time (RT) precision, area precision, and QC recovery was performed to assess the workflow performance.&nbsp;</li><li>The MassHunter Optimizer simplified method development, while the HES 2.0 ion source provided exceptional sensitivity, achieving sub-ppb MDLs.&nbsp;</li><li>For all FTOHs, an LOQ of 20 μg/kg with recoveries of 65% to 135% and %RSD &lt; 10% were achieved, highlighting the high extraction efficiency, accuracy and reliability of the automated workflow.&nbsp;</li><li>Automation reduces human errors, decreases chemical usage, and enhances productivity, offering reliable trace-level volatile PFAS monitoring in FCMs for regulatory guidance.</li></ul><h3>2. Shimadzu: Analysis of Benzene and Toluene by <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Brevis+GC-2050">Brevis GC-2050</a> Using ASTM D3606&nbsp;</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00902_en_41581fffcc.pdf">Full PDF for download</a></li></ul><h4>User Benefits</h4><ul><li>Quantitation of benzene and toluene in fuels based on ASTM D3606 is possible.&nbsp;</li><li>Highly accurate backflush analysis is possible by using the SMI flow device.&nbsp;</li><li>The compact design of the Brevis GC-2050 enables space-saving in the laboratory.</li></ul>Benzene and toluene are widely used as feedstocks for chemical products, but due to concerns about their effects on human health, the permissible concentrations of these two compounds are specified in various regulations. ASTM D3606 1) provides two quantification methods (Procedures A and B) for benzene and toluene in automotive fuels. The corresponding concentrations of benzene and toluene are 0.12-5.2 Vol% and 0.4-19.7 Vol% when using Procedure A and 0.10-5.0 Vol% and 2.0-20.0 Vol% when using Procedure B. In this Application News article, benzene and toluene were quantified by Procedure A in ASTM D3606. Satisfactory linearity of the calibration curves and reproducibility of the quantitation values could be obtained for both compounds.<h4>System Configuration and Analysis Conditions</h4>Table 1 shows the system configuration and analysis conditions. The compact <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Brevis+GC-2050">Brevis GC-2050,</a> with a width of about 35 cm, can contribute to space-saving in the laboratory while also demonstrating high analytical performance. In procedure A, benzene and toluene are measured with a backflush system using a capillary column. Backflush has the advantage of shortening the analysis time. Fig. 1 shows a schematic diagram of the backflush system. In addition to the FID detector (FID1) connected to the Wax analytical column, a second FID detector (FID2) which is connected to the restrictor tube, is used for monitoring to determine the timing of backflushing. The gas that flows through the columns is supplied from the injection port (SPL) and digital flow controller (AUX-APC). This is connected to discs called an SMI Flow Disc and 2-DET Splitter, which are used to split the flow to the two detectors. The SMI Flow Disc is a flow device for capillary analysis, and has the features of minimal leakage, a low dead volume, a low heat capacity, and inertness. For this reason, the device has the advantages that the temperature inside the device easily follows the temperature of the column oven, and it is also possible to analyze components with high adsorptivity. Before backflushing, the SPL pressure is set high, and during the backflush operation, the gas in the pre-column is made to flow in the reverse direction (backflushed) by changing the pressures of the SPL and AUX-APC. In this experiment, the initial backflush time was set to 3.1 min to match the elution time of toluene (Fig. 2).<h4>Conclusion</h4>Using the Brevis GC-2050, an analysis of benzene and toluene as specified in ASTM D3606 was conducted. The analysis time could be shortened by using a backflush system. As the quantitation values of benzene and toluene were within the standard range for both reproducibility and repeatability, satisfactory results were obtained.<h3>3. Thermo Fisher Scientific: How NeverVent technology enables consistent uptime for continued lab operation&nbsp;</h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/sl_003311_gc_vacuum_probe_interlock_nevervent_food_beverage_sl003311_na_en_529ea8c8af.pdf">Full PDF for download</a></li></ul><h4>Benefit summary&nbsp;</h4><ul><li>Eliminates unnecessary downtime&nbsp;</li><li>Maintains productivity&nbsp;</li><li>Simplifies maintenance&nbsp;</li><li>Enables disruption-free ionization type change&nbsp;</li><li>Increases ROI</li></ul><h4>What is NeverVent technology and how does it work?&nbsp;</h4>Thermo Scientific™ NeverVent ™ technology is unique to <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products?category=5&amp;manufacturerItems=3">Thermo Fisher Scientific’s GC-MS products</a>. It allows for routine maintenance, exchange of ionization mode, and direct probe work to be performed without the need to break the vacuum of the mass spectrometer:&nbsp;<ul><li>Removing/replacing the ionization source: Utilizing the vacuum probe interlock (VPI) in combination with an isolation valve, the ionization source can be removed the from the system without venting the MS. The source can either be cleaned or replaced with a spare clean source, and samples can be run without long stabilization times which would be required if the system was vented.&nbsp;</li><li>Changing ionization type: Using the VPI, the ionization source can be replaced with a different type of ionization source, for example, switching from Electron Ionization (EI) to Chemical ionization (CI) within a few minutes.&nbsp;</li><li>Using direct sampling probes: The VPI also allows the use of direct probes on some NeverVent GC-MS systems. This enables direct sampling into the MS system, bypassing the GC separation, and is useful in compound characterization and when analyzing very difficult to volatilize samples like oils or metal complexes.&nbsp;</li><li>Changing the GC column without venting: When performing common column maintenance like trimming, or replacing the column entirely, the V-Lock Source Plug allows the MS to be sealed off from inside the manifold. Columns can be exchanged or maintained without ever breaking vacuum.</li></ul><h4>What are the benefits to NeverVent technology?&nbsp;</h4>NeverVent technology allows a significant increase in instrument uptime. On a traditional GC-MS when performing maintenance, such as ionization source cleaning or column exchange, the MS must be vented. Venting the MS introduces air and moisture into the system. Once the maintenance is performed, the system is then pumped back down to vacuum and a stabilization period is required to ensure air and moisture are evacuated from the system. This process often takes overnight to complete and means samples cannot be run until the following day.&nbsp;Due to the unique design of a NeverVent GC-MS system, the vacuum is maintained which means samples can be run shortly after the maintenance is performed. This could be the difference betwen running a batch of samples overnight or waiting for a system to be ready to run. Utilizing NeverVent technology eliminates unnecessary instrument downtime due to venting the systems during maintenance, thus increasing productivity. Figure 2 highlights the time savings that can be achieved with NeverVent technology.&nbsp;For a typical GC-MS system where maintenance on the source is performed every three months, NeverVent technology can give you an extra four days of operation per year. When adding in column and ionization mode changings, the productivity gains are even more significant.

News from LabRulezGCMS Library - Week 33, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 18th August 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you poster by Agilent Technologies / ASMS and application note by Shimadzu!<h3>1. Agilent Technologies / ASMS: New Pollutant Screening of Environmental Samples Using High-Resolution GC/Q-TOF and Accurate Mass Spectral Library of Emerging Environmental Pollutants&nbsp;</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_7250_pdcl_library_pal3_suremass_asms_2025_thp_083_en_agilent_3f1ac53d50.pdf">Full PDF for download</a></li></ul>This paper conducts qualitative and semi - quantitative analysis of complex GC/Q-TOF sample data by using high-resolution, accurate-mass gas chromatography/quadrupole time-of-flight mass spectrometry (GC/Q-TOF), an accurate mass spectral library of environmental pollutants specifically created for emerging pollutant screening, and analytical software with a screening process platform. Actual environmental water samples are used to verify the sensitivity, accuracy, and spiked recovery rate of the solution. All results confirm that this solution is simple, stable, and effective, providing technical support for emerging pollutant screening.<h4>Experimental</h4><h5>Instrument Analysis&nbsp;</h5>The samples were analyzed by <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC">Agilent 8890 GC</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7250+GC%2FQ-TOF">7250 high resolution accurate mass GC/Q-TOF system</a>, It was configurated with a mid-column backflush setup (Figure 1). A 55.5 - min retention time locked GC oven temperature program is utilized which is listed in Table 1. The key mass spectrometry parameters of the GC/Q-TOF are as follows: It operates in the Electron Ionization (EI) mode with an energy of 70 electron volts, conducts detection in the time-of-flight scan mode within a mass-to-charge ratio range of 50 - 1000. The spectral acquisition rate is 5 Hz, and both the interface temperature and the source temperature are set at 280 °C. Data analysis is performed with the assistance of MassHunter data analysis software. The high-resolution accurate mass spectral library employed in the screening process is independently created by the laboratory.<h5>Data Analysis&nbsp;</h5><ul><li>The data processing used Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=Masshunter+software">Masshunter data analysis software</a>, including Suremass.&nbsp;</li><li>The target screening of new pollutants was based on an independently created by the laboratory GC/Q-TOF PCDL library1.</li></ul><h4>Conclusions&nbsp;</h4><ul><li>Based on the currently collected list of new pollutants, a truly meaningful new pollutant PCDL high-resolution spectral library has been created.&nbsp;</li><li>This work demonstrated a total workflow for targeted screening and semi-quantification in real water sample.&nbsp;</li><li>The confidence in identification of new pollutants was enhanced by stable RT and excellent mass accuracy as a result of using an RTL backflush method and highresolution accurate mass measurement.</li></ul><h3>2. Shimadzu: Analysis of SAF Using Comprehensive Two- Dimensional Gas Chromatography (GC× GC)&nbsp;</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00862_en_f1ee0a435f.pdf">Full PDF for download</a></li></ul><h4>User Benefits</h4><ul><li>By comparing chromatograms obtained as two-dimensional images, it can be utilized for quality control Inspection of SAF.</li><li>Changing the column combination customizes separation characteristics to the sample composition.</li><li>Utilizing the FASST (Fast Automated Scan/SIM Type) allows for the simultaneous analysis of the composition of SAF and the quantitative analysis of antioxidants.</li></ul>SAF (Sustainable Aviation Fuel) produced from waste cooking oil, used paper, and sugarcane has gained attention in recent years from the perspective of achieving a carbon neutral society. The physical properties of SAF,such as combustibility, vary depending on its components. Therefore, component analysis of SAF is crucial; however, since SAF is a mixture of various hydrocarbons, complete separation of each component is extremely challenging. Comprehensive two-dimensional gas chromatography (GC×GC), which utilizes the separation characteristics of two different types of columns, is an effective method for analyzing SAF with such a complex composition. Additionally, the GCMS-QP2050 enables ultra-fast scanning (30,000 u/sec), which improves the separation of adjacent peaks and allows for high-precision qualitative analysis(Application News No.01-00788-EN).In this application, two types of SAF (A and B) and one intermediate product from the SAF production process (C) were measured using a combination of GC×GC with a non-polar column as the first column and a medium-polarity column as the second column. The two-dimensional images allow for a visual representation of the composition distribution, making quality control Inspection. Moreover, high separation of paraffins and naphthenes using a combination of a medium-polar column as the first column and a non-polar column asthe second column, as well as the quantification of antioxidants in SAF, which are regulated by concentration in ASTM D2425 will be introduced.<h5>System Configuration</h5><ul><li>GC Model: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexis%E2%84%A2+GC-2030">Nexis GC-2030</a> / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=AOC-30i">AOC-30i</a></li><li>MS Model: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050">GCMS-QP2050</a> (TMP exhaust: 255 L/sec)</li><li>Injection Port: SPL</li><li>Modulator: ZX1 thermal modulator (ZOEX corp.)</li><li>Nitrogen generator: MT-24F (System Instruments Co., Ltd.)</li><li>Software:<ul><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Labsolutions+GCMS">LabsolutionsTM GCMS</a></li><li>GC Image (GC Image, LLC)</li></ul></li><li>Library: NIST Mass Spectral Library</li></ul><h4>Conclusion</h4>Three SAF samples were measured using a combination of lowpolar to medium polar columns and compared the twodimensional images. The two-dimensional images allow for intuitive comprehension of the distribution of each component, making it easy to identify differences in composition and conducting quality control Inspection. Additionally, in the measurement of SAF using a combination of medium-polar to non-polar columns, the separation of paraffins and naphthenes was improved. Furthermore, by utilizing the FASST, composition analysis of SAF and quantitative analysis of antioxidants were simultaneously performed, which are regulated by concentration in ASTM D2425.

News from LabRulezGCMS Library - Week 34, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 25th August 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies and Shimadzu!<h3>1. Agilent Technologies: A More Sustainable Analysis of Ethylene Oxide and 1,4-Dioxane in Surfactants with Hydrogen Carrier Gas&nbsp;</h3>Using an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977B+GC%2FMSD">5977B GC/MSD</a> with an Agilent HydroInert Source<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_ethylene_oxide_1_4_dioxane_surfactants_hydrogen_carrier_gas_5994_8335en_agilent_886a988649.pdf">Full PDF for download</a></li></ul>EO and 1,4-dioxane are key industrial chemicals, frequently found in the production of surfactants. During alkoxylation processes, residual raw materials or byproducts, such as EO and 1,4-dioxane, may remain in the final surfactant product (Figure 1). Although manufacturers have made significant strides in reducing these byproducts, increasing regulatory scrutiny on EO and 1,4-dioxane underscores the need for precise analytical methods to detect these compounds at low concentrations.1–4 Thus, there is an urgent need to develop methods that can accurately quantify these compounds at levels as low as 0.1 ppm in consumer products.This study presents a method for the detection of EO and 1,4-dioxane using GC/MS with an HS sampler and a HydroInert source for hydrogen carrier gas. The use of hydrogen instead of helium not only addresses the global helium shortage but also ensures excellent sensitivity and linearity, while maintaining the integrity of the analytical process. The HydroInert source further eliminates chemical reactions often associated with hydrogen in mass spectrometry, offering a sustainable and reliable solution. The method developed in this study successfully quantifies both EO and 1,4-dioxane at the low concentrations required by current regulations, offering an accurate, reliable approach for compliance in surfactant manufacturing.<h4>Experimental&nbsp;</h4>This work was carried out using an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890+GC">7890 GC</a> with helium carrier gas and an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC">8890 GC</a> with hydrogen carrier gas. Both GC systems were configured with an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977B+GC%2FMSD">5977B GC/MSD</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=PAL3+autosampler">PAL3 autosampler</a> for headspace sampling. For the analysis using hydrogen carrier gas, the GC/MSD was fitted with a HydroInert source. The HydroInert source produces spectra in hydrogen that closely match those from helium-based libraries, such as NIST. This ensures spectral fidelity, allowing the same quantification and qualifier ions used in helium methods to be applied in SIM and MRM modes with hydrogen. Method parameters are shown in Table 1.<h4>Conclusion&nbsp;</h4>This work establishes a first of its kind method using hydrogen carrier gas to reliably measure ethylene oxide and 1,4-dioxane in surfactants. Mass spectrometry detection was optimized for use with hydrogen by installing an Agilent HydroInert source. The HydroInert source helps to avoid sensitivity loss and spectral anomalies that are common with hydrogen carrier gas applications, resulting in suitable linearity, precision, accuracy, and LOQs for this analysis.<h3>2. Shimadzu: How Long Does A Perfume Last on Skin? – Fragrance Analysis by <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050">GCMS-QP2050</a> and Smart Aroma Database</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_04_ad_0309_en_60c887beed.pdf">Full PDF for download</a></li></ul><h4>User Benefits</h4><ul><li>Achieve highly accurate and reproducible analysis of aroma compounds on human skin, ensuring reliable data for evaluating perfume performance.</li><li>Smart Aroma Database simplifies the qualitative and quantitative analysis process, reducing the time and effort required for data interpretation.</li></ul>The duration on how long fragrance lasts on human skin is a critical factor in the development and evaluation of perfumes. Gas Chromatography Mass Spectrometry (GC-MS) is a powerful analytical technique that allows for the detailed analysis of volatile and semi-volatile compounds, making it an ideal tool for studying fragrance. In this application note, a study was performed to examine fragrance on human skin at different durations after applying a perfume. Here, we explore the use of a Monolithic Material Sorptive Extraction (MMSE) MonoTrap, a sorptive extraction device to extract fragrance from human skin, followed by analysis using Shimadzu GCMS-QP2050 (Fig.1). Additionally, Smart Aroma Database was used to simplify the method development.<h4>Experimental</h4><h5>Instrumental and Analytical Conditions&nbsp;</h5><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050">GCMS-QP2050</a> (Shimadzu Corporation, Japan) was employed in this work (Fig. 1). The details of the system configuration is shown in Table 1. Sample acquisition was done by following the analytical method from Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Smart+Aroma+Database">Smart Aroma Database</a>. MonoTrap SG DCC18 was purchased from GL Sciences, Japan (catalog no. 1050-70002).<h4>Results &amp; Discussion&nbsp;</h4><h5>Fragrance Compounds Detection&nbsp;</h5>The scan total ion chromatogram (TIC) of the diluted perfume sample is shown in Fig. 4. A total of 60 out of the 498 fragrance compounds in Smart Aroma Database were detected. These compounds were then monitored for this study. Fig. 5 shows a few mass chromatograms of the monitored fragrance compounds.<h5>On-skin Fragrance Study&nbsp;</h5>The on-skin fragrance study was conducted to evaluate the persistence of perfume compounds over time. Sampling was performed at three distinct time points: 15 minutes, 1 hour, and 6 hours after applying the perfume (as described in Fig. 2). Fig. 6 shows the percentage of compounds detected (out of 60 compounds) in these three different time points.<h4>Conclusion&nbsp;</h4>In this study, we demonstrate the effectiveness of using GCMSQP2050 with Smart Aroma Database and Monotrap adsorbent to analyze the behavior of perfume fragrance on human skin. The result shows decrease percentage of number of compounds detected over time. The peak area of most compounds were reduced as well. Sampling repeatability shows that 57 out of 58 detected aroma compounds exhibiting %RSD values below 20% (n=3).

News from LabRulezGCMS Library - Week 35, 2025

During the manufacture of pharmaceuticals, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=45&amp;search=1%2C+4-Dioxane">1, 4-Dioxane</a> is used as a cleansing agent. It is also a byproduct of plastic manufacturing. The most likely exposure to 1, 4-Dioxane is at an industrial site. However, if any 1, 4-Dioxane is released into the environment during manufacturing there is a potential for it to migrate into ground water. The fact that 1, 4-Dioxane is so miscible in water makes degradation of the chemical challenging. Ethanol, on the other hand, has been a popular gasoline additive. Since it burns more quickly and completely than gasoline, emissions from car exhaust are decreased. The downside of this is underground storage tank leakage and fuel spills cause ground water and drinking water to be contaminated with both the fuel and the ethanol additive. Since ethanol is also very miscible in water, the detection of ethanol contamination in water can be difficult.&nbsp;There have been several innovations that help overcome the obstacles of detecting 1, 4-Dioxane and Ethanol. The first one is the SIM mode of the mass spectrometer. This mode allows better detection of hard to extract compounds. Furthermore, mass spectrometers are now equipped to run SIM/Scan, this not only helps detect more difficult compounds, but also enables the detection of an extensive list of <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=45&amp;search=USEPA+Method+8260">USEPA Method 8260</a> compounds without having to run the samples twice. Advancements in purge and trap sampling have also facilitated better detection of these compounds. Most effective in this has been the ability to heat the samples. However, there are drawbacks to better detection. The most problematic of these is the tendency of 1, 4-Dioxane and Ethanol to “stick” to the glass ware. This susceptibility has caused many headaches in environmental labs.&nbsp;This application note will investigate seven variations of <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=45&amp;search=purge+and+trap">purge and trap</a> sampling. The data will then be evaluated in order to recommend the optimum purge and trap sampling parameters for your lab.<h4>Experimental:&nbsp;</h4>The sampling system used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Evolution concentrator</a> affixed with a Vocarb 3000 trap. The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler</a> equipped with the syringe option was employed as the autosampler. The separation and analysis were performed by an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890A+Gas+Chromatograph">Agilent 7890A Gas Chromatograph (GC)</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5975C+Mass+Spectrometer">5975C inert XL Mass Spectrometer (MS).</a> The GC was configured with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=7&amp;search=Rxi-624+Sil+MS">Restek Rxi-624 Sil MS</a> 30m x 0.25mm x 1.4µm column. The purge and trap and GC/MS parameters used for this study are listed below.<h5>Purge and Trap Parameters</h5><ul><li>Concentrator: EST Encon Evolution</li><li>Trap type: Vocarb 3000</li><li>Valve oven temperature: 150 °C</li><li>Transfer line temperature: 150 °C</li><li>Trap temperature: 35 °C</li><li>Moisture Reduction Trap (MoRT) temperature: 39 °C</li><li>Purge time: 11 min</li><li>Purge flow: 40 mL/min</li><li>Dry purge: Ambient temperature, 40 mL/min, 1.0 min</li><li>Desorb pressure: 5 psi (with control ON)</li><li>Desorb time: 0.5 min</li><li>Desorb preheat delay: 10 sec</li><li>Desorb temperature: 250 °C</li><li>MoRT bake temperature: 210 °C</li><li>Bake temperature: 260 °C</li><li>Sparge vessel bake temperature: 40 °C for 3 min, ramp to 100–110 °C, hold</li><li>Bake time: 6 min</li><li>Bake flow: 85 mL/min</li></ul><h5>Auto-Sampler (EST Centurion WS):</h5><ul><li>Sample type: Water</li><li>Sample volume: 5 or 10 mL</li><li>Internal standard volume: 5 µL</li></ul><h5>GC/MS Parameters</h5><ul><li>System: Agilent 7890A GC / 5975C inert XL MS</li><li>Inlet: Split mode, 220 °C, 40:1 split ratio, 12.153 psi head pressure</li><li>Column: Restek Rxi-624Sil MS, 30 m × 0.25 mm × 1.4 µm</li><li>Oven program: 45 °C (1 min) → ramp 15 °C/min → 220 °C, hold 1.33 min (total run ~14 min)</li><li>Column flow rate: 1 mL/min helium</li><li>Total flow: 44 mL/min</li><li>Source temperature: 230 °C</li><li>Quadrupole temperature: 150 °C</li><li>Transfer line temperature: 180 °C</li><li>Scan range: m/z 35–300, 5.2 scans/sec</li><li>SIM ions:<ul><li>45, 46 (0.7–3.49 min)</li><li>58, 88 (3.5–14 min)</li></ul></li><li>Solvent delay: 0.7 min</li></ul>For each parameter iteration, see the text below, a calibration curve was established with a linear range of 0.5 to 200ppb using standards from Restek. After each of the prescribed curves was determined; Method Detection Limits (MDLs), precision and accuracy and carryover studies were performed. A series of seven low level standards were run in order to establish MDLs per 40CFR Part 136, Appendix B. Next, seven replicate samples of the 50ppb standard were run in order to establish the precision and the accuracy of the experimental parameters. Finally, a series of four 50ppb standards were run with each standard followed by three blanks. The amount of carryover was then analyzed in the first blank. The data from each parameter variation was compiled and compared in order to determine the optimum conditions for this analysis. An average of the results for each analysis condition is listed in Table 1.<h5>Purge and Trap Sampling Test Parameters</h5><ul><li>Baseline: 5 mL traditional sparger, room temp purge, 110 °C sparge bake</li><li>Iteration A: 5 mL traditional sparger, 40 °C purge, 110 °C sparge bake</li><li>Iteration B: 5 mL traditional sparger, 60 °C purge, 110 °C sparge bake</li><li>Iteration C: 5 mL traditional sparger, 40 °C purge, no sparge bake</li><li>Iteration D: 40 mL vial, 10 mL purge volume, 40 °C purge, no sparge bake</li><li>Iteration E: 5 mL fritless bulbless sparger, 40 °C purge, 110 °C sparge bake</li><li>Iteration F: 5 mL fritless bulbless sparger, 40 °C purge, no sparge bake (Iteration E used the patented Water/Soil prep mode)</li></ul><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_4_Averaged_Results_Summary_306dcbfde6.jpg" alt="EST Analytical: Table 1 Averaged Results Summary" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_4_Averaged_Results_Summary_306dcbfde6.jpg 245w," sizes="100vw" width="1493" height="351">The primary compounds of interest for the study were Ethanol and 1, 4-Dioxane. For this reason, the data for these compounds was compiled separately in order to better distinguish the benefits or detriment of each purge and trap parameter set. The experimental results of the precision and percent recovery studies are displayed in Tables 2 and 3.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_5_Ethanol_and_1_4_Dioxane_Precision_at_50ppb_3a195e1acb.jpg" alt="EST Analytical: Table 2 Ethanol and 1, 4-Dioxane Precision at 50ppb" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_5_Ethanol_and_1_4_Dioxane_Precision_at_50ppb_3a195e1acb.jpg 245w," sizes="100vw" width="1316" height="236"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_6_Ethanol_and_1_4_Dioxane_Percent_Recovery_at_50ppb_cb12616f47.jpg" alt="EST Analytical: Table 3 Ethanol and 1, 4-Dioxane Percent Recovery at 50ppb" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_6_Ethanol_and_1_4_Dioxane_Percent_Recovery_at_50ppb_cb12616f47.jpg 245w," sizes="100vw" width="1318" height="234">For the carryover studies, Ethanol and 1, 4-Dioxane were examined along with the carryover of 1, 2, 4- Trichlorobenzene, Naphthalene and 1, 2, 3-Trichlorobenzene. The reason the heavier compounds were included in this study was a concern that changing the sampling parameters may help the Ethanol and 1, 4-Dioxane carryover, but harm the carryover of the heavier compounds of interest. Table 4 shows a listing of the carryover results, in parts per billion, while Figure 1 displays the percent carryover of the different purge and trap experimental parameters for just the Ethanol and 1, 4-Dioxane.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_7_Carryover_in_First_Blank_after_a_50ppb_Standard_7d2bc81626.jpg" alt="EST Analytical: Table 4 Carryover in First Blank after a 50ppb Standard" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_7_Carryover_in_First_Blank_after_a_50ppb_Standard_7d2bc81626.jpg 245w," sizes="100vw" width="1332" height="426"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_1_Ethanol_and_1_4_Dioxane_Percent_Carryover_after_a_50ppb_Standard_Graphic_f57c981913.jpg" alt="EST Analytical: Figure 1 Ethanol and 1, 4-Dioxane Percent Carryover after a 50ppb Standard Graphic" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_1_Ethanol_and_1_4_Dioxane_Percent_Carryover_after_a_50ppb_Standard_Graphic_f57c981913.jpg 245w," sizes="100vw" width="1358" height="787">After all the studies were completed, two purge and trap parameter variations showed the best precision, percent recovery, and carryover while meeting the USEPA Method 8260 linearity and response factor requirements. An abbreviated listing of the results for these two iterations are shown in Table 5.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_8_Results_of_the_Water_Extraction_and_the_Fritless_Bulbless_Sparge_Vessel_With_Sparge_Bake_Studies_9b71ec4951.jpg" alt="EST Analytical: Table 5 Results of the Water Extraction and the Fritless - Bulbless Sparge Vessel With Sparge Bake Studies" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_8_Results_of_the_Water_Extraction_and_the_Fritless_Bulbless_Sparge_Vessel_With_Sparge_Bake_Studies_9b71ec4951.jpg 161w," sizes="100vw" width="1256" height="1221"><h4>Conclusions:&nbsp;</h4>All seven purge and trap parameter iterations passed the USEPA Method 8260 requirements for linearity and method detection limits. The problem with some of the experimental parameters was found in the carryover and precision and accuracy studies. The carryover using the traditional sparge vessel showed a large amount of carryover for the Ethanol and 1, 4-Dioxane. Since the carryover was so high, the precision and accuracy data suffered. The Fritless/Bulbless sparge vessel, on the other hand, displayed much lower carryover for the Ethanol and 1, 4-Dioxane especially when the patented sparge bake was not used. However, the 1, 2, 4-Trichlorobenzene, Naphthalene and 1, 2, 3-Trichlorobenzene carryover after the 50ppb standard was above the lower limit of the curve.&nbsp;Thus, the sparge bake would be recommended in order to limit the carryover of the heavier compounds. The optimum purge and trap parameters proved to be the patented water extraction technique. This technique provided linearity and method detection limits that met the USEPA Method 8260 requirements, while providing excellent precision and accuracy data. During water extraction, the sample is transferred to an empty 40ml vial and then purged in the soil station of the Centurion. The “fresh” vial provides a clean sparge vessel for every sample thus limiting carryover for both the Ethanol and 1, 4-Dioxane and for the heavy compounds. This lack of carryover aided in providing optimum precision and accuracy and carryover results and would be the recommended method for examining these troublesome compounds.

Optimization of 1,4-Dioxane and Ethanol Detection Using USEPA Method 8260

At the forefront of global anti-doping efforts, the Laboratoire Anti-Dopage Français (LADF) plays a critical role in ensuring fair play and integrity in elite sports. We spoke with Dr. Magnus Ericsson, Director of LADF and a leading expert in analytical chemistry, to explore how the lab detects banned substances, manages high-throughput workflows, and leverages advanced Thermo Fisher Scientific technologies to stay ahead of constantly evolving challenges in anti-doping science.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Thermo_Fisher_Scientific_Inside_Laboratoire_Anti_Dopage_Francais_LADF_An_Interview_with_Director_Dr_Magnus_Ericsson_6aca8272d5.jpg" alt="Thermo Fisher Scientific: Inside Laboratoire Anti-Dopage Français (LADF): An Interview with Director Dr. Magnus Ericsson" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Thermo_Fisher_Scientific_Inside_Laboratoire_Anti_Dopage_Francais_LADF_An_Interview_with_Director_Dr_Magnus_Ericsson_6aca8272d5.jpg 245w," sizes="100vw" width="1024" height="512"><article><div><h3>Screening and confirmation: A rigorous two-step approach</h3>Every year, LADF analyzes tens of thousands of biological samples using a workflow aligned with World Anti-Doping Agency (WADA) guidelines. This two-step process—screening and confirmation—forms the backbone of modern doping analysis. During the screening phase, high-throughput, non-targeted assays detect a broad spectrum of compounds. This aligns with recent advancements in mass spectrometry that allow LC-HRAM (high-resolution accurate mass) systems to scan for hundreds of substances in a single run, ensuring rapid and comprehensive coverage of the WADA Prohibited List (1). Suspicious samples then undergo confirmation testing using validated targeted methods that meet WADA’s stringent sensitivity and specificity criteria. LADF employs the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/485">Thermo Scientific TSQ 9610 Triple Quadrupole GC-MS/MS system</a> for this task. Introduced in 2023, this triple quadrupole instrument has already supported the analysis of over 40,000 urine samples, ensuring reliable confirmatory data. “The TSQ 9610 mass spectrometer has helped us to improve our workflow in the lab,” says Dr. Ericsson. “We started using it in 2023 and today we have analyzed more than 40,000 samples… with great success.” Implementation of <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/77">Thermo Scientific TraceFinder software</a> has also enabled seamless software continuity with LADF’s existing LC-MS and GC-MS platforms—minimizing training needs and ensuring consistent operations.<h3>Unlocking historical insights with retrospective analysis</h3>Modern anti-doping labs benefit not just from real-time detection but also from retrospective analysis, enabled by HRAM technology. LADF leverages the high-resolution <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/403">Thermo Scientific Orbitrap Exploris 120 mass spectrometer</a> to re-mine stored HRAM data and search for newly -banned substances. This capability aligns with a broader trend in doping control. HRAM instruments now routinely provide resolution &gt;60,000 FWHM and mass accuracy &lt;2 ppm, allowing researchers to revisit past datasets and identify emerging doping agents without reanalyzing physical samples (1). “Working with high-resolution mass spectrometry, we have the possibility to go back and search in previously analyzed data,” Dr. Ericsson explains. Retrospective analysis is becoming increasingly vital as WADA continues to expand its list of monitored substances.<h3>Speeding up turnaround times without sacrificing accuracy</h3>During major competitions, laboratories are under intense pressure to deliver results rapidly. LADF tackles this challenge using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/742">Thermo Scientific Vanquish Duo UHPLC</a> paired with the Orbitrap Exploris 120 mass spectrometer, enabling parallel workflows and multiplexed analyses in 96-well formats. “We are able to save maybe a couple of hours of time. And this is a huge benefit for us,” notes Dr. Ericsson. Recent advances support this approach. New UHPLC and HRAM technologies allow scan-to-scan polarity switching at &gt;1 Hz, making it possible to detect a wide array of acidic and basic substances simultaneously—significantly speeding up comprehensive screening workflows (1).<h3>Building toward a one-stop shop</h3>LADF aims to become a true “one-stop shop” for anti-doping services—mirroring Thermo Fisher Scientific’s role as their trusted, all-in-one partner for laboratory technologies by consolidating their analytical infrastructure under a single provider. “It’s nice to have a one-stop shop… which means that you work mostly with one major provider,” says Dr. Ericsson. Thermo Fisher Scientific has delivered leading technologies for the analysis of performance-enhancing drugs and other prohibited substances for more than a quarter century. In line with its commitment to advance the field, the technologies the company offers bolster the analytical arsenal of doping control laboratories, enabling them to provide multiple perspectives to enhance the reliability of results. This strategic alignment not only reduces system fragmentation and compatibility issues but also enables rapid method implementation and consistent training across staff. Such standardization is key as doping tests grow more complex, involving both small molecules and peptide-based substances.<h3>Looking ahead: The future of anti-doping analysis</h3>As doping methods evolve, so must detection technologies. LADF continues to invest in instruments that deliver robustness, low maintenance, and ultra-sensitivity. “It’s the sensitivity and the selectivity… and the possibility to increase the selectivity by doing, for instance, different MS/MS experiments,” says Dr. Ericsson. The industry trend supports this need. New approaches like stable isotope-labeled (SIL) internal standards, supercritical fluid chromatography (SFC), and top-down proteomics with Thermo Scientific Orbitrap instruments are being developed to quantify complex peptides and detect gene doping or biologics (1). In addition, growing concerns around unintentional doping—via contaminated supplements, food, or even environmental exposure—are pushing labs to adopt even higher sensitivity assays and more advanced data interpretation protocols (1). With a clear vision and cutting-edge technology, LADF is not only keeping pace with modern anti-doping demands but also setting a gold standard for scientific excellence in sport. Discover <a target="_blank" rel="noopener noreferrer" href="https://www.thermofisher.com/content/lifetech/global/en/home/industrial/forensics/antidoping.html">Thermo Fisher Scientific’s anti-doping solutions</a> and <a target="_blank" rel="noopener noreferrer" href="https://view.highspot.com/viewer/be96860291ab6345fc58cc95d9bc3156">watch Dr. Ericsson’s complete testimonial here.</a><h3>Additional resources</h3><ul><li>Video – <a target="_blank" rel="noopener noreferrer" href="https://www.youtube.com/watch?v=-8zRtsRkAcU">Mass Spectrometry Enables Top WADA Lab to Beat the Cheats: Athlete Doping Control</a></li><li>BBC Video – <a target="_blank" rel="noopener noreferrer" href="https://www.bbc.com/storyworks/connecting-the-dots/thermo-fisher">How can technology maintain sports integrity?</a></li><li>Testimonial – <a target="_blank" rel="noopener noreferrer" href="https://www.youtube.com/watch?v=mi1VHutyqPA">LCH Ludovic Bailly-Chouriberry Testimonial video for TSQ Altis Plus MS</a></li><li><a target="_blank" rel="noopener noreferrer" href="https://assets.thermofisher.com/TFS-Assets/CMD/Technical-Notes/tn-000304-ms-testosterone-human-serum-faims-tn000304-en.pdf">TN000304 – Analysis of testosterone from human serum using FAIMS technology</a></li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/tn_001896_gc_ms_gc_ms_ms_tsq_9610_steroids_urine_tn001896_na_en_d1fd813050/tn-001896-gc-ms-gc-ms-ms-tsq-9610-steroids-urine-tn001896-na-en.pdf">TN001896 – Staying ahead of regulations for the analysis of steroids in urine with GC-MS/MS</a></li></ul><blockquote>Visit us on&nbsp;<a target="_blank" rel="noopener noreferrer" href="https://www.linkedin.com/showcase/72003132/admin/dashboard/">LinkedIn:</a>&nbsp;#Antidoping, #LADF, #WADA, #SportsIntegrity</blockquote></div></article><section><blockquote><h4>Ema Ruzic</h4>Vertical Marketing Manager, Chromatography and Mass Spectrometry Division (CMD)</blockquote></section>

Inside Laboratoire Anti-Dopage Français (LADF): An Interview with Director Dr. Magnus Ericsson

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 1st September 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you poster by Agilent Technologies / ASMS and application notes by EST Analytical and Shimadzu!<h3>1. Agilent Technologies / ASMS: Analysis of Phthalates Using GC/MS With Hydrogen Carrier Gas: The Importance of Reducing Interferences and Contamination&nbsp;</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_5977c_phthalates_hydrogen_gas_asms_2025_mp_359_en_agilent_d51f599179.pdf">Full PDF for download</a></li></ul>Due to the price of helium (He), many laboratories are looking for alternative carrier gases for their gas chromatography/mass spectrometry (GC/MS) methods. This work describes the evaluation of a single quadrupole GC/MS method for the analysis of 19 phthalates using hydrogen carrier gas and an EI source 1 . The method provides excellent peak shape, resolution, sensitivity, and a 13 min run time. Calibration curves were linear for 16 of the phthalates, with the remaining 3 alkoxy phthalates requiring a quadratic fit. Except for DINP and DIDP (mixtures of isomers), all compounds could be quantitated at low pg levels. Specific attention to the consumables used and their preparation before use is discussed and is important for reaching the lowest calibration levels.<h4>Experimental</h4><ul><li>GC: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+gc">Agilent 8890 GC</a> with <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7693A">Agilent 7693A automatic liquid sampler</a> and tray</li><li>Column: Agilent HP-5MS UI 20 m x 0.18 mm id x 0.18 µm (p/n 19091S-577UI)</li><li>MSD: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977C+GC%2FMSD">Agilent 5977C Inert Plus GC/MSD</a></li></ul><h4>Conclusions</h4><ul><li>The Agilent 5977C GC/MSD and 8890 GC, when used with the method described here, provide excellent peak shape, resolution, sensitivity, and a 13 min run time..&nbsp;</li><li>The combination of hydrogen carrier and the Agilent J&amp;W HP-5ms 180 µm diameter column allowed for reduced analysis time relative to helium and a 250 µm diameter column .&nbsp;</li><li>Calibration curves were linear for 14 of the phthalates from 1 to 1,000 pg. DMEP and DBEP required quadratic curve fits, and DMEP and DEHP were calibrated from 2.5 to 1,000 pg. DINP and DIDP were calibrated from 50 to 20,000 pg with a linear fit.&nbsp;</li><li>Specific attention to the consumables used and their preparation before use is important for reaching the lowest calibration levels.</li></ul><h3>2. EST Analytical: The Determination of Flavors in E-Liquids Using Purge and Trap Concentration</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_E_Liquid_Compound_Sampling_Using_Purge_and_Trap_5c709b52f0.pdf">Full PDF for download</a></li></ul>E-liquid can be composed of propylene glycol or vegetable glycerin alone or can be a combination of the two. Propylene glycol is less viscous and carries better flavor. It also acts as a preservative. However, it does produce less vapor and some people are allergic to it. Vegetable glycerin, on the other hand, is much denser, is super hypoallergenic and produces more vapor. The drawback to the vegetable glycerin is that it is not a preservative, so the vape liquid will not last as long. Both glycerin and propylene glycol readily dissolve in water, so preparing the samples to test by purge and trap was relatively easy. Conversely, as the E-liquid emitted a strong odor of the added flavors, only a small amount of the solution could be used for analysis. The volatile flavor components of the vape liquid were examined by dissolving the solution in water and sampling the water using purge and trap.<h4>Experimental</h4>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">Evolution purge and trap concentrator </a>was configured with a Vocarb 3000 trap. The trap was conditioned at 260ºC for one hour. The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS syringe autosampler</a> was set in water mode in order to run 5 ml samples. Next, samples were prepared using 10ul of vape solution dissolved in 100mls of de-ionized water. The parameters for the autosampler/purge and trap concentrator and the Gas Chromatograph/Mass Spectrometer (GC/MS) are outlined in Tables 1 and 2.<h4>Conclusions</h4>Since vape solution readily dissolves into water, purge and trap sampling proved to be an excellent technique for the determination of the volatile compounds in the E-liquids. Purge and trap sampling is an exhaustive sampling technique, so the results were very reproducible and provided the sensitivity to determine the lower level compounds in the solution. Furthermore, it was found that nicotine addition to the solution has an effect some of the compounds in the solution. So, the taste of the vape liquid is affected by the amount nicotine in the mix.<h3>3. Shimadzu: Determination of Nitrobenzene Compounds in Nifedipine by GCMS&nbsp;</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_03_gcms_589_en_23eda751e7.pdf">Full PDF for download</a></li></ul><h4>User Benefits</h4><ul><li>The direct dissolution protocol without pre-treatment, significantly enhancing analytical efficiency.</li><li>The specificity of the method is ensured by monitoring the characteristic ions of nitrobenzene compounds in selected ion monitoring (SIM) mode, which provides robust resistance to interferences.</li></ul>Nifedipine, a dihydropyridine calcium channel blocker with vasodilatory properties, is primarily indicated for the clinical management of hypertension and angina pectoris. Its synthetic route commences with 2-nitrotoluene as the starting material. Notably, the intermediate 2-nitrobenzyl alcohol, the byproduct 2- nitrobenzyl bromide, the reaction product 2-nitrobenzaldehyde, and potential impurities (3-nitrobenzaldehyde and 4- nitrobenzaldehyde) all contain nitrobenzene moieties, rendering them candidatesfor monitoring as potential genotoxic impurities. Previous studies have demonstrated that 2-nitrobenzaldehyde and 4-nitrobenzaldehyde exhibit mutagenicity in the Ames test, while 2-nitrotoluene has shown carcinogenicity in animal experiments. In accordance with the toxicological concern threshold (TTC) control approach specified in ICH M7, a threshold of 1.5 μg/day is recommended for genotoxic impurities in pharmaceuticals intended for lifelong administration. In this study, a method for the determination of six genotoxic impurities in nifedipine was developed using a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050">Shimadzu GCMSQP2050</a> gas chromatography mass spectrometry. This method features simplified sample preparation, high sensitivity, and favorable repeatability, thereby enabling effective monitoring of the six nitrobenzene compounds as genotoxic impurities in nifedipine pharmaceutical.<h4>Analytical Conditions</h4>The analytical conditions are shown in Table1. <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050">GCMS-QP2050</a> system was used for this Application News.<h4>Conclusion&nbsp;</h4>A GC-MS method was established for the quantification of six nitrobenzene genotoxic impurities in nifedipine pharmaceuticals using a Shimadzu GCMS-QP2050 system. The calibration curves showed excellent linearity within the concentration range of 20-200 μg/L, with correlation coefficients (R&gt;0.999). Precision was evaluated through six replicate injections of the 50 μg/L standard solution, and the relative standard deviations (RSDs) of peak areas for all analytes were less than 4%. Spike recovery experiments were performed at three concentration levels (0.005, 0.01, and 0.032 μg/g) in actual matrices, resulting in recovery rates ranging from 95.85% to 117.64%. This method is characterized by simplified sample preparation, high sensitivity (IDLs of 0.263-0.496 μg/L), and good repeatability. Overall, it provides a validated analytical strategy for quality control monitoring of the target genotoxic impurities.

News from LabRulezGCMS Library - Week 36, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 8th September 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you poster by Agilent Technologies / ASMS and application notes by EST Analytical and Shimadzu!<h3>1. Agilent Technologies / ASMS: Optimizing the Efficiency and Productivity of GC/MS Workflows to Improve Laboratory Sustainability</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_db_5q_hydroinert_sustainability_asms_2025_mp_365_en_agilent_3cc1d968a1.pdf">Full PDF for download</a></li></ul>Today, laboratories consume a staggering 10 times more energy and water than a typical office [1]. Labs with GC and GC/MS systems have unique sustainability challenges due to the resource-intensive nature of these instruments. They consume large amounts of gas and energy while also generating hazardous waste products. According to Agilent customer surveys, 85 percent of labs and organizations have sustainability goals in place, and 83 percent of lab leaders believe their current workflow requires optimization to meet their sustainability ambitions [2]. A more efficient laboratory is a more sustainable one. This poster outlines some simple approaches that laboratories can take, today, to optimize workflow efficiency and productivity, thus minimizing resource consumption.<h4>Experimental</h4>Laboratory workflows are the cornerstone of laboratory operations. In this poster we will illustrate the impact of column scaling for GC/MS workflows, the use of hydrogen as an alternative, renewable carrier gas for GC and GC/MS. Hydrogen offers unique safety and reactivity challenges that we will address with Agilent HydroInert source. Lastly, we will demonstrate simple and effective ways to conserve gases, focusing on existing helium carrier gas workflows. In the end, these simple, easy-toimplement practices will illustrate how sustainability can be accomplished in conjunction with improving workflow profitability and productivity.<h4>Alternative Carrier Gases</h4><h5>Carrier Gases&nbsp;</h5>Helium shortages have impacted analytical laboratories since 2006 and repeatedly been in short supply[3]. While helium’s availability has improved in recent years, there are still concerns surrounding supply stability and rising costs. Knowing the cyclic nature of the helium supply chain, exploring alternative carrier gas options like hydrogen and nitrogen are necessary for laboratory managers looking for sustainability, flexibility, and cost savings measures. Specifically, hydrogen carrier gas is a good option for GC/MS methods and when using the Agilent Method Translator tool, methods can easily be transferred. Figure 3 highlights parameter adjustments for translation like pressure, flow, velocity, and temperature program rates to ensure similar relative retention orders with the alternative gas. Hydrogen when compared to nitrogen as a carrier gas provides the best alternative for chromatographic resolution and speed. Figure 4 demonstrates a method transfer of helium to hydrogen carrier gas for ASTM D5769.<h4>Consumables Impact&nbsp;</h4><h5>Tailored <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?instrumentationItems=19&amp;mainauthorItems=10">GC Columns&nbsp;</a></h5>Consumables in GC/MS workflows are often overlooked as contributing factors to sustainability and optimization. For example, minimizing column bleed and improving GC column thermal durability can have a major beneficial impacted for both data quality and instrument uptime. <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?instrumentationItems=19&amp;mainauthorItems=10&amp;search=J%26W+5Q">Agilent J&amp;W 5Q GC columns</a> provide the lowest bleed standard for GC/MS workflows. This provides less downtime from ion source cleaning, faster conditioning, and minimize reruns due to data quality issues. Figure 5 and 6 highlight thermal stability and sensitivity of the DB-5Q and HP-5Q columns.<h4>Conclusions</h4>Optimizing the efficiency and productivity of GC/MS workflows are critical for analytical laboratories to stay competitive and profitable. This poster demonstrated a time savings of 50% with column scaling from a conventional GC/MS column to a high-efficiency column, successful alternative carrier gas method transfer, reducing potential source reactivity when using hydrogen carrier, and demonstrated 3.8 to 7X factor reduction of carrier gas consumption when using software features and the Helium Conservation module.<h3>2. EST Analytical: Drinking Water Analysis Conditions for USEPA Method 524.3 and the Newly Proposed Method 524.4</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_Drinking_Water_Analysis_Conditions_for_USEPA_Method_524_3_and_524_4_Agilent_315971a468.pdf">Full PDF for download</a></li></ul>In June 2009, the United States Environmental Protection Agency (USEPA) promulgated a new drinking water method, 524.3. Due to advances in analytical instrumentation, Method 524.3 allows laboratories to modify purge and trap and GCMS conditions. Currently the USEPA is investigating the option of using Nitrogen as the purge gas in a new drinking water method, 524.4. This application note will explore purge and trap conditions for both Helium and Nitrogen purge gases.<h4>Discussion: &nbsp;</h4>When the USEPA published Method 524.3, they allowed some method flexibility. However, the method still required Helium as the purge gas. Due to fluctuations in the price and availability of high purity Helium, the USEPA has drafted Method 524.4 which would allow for high purity Nitrogen to be used for the purge gas.&nbsp;Method 524.4 provides the same flexibility as Method 524.3, thus method parameters can be modified in order to optimize purge and trap cycle times. Although the new method allows for a shorter desorb time, moisture build up can still be a problem as the new preservation scheme causes effervescing in the sparge vessel. EST has two features that can aid in moisture control and the “foaming” caused by the effervescing. First, EST has a foam sensor to detect any issues with foaming. The foam sensor for the Encon Evolution has a unique placement above the bulb of the sparge vessel, thus allowing the bulb to control the effervescing bubbles and not sending a false positive signal to the software causing the sample sequence to be aborted. Secondly, the Encon Evolution utilizes an 8 port valve instead of a 6 port valve. This unique engineering has the advantage of excluding the Moisture Reduction Trap (MoRT) from the desorb pathway thus aiding in moisture control for the system. Furthermore, the Centurion WS has the ability of taking samples from the vials without moving the samples. This eliminates opportunities for vial movement errors that would negatively impact productivity.<h4>Experimental:&nbsp;</h4>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Encon Evolution purge and trap concentrator</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS Autosampler </a>were interfaced to a GC/MSD. The purge and trap concentrator was configured with a Vocarb 3000 (K) analytical trap. A chiller unit capable of keeping the sample vials cooled below 10°C was installed on the Centurion WS autosampler. The experimental parameters are listed in Tables 1 and 2.<h4>Conclusion:&nbsp;</h4>The Encon Evolution and Centurion WS performed very well using both the Helium and Nitrogen purge gases and the 440ml and 390ml purge volumes. The Nitrogen and the Helium purge gases met USEPA method 524.3 criteria. Furthermore, the 440ml purge volume and the 390ml purge volume produced comparable results. Overall, the principal difference between the two purge gases was exhibited in the compound response. When examining the overall compound response factors over the curve range, it is evident that the analytes’ responses are slightly lower with the Nitrogen purge gas as opposed to the Helium purge gas.<h3>3. Shimadzu: Ultra-Sensitive Analysis of β-cyclocitral in Water Using Solid Phase Micro Extraction and Gas Chromatography–Mass Spectrometry</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_022_en_c7d7b3ef8a.pdf">Full PDF for download</a></li></ul><h4>User Benefits</h4><ul><li>SPME-GC-MS supports effective monitoring of water environments</li><li>Excellent sensitivity, achieving quantification of β-cyclocitral in water within the ultra-trace level</li><li>SPME provides a solvent-free extraction, efficient, and highly sensitive method for detecting β-cyclocitral&nbsp;</li></ul>Cyanobacterial blooms, commonly known as algal blooms, cause rivers and lakes to turn vividly green due to the excessive growth of cyanobacteria. This phenomenon is caused by factors such as global population growth, industrial pollution, and rising water temperatures caused by climate change. 1)Cyanobacterial blooms produce volatile organic compounds (VOCs) like β-cyclocitral and β-ionone, which cause unpleasant odors and reduce the quality of drinking water and aquatic products. This leads to consumer complaints and economic lossesin aquaculture and water treatment.&nbsp;Detecting and quantifying β-cyclocitral (Figure. 1) at trace levels is therefor essential for effective water management. However, conventional solvent extraction methods often fail to detect βcyclocitral, as it requires acidification or heating to be effectively released from the matrix. 2)&nbsp;In contrast, solid phase microextraction (SPME) enables efficient detection by facilitating the thermal desorption of β-cyclocitral from sample matrices onto the fiber. Moreover, SPME reduces solvent use and shortens sample preparation time compared to traditional extraction techniques, making it a suitable approach for the analysis of thermally induced volatile compounds like βcyclocitral.&nbsp;This application news describes the suitability of β-cyclocitral analysis using SPME automatic injection (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=AOC-6000+Plus">AOCTM-6000 Plus</a>) and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2020+NX">GCMS-QP2020 NX</a> of Shimadzu. The developed method enables highly sensitive quantitation of β-cyclocitral, achieving detection at the pg/mL level.<h4>Analytical Conditions</h4>β-cyclocitral in water was analyzed using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2020+NX">GCMS-QP2020 NX</a> of Shimadzu equipped with the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=AOC-6000+Plus">AOC-6000 Plus autosampler</a> as shown in Figure 2. The detailed analytical conditions of instrument was provided in Table 1. For the SPME analysis, 50/30 μm DVB/CAR/PDMS fiber was used, and SH-PolarWax (30 m × 0.25 mm I.D., 0.25 μm) was used as the analytical column. The AOC-6000 Plus supports various injection techniques, including liquid injection, headspace (HS) injection, and solidphase microextraction (SPME) injection. Furthermore, sample preparation and preprocessing in the AOC-6000 Plus are automatically carried out during injection into the GC system, improving efficiency and reproducibility.<h4>Conclusions&nbsp;</h4>In this application news, SPME-GC-MS method was developed and validated for the ultra-sensitive quantitation of β-cyclocitral in water using the Shimadzu GCMS-QP2020 NX coupled with the AOC-6000 Plus. The method demonstrated quantification capability down to the picogram-per-milliliter (pg/mL) level, excellent linearity (R² &gt; 0.999). Accuracy and precision were confirmed with a recovery of 105.3% and %RSD of 0.7. These results confirm the reliability and suitability of the SPME-GC-MS method for ultra-trace quantification of β-cyclocitral in environmental watersamples.

News from LabRulezGCMS Library - Week 37, 2025

<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=45&amp;search=USEPA+Method+524.2">USEPA Method 524.2</a> calls for purge and trap sampling coupled with a Gas Chromatograph (GC) and Mass Spectrometer (MS) for separation and analysis. It has an extensive list of compounds and requires lower detection limits due to its use in drinking water testing. A 20% relative standard deviation for compound response factors is required across the calibration curve while the calibration check standard analytes have to be within 30% of the expected concentration. Currently, this method calls for a 5mL or 25mL purge volume and a four minute desorb time. These method requirements can pose a challenge for the analyst due to the amount of moisture that is created.&nbsp;The negative effects of the increased water vapor include instability of the chromatography, band eluting and poor peak shape to name a few. A side effect of this instability is sample re-runs and lost laboratory productivity. In addition, a common practice for mitigating moisture is increasing the GC inlet split rate. This poses yet another difficulty as the increased split rate can result in reduced sensitivity. EST Analytical’s eight port valve in the Evolution purge and trap concentrator aids in limiting the water exposure because the water management of the system is not part of the desorb pathway. This feature also enables laboratories to use a smaller split ratio at the GC inlet thus increasing sensitivity.<h4>Experimental:&nbsp;</h4>The sampling system used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Evolution purge and trap concentrator</a> and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler</a>. The concentrator was affixed with a Vocarb 3000 trap and connected to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890A">Agilent 7890A GC</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5975C">5975C inert XL MS</a>. The GC was configured with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=7&amp;search=Restek+Rxi-624+Sil+MS">Restek Rxi-624 Sil MS</a> 30m x 0.25mm x 1.4µm column. The purge and trap and GC/MS parameters used for this study are listed below.<h5>Purge and Trap Parameters</h5><ul><li>Concentrator: EST Evolution</li><li>Trap type: Vocarb 3000</li><li>Valve oven temperature: 130 °C</li><li>Transfer line temperature: 130 °C</li><li>Trap temperature: 35 °C</li><li>Moisture Reduction Trap (MoRT) temperature: 39 °C</li><li>Purge time: 11 min</li><li>Purge flow: 40 mL/min</li><li>Dry purge Temp.: Ambient</li><li>Dry Purge Flow: 40mL/min</li><li>Dry Purge Time: 1.0 min &nbsp;</li><li>Desorb pressure Control: ON</li><li>Desorb Pressure: 5psi</li><li>Desorb time: 4 min</li><li>Desorb preheat delay: 15 sec</li><li>Desorb temperature: 250 °C</li><li>MoRT bake temperature: 210 °C</li><li>Bake temperature: 260 °C</li><li>Sparge vessel bake temperature: 110 °C</li><li>Bake time: 6 min</li><li>Bake flow: 70 mL/min</li></ul><h5>Auto-Sampler (EST Centurion WS):</h5><ul><li>Sample type: Water</li><li>Water volume: 25 mL</li><li>Internal standard volume: 5 µL</li></ul><h5>GC/MS Parameters</h5><ul><li>System: Agilent 7890A GC / 5975C inert XL MS</li><li>Inlet: Split mode, 220 °C, 40:1 split ratio, 12.153 psi head pressure</li><li>Column: Restek Rxi-624Sil MS, 30 m × 0.25 mm × 1.4 µm</li><li>Oven program: 45 °C (1 min) → ramp 15 °C/min → 220 °C, hold 1.33 min (total run ~14 min)</li><li>Column flow rate: 1 mL/min helium</li><li>Total flow: 44 mL/min</li><li>Source temperature: 230 °C</li><li>Quadrupole temperature: 150 °C</li><li>Transfer line temperature: 180 °C</li><li>Scan range: m/z 35–300, 5.2 scans/sec</li><li>Solvent delay: 0.7 min</li></ul>A calibration curve was established with a linear range of 0.25 to 40µg/L using the USEPA Method 524.2 standards from Restek. After the curve was determined, method detection limits were ascertained by running a series of seven replicate 0.25 µg/L standards and calculated using the procedure outlined in 40 CFR Part 136 Appendix B. Finally, seven 20 µg/L standards were examined in order to verify the precision and accuracy of the analysis. The results of this study are displayed in Tables 1 and 2 while Figure 1 presents a 20 µg/L standard GC/MS chromatogram.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_3_Compound_Linearity_and_Response_Factor_Table_f63b77844f.jpg" alt="EST Analytical: Table 1 - Compound Linearity and Response Factor Table" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_3_Compound_Linearity_and_Response_Factor_Table_f63b77844f.jpg 153w," sizes="100vw" width="1104" height="1126"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Table_4_MDL_and_Precision_and_Percent_Recovery_Table_27572600f0.jpg" alt="EST Analytical: Table 2 - MDL and Precision and Percent Recovery Table" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Table_4_MDL_and_Precision_and_Percent_Recovery_Table_27572600f0.jpg 186w," sizes="100vw" width="1358" height="1143"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/EST_Analytical_Figure_1_20mg_L_Standard_Chromatogram_7ff795984b.jpg" alt="EST Analytical: Figure 1 - 20 µg/L Standard Chromatogram" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_EST_Analytical_Figure_1_20mg_L_Standard_Chromatogram_7ff795984b.jpg 245w," sizes="100vw" width="1431" height="789"><h4>Conclusions:&nbsp;</h4>This study demonstrated the effectiveness of the Evolution/Centurion purge and trap sampling system. The results passed all of the USEPA Method 524.2 criteria for both linearity and detection limits. Since the Evolution bypasses the water management trap during the four minute desorb process, the amount of water effecting the experiments was limited. Furthermore, the forty to one split ratio at the GC inlet provided excellent detection limits as the system was more sensitive to the low level standard requirements of the method. The lower split rate has an added benefit of reducing laboratory helium consumption when setting it against other system’s higher split ratios. Finally, the precision and percent recovery results showed the reliability of the system in producing accurate experimental findings.

USEPA 524.2 Method Validation Using the Evolution Purge and Trap Concentrator and the Centurion WS Autosampler

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 15th September 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you posters by Agilent Technologies / ASMS, Shimadzu / ASMS and application note by EST Analytical!<h3>1. Agilent Technologies / ASMS: Beyond Aligners: Unmasking Hidden Extractables and Leachables in Orthodontic Devices</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_7250_extractables_leachables_asms_2025_tp_318_en_ucsf_3e88cfbf5c.pdf">Full PDF for download</a></li></ul>Increasingly popular in orthodontics, clear aligners promised to users’ improved comfort, compliance and flexibility. It also came with prolonged intraoral exposure. The literature on the potential for leaching components of the polymer used to manufacture the invisible aligners is sparse. Despite the benefits, user submitted cases in the FDA retrospective analysis report several adverse effect ranging from swelling, hives, itchiness and even difficulty breathing1 . Previous works examined the potential of leaching in retainers but used conditions far from the in-vivo setting2 . We used samples closest to user conditions and harnessed the power of Gas Chromatography High Resolution Mass Spectrometry (GC-HRMS) and the power of curated and annotated libraries to find candidate compounds that could be at the origin of the reported adverse effects. We also used multivariate statistics to establish relationships between the compounds and metadata.<h4>Experimental</h4><h5>Sample Analysis&nbsp;</h5>Samples were analyzed using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7250">Agilent 7250 accurate mass GC-qTOF</a> equipped with the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890+GC">8890 GC</a> and a DB-5MS UI column (30m x 0.25 x 0.25). The inlet temperature was 280°C and the transfer line temperature was 325°C. The oven program was as follows: 50°C for 1 min, ramp at 25°C to 170°C, hold for 1 min; then ramp at 15°C to 300°C, hold for 10 min; then ramp at 20 °C to 325°C and hold for 5 min. The solvent delay was 4 min. The data were acquired in electron ionization (EI) mode using mass range 45 to 1000 m/z. The source temperature was 230°C, and the emission current was 5 µA. A mix of alkanes was run along with the samples and blanks and an Extractables and Leachables (E&amp;L) standard mixture was run as a quality check.&nbsp;<h5>Data Analysis&nbsp;</h5>Retention indices were used in consolidating library matches in both the Agilent HRMS E&amp;L library and the NIST23 library. Data analysis was conducted on Unknown Analysis software from Agilent that performs compound annotation based on library matching and retention index. All compounds were individually reviewed based on ExactMass, retention index delta and library match factor (Figure 2). Canonical Correlation Analysis was performed using the FactoMineR package in R.<h4>Conclusions</h4>The aligners used in the current study were approved in the late 90s when E&amp;Ls methods were not as prominent or sensitive as they are today. This study stands out with:&nbsp;<ul><li>The first report of numerous E&amp;L compounds with known potential adverse effects in a population of clear aligner users&nbsp;</li><li>Providing an insight of the relationships between E&amp;Ls and user’s metadata such as age, DWT and TSS&nbsp;</li><li>Providing the necessary libraries to find parent compounds and their potential metabolites</li></ul><h3>2. EST Analytical: Optimization of 1,4-Dioxane and Ethanol Detection Using USEPA Method 8260</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_1_4_Dioxane_and_Ethanol_by_8260_App_Note_b669c79f53.pdf">Full PDF for download</a></li></ul>During the manufacture of pharmaceuticals, 1, 4-Dioxane is used as a cleansing agent. It is also a byproduct of plastic manufacturing. The most likely exposure to 1, 4-Dioxane is at an industrial site. However, if any 1, 4-Dioxane is released into the environment during manufacturing there is a potential for it to migrate into ground water. The fact that 1, 4-Dioxane is so miscible in water makes degradation of the chemical challenging. Ethanol, on the other hand, has been a popular gasoline additive. Since it burns more quickly and completely than gasoline, emissions from car exhaust are decreased. The downside of this is underground storage tank leakage and fuel spills cause ground water and drinking water to be contaminated with both the fuel and the ethanol additive. Since ethanol is also very miscible in water, the detection of ethanol contamination in water can be difficult.&nbsp;There have been several innovations that help overcome the obstacles of detecting 1, 4-Dioxane and Ethanol. The first one is the SIM mode of the mass spectrometer. This mode allows better detection of hard to extract compounds. Furthermore, mass spectrometers are now equipped to run SIM/Scan, this not only helps detect more difficult compounds, but also enables the detection of an extensive list of USEPA Method 8260 compounds without having to run the samples twice. Advancements in purge and trap sampling have also facilitated better detection of these compounds. Most effective in this has been the ability to heat the samples. However, there are drawbacks to better detection. The most problematic of these is the tendency of 1, 4-Dioxane and Ethanol to “stick” to the glass ware. This susceptibility has caused many headaches in environmental labs.&nbsp;This application note will investigate seven variations of purge and trap sampling. The data will then be evaluated in order to recommend the optimum purge and trap sampling parameters for your lab.<h4>Experimental</h4>The sampling system used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Evolution concentrator</a> affixed with a Vocarb 3000 trap. The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler</a> equipped with the syringe option was employed as the autosampler. The separation and analysis were performed by an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7890A">Agilent 7890A Gas Chromatograph (GC)</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=5975C">5975C inert XL Mass Spectrometer (MS)</a>. The GC was configured with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=9&amp;search=Rxi-624+Sil+MS">Restek Rxi-624 Sil MS</a> 30m x 0.25mm x 1.4µm column. The purge and trap parameters used for this study are listed in Tables 1 and 2 while Table 3 shows the GC/MS parameters.<h4>Conclusions</h4>All seven purge and trap parameter iterations passed the USEPA Method 8260 requirements for linearity and method detection limits. The problem with some of the experimental parameters was found in the carryover and precision and accuracy studies. The carryover using the traditional sparge vessel showed a large amount of carryover for the Ethanol and 1, 4-Dioxane. Since the carryover was so high, the precision and accuracy data suffered. The Fritless/Bulbless sparge vessel, on the other hand, displayed much lower carryover for the Ethanol and 1, 4-Dioxane especially when the patented sparge bake was not used. However, the 1, 2, 4-Trichlorobenzene, Naphthalene and 1, 2, 3-Trichlorobenzene carryover after the 50ppb standard was above the lower limit of the curve. Thus, the sparge bake would be recommended in order to limit the carryover of the heavier compounds. The optimum purge and trap parameters proved to be the patented water extraction technique. This technique provided linearity and method detection limits that met the USEPA Method 8260 requirements, while providing excellent precision and accuracy data. During water extraction, the sample is transferred to an empty 40ml vial and then purged in the soil station of the Centurion. The “fresh” vial provides a clean sparge vessel for every sample thus limiting carryover for both the Ethanol and 1, 4-Dioxane and for the heavy compounds. This lack of carryover aided in providing optimum precision and accuracy and carryover results and would be the recommended method for examining these troublesome compounds.<h3>3. Shimadzu / ASMS: Quantitation of Acetaldehyde, Ethylene Oxide, 2-Chloroethanol, Ethylene Glycol, 1,4-Dioxane &amp; Diethylene Glycol in PEG 3350 by using dynamic headspace GC-MS/MS</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_2025_TP_301_ad1ab4ac3e.pdf">Full PDF for download</a></li></ul>Polyethylene glycol 3350 (PEG 3350) is used to treat occasional constipation and it is in a class of medications called osmotic laxatives. PEG 3350 is an addition polymer of ethylene oxide and water with formula H(OCH2CH2)n OH, in which n represents the average number of oxyethylene groups. The average molecular weight of PEG 3350 is 3015–3685 g/mol (Da). Acetaldehyde, Ethylene Oxide (EtO), 2-Chloroethanol (2-CE), Ethylene Glycol (EG), 1,4- Dioxane and Diethylene Glycol (DEG) are the probable impurities of PEG 3350. All these above impurities are highly toxic &amp; hazardous substances.&nbsp;As per the USP monograph, different chromatography techniques and sample preparation methods are used to quantify above mentioned impurities. This study reports a single sensitive and reliable analytical method for quantitation of all above impurities by using dynamic headspace (Trap) coupled with GC-MS/MS system. Limit of impurities and detail method of analysis are shown in table 1.This study reports highly sensitive single method for the simultaneous quantification of multiple probable impurities of PEG 3350 by using dynamic headspace (Trap) coupled with triple quadrupole gas chromatography (GC-MS/MS) system.&nbsp;<h4>Materials and methods&nbsp;</h4>For this study, individual impurity reference standards were procured from Sigma Aldrich, whereas PEG 3350 powder sample was procured from local medical store. 10% of PEG 3350 powder sample solution (as such sample solution) and respective levels of matrixmatched calibration standard solutions were prepared in acetonitrile. Standard addition method was used to quantify impurities in the PEG 3350 sample. This method was part validated with respect to (w.r.t) precision, linearity/accuracy and sample analysis. <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-TQ8050+NX">GCMS-TQ8050 NX</a> equipped with headspace sampler <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=HS-20+NX">HS-20 NX </a>(Trap) (Figure 1), manufactured by Shimadzu Corporation Japan, was used to quantify impurities in the PEG 3350 sample<h4>Conclusion</h4><ul><li>Trace level quantification of Acetaldehyde, EtO, 2-CE, 1,4-Dioxane, EG and DEG in PEG 3350 sample was successfully performed by using Shimadzu GCMS-TQ8050 NX with HS-20 NX (Trap) dynamic headspace sampler.</li><li>Dynamic headspace mode outperforms the current regulatory limits, delivering multifold times more sensitivity compared to other injection techniques.</li><li>Shimadzu GCMS-TQ8050 NX features a new highly efficient detector and superior noise reduction technology that enhance sensitivity and enables quantitation of impurities even at trace levels.</li></ul>

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News from LabRulezGCMS Library - Week 38, 2025

USEPA 524.2 Method Validation Using the Evolution Purge and Trap Concentrator and the Centurion WS Autosampler

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