Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 12th August 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!
<blockquote>
<h4>👉 <a href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></h4>
</blockquote>
<blockquote>
👉 Need info about different analytical techniques? Peek into <a href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.
</blockquote>
This week we bring to you a poster from <a href="https://gcms.labrulez.com/events/568">ASMS 2024</a> by LECO, applications and other documents by Agilent Technologies, and Shimadzu!
<h4>1. LECO: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/Leachables_Topical_Ointments_Sample_Prep_BTX_GC_TOFMS_Chroma_TOF_Sync_JB_ASMS_24_LPSS_325_c545e07c6d.pdf">Employing Novel Sample Preparation and Analysis by GC-TOFMS for Improved Target and Non-Target Detection of Leachables in Cream/Gel Drug Products</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
Introduction: Topical ointments are commonly used to treat diseases and skin conditions by introducing the active drug ingredient through the dermis. To ensure the safety of the product for consumers, the US FDA requires that these formulations undergo leachables studies to determine the presence of chemicals which may migrate into the product from the packaging materials. Topical ointments such as creams and gels often take the form of oil-in-water emulsions which presents a challenging matrix for these analyses. Since these emulsions cannot be analyzed directly, novel sample preparations must be developed. Even with improved sample preparation techniques, the resulting extracts can still be challenging for traditional GC-MS systems. In this collaborative study, two different sample preparation methods were employed to extract a group of five chemicals commonly found in metal packaging containers such as tubes and tins. Unspiked and blind spiked samples from extraction methods A and B were provided for analysis on LECO’s Pegasus® BTX GC-Time-of-Flight (TOF) MS system. The goal was to determine the ability of the system to effectively detect and identify these chemicals with a non-target approach by leveraging mass spectral deconvolution and a software tool (ChromaTOF® Sync) designed for the comparison of samples.
Conclusions
<ul>
<li>The Pegasus BTX GC-TOFMS successfully detected and identified all five spiked leachables in this non-target case study. Non-target analyses can be critically important for extractable and leachable studies to ensure drug product safety.</li>
<li>ChromaTOF Sync was used to successfully compare unspiked and blind-spiked ointment extracts to quickly find the leachable analytes which were present at significantly higher levels in the spikes. Automated deconvolution was crucial for uncovering the spiked analytes from the complex matrix interferences.</li>
<li>A brief demonstration of GCxGC separation power to improve the trace level identification of 9,10-anthracenedione in the presence of heavy matrix background was effectively demonstrated.</li>
</ul>
<h4>2. Agilent Technologies: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/an_residual_nmp_lithium_ion_battery_electrodes_5994_7677en_agilent_66bf9d9256.pdf">Analysis of Residual N-Methyl-2-Pyrrolidone (NMP) in Lithium-Ion Battery Electrodes</a></h4>
<ul>
<li>Application</li>
</ul>
An analysis approach using the Agilent 8697 headspace sampler with the Agilent 8860 GC system and flame ionization detector
Abstract: Accurately measuring N-methyl-2-pyrrolidone (NMP) residue is crucial for ensuring appropriate control of electrode quality in lithium-ion battery manufacturing. This necessitates the extraction of residual NMP from battery electrodes for subsequent gas chromatography (GC) analysis. Two common extraction approaches include liquid extraction (LE) of NMP from electrodes and heated extraction through a headspace sampler. This application note describes an NMP analysis method using headspace-based extraction and GC analysis with a flame ionization detector (FID). Residual NMP analysis was then conducted on real electrode samples to compare the results between headspace sampling (HS) and LE techniques.
Conclusion: In this study, a method for analyzing residual NMP in electrodes was developed using the Agilent 8697 headspacesampler coupled with the Agilent 8860 GC system and FID. The method&#39;s investigation assessed the system&#39;s performance in terms of matrix-matched calibration, quantitation precision, detection limit, and system carryover. The HS approach demonstrated an excellent detection limit and quantitation precision for targeted NMP analysis. In the carryover test, no NMP was detected in the blank run immediately after analyzing a blank cathode spiked with 100 µg NMP. The comparison between HS and LE analytical methods showed that HS could accurately quantify NMP in anode samples. The recovery rate of NMP from cathodes using the HS technique was approximately 65 to 78% of that achieved by the LE-based method. Given its operational simplicity and quantitation precision, HS is suitable for the process control of an established electrodes manufacturing route, while LE is recommended for the development of manufacturing processes and troubleshooting electrode quality issues.
<h4>3. Agilent Technologies: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/flyer_5q_gc_column_campaign_5994_7659en_agilent_5f55755564.pdf">Get the Most from Your MS Agilent J&amp;W DB-5Q and HP-5Q GC columns</a></h4>
<ul>
<li>Other</li>
</ul>
<h5>Agilent J&amp;W DB-5Q and HP-5Q GC columns</h5>
Meet the new gold standard for GC/MS
Agilent J&amp;W 5Q GC columns are designed to ensure optimal analyte delivery to your quadrupoles. They combine industry-leading ultra inert performance with ultra low-bleed technology, setting a new standard for GC/MS column reliability and productivity.
<ul>
<li>Ultra low-bleed performance enhances data accuracy with high spectral fidelity and stable baseline integration.</li>
<li>Ultra inert performance increases sensitivity for active, trace-level analytes and provides balanced deactivation for multiclass analyte panels.</li>
<li>Ultrafast conditioning and outstanding column durability improve uptime by minimizing the frequency of column changes.</li>
<li>Identical selectivity to current 5ms columns simplifies adaptation to existing retention time libraries and retention time locking.</li>
<li>Compatibility with any GC/MS system ensures a seamless fit for all Agilent GC platforms.</li>
</ul>
<h4>4. Shimadzu: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c180_e101_c8f3739683.pdf">GC/GC-MS Glass Insert/Liner Selection Guide</a></h4>
<ul>
<li>Guides</li>
</ul>
<h5>Contents</h5>
1. Introduction
<ul>
<li>1-1. Glass Inserts/Liners 3</li>
<li>1-2. Sample Injection Unit/Injection Method 4</li>
</ul>
2. Glass Insert Selection
<ul>
<li>2-1. Glass Insert Selection by GC Model/Sample Injection Unit<ul>
<li>GC-2030/GC-2050</li>
<li>GC-2010 series</li>
<li>GC-2014 series</li>
<li>GC-2025</li>
<li>HS-10</li>
</ul>
</li>
<li>2-2. Glass Insert Selection by Application<ul>
<li>SPME/SPME Arrow</li>
<li>Aqueous Solvent Analysis</li>
<li>SPL (Split/Splitless)</li>
</ul>
</li>
</ul>
3. Selection Guide
4. All Glass Insert List
<ul>
<li>4-1. Glass Insert Compatible Instruments</li>
<li>4-2. Glass Insert Information Table</li>
</ul>
5. Accessories

News from LabRulezGCMS Library - Week 33, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 2nd September 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote><h4>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></h4></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 to you applications and technical notes by Agilent Technologies, Shimadzu, and Thermo Fisher Scientific!<h4>1. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00738_en_be6d7795f2.pdf">Residual NMP and Solvent Analysis in Lithium-ion Battery Cathode</a></h4><ul><li>application</li></ul>User Benefits<ul><li>Analyze residual NMP and similar solvent structures in the cathode of lithium-ion batteries.</li><li>Optimize drying conditions in the cathode manufacturing process and quantify the amount of residual solvents for quality control.</li><li>Minimize equipment footprint by combining Brevis GC-2050 and GCMS-QP2050.</li></ul>Introduction: Lithium-ion batteries (LiB) consist of cathode and anode, electrolyte, separator, etc. The electrodes are formed by coating a slurry of active material, conductive additives, binders, etc., mixed in an organic solvent, on a metal film (current collector) and then dried. N-Methyl-2-pyrrolidone (NMP) is known as an organic solvent used in solvent-based slurries, and especially for quality control of the cathode, the residual amount of NMP in the cathode is examined during the drying process.In this application, a simple analysis method for residual NMP in the cathode of lithium-ion battery NCM (nickel-cobalt-manganese ternary material) using GC-FID with headspace method is introduced. In addition, results of qualitative analysis of other solvents remaining in the NCM cathode using GC-MS and comparison of residual solvent amounts in five different cathodes with different drying processes are also presented.Summary: By using headspace GC-FID, it is possible to easily analyze residual NMP in the cathode and quantify residual solvents without the need for preprocessing. Additionally, with headspace GC-MS, qualitative analysis of residual organic solvents can also be performed.Using compact models such as Brevis GC-2050 or GCMS-QP2050 allows for minimization of experimental space and detailed analysis of solvent analysis for each drying process. This can be applied to quality control and research and development in the cathode manufacturing process.<h4>2. <style type="text/css"></style>Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_forensic_triple_quad_mrm_database_toxicological_5994_7594en_agilent_0dbf3ad769.pdf">A Forensic Triple Quadrupole GC/MS MRM Database for Forensic and Toxicological Workflows</a></h4><ul><li>application</li></ul>Abstract: Systematic toxicological analysis is crucial in forensic laboratories, requiring robust and reliable analytical methods. Gas chromatography coupled to triple quadrupole mass spectrometry (GC/TQ) is a versatile and widely used technique that provides uniform results across instruments and laboratories. The aim of this study was to establish a database of multiple reaction monitoring (MRM) transitions for toxicologically relevant compounds amenable to GC/MS. The resulting curated database includes 176 entries, including 154 unique compounds with up to 12 transitions per compound. The database allows for instantly building methods for targeted screening and confident quantitation of GC-amenable, forensic, and toxicologically relevant compounds.The database is available for download as a CSV file in Appendix 1 of this application note.Conclusion: The forensic toxicology database, with a curated set of 1,803 MRM transitions for 176 toxicologically relevant compounds, was successfully developed. The compounds included &nbsp;benzodiazepines, antidepressants, opioids, and drugs of abuse. The application of this MRM method to an authentic real-world sample showcased its ability to detect and quantitate toxicants at trace levels due to the high sensitivity and selectivity of the MS/MS approach. This approach addresses limitations when relying solely on full scan data acquisition mode.The developed MRM database can be used for simplified data acquisition method creation, providing a valuable resource for the development of screening and quantitation methods in forensic labs. The developed MRM curation workflow showed promise for continuous expansion, offering a uniform and practical approach for adding new chemicals to the database.<h4>3. <style type="text/css"></style>Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/te_hydroinert_ei_source_functionality_longevity_5994_7680en_agilent_991ba3a869.pdf">Optimizing HydroInert EI Source Functionality and Longevity</a></h4><ul><li>technical note</li></ul>Introduction: The benefits of hydrogen in gas chromatography (GC) are widely accepted, as it can be generated in the lab in a cost-effective manner, produces fast chromatography, and allows for higher sample throughput. Since hydrogen is a reactive gas, hydrogenation and dechlorination reactions can and do occur in the mass spectrometer electron ionization (EI) source. These reactions can make applying hydrogen carrier gas to many applications difficult. A specially designed extractor source for the Agilent Inert Plus GC/MSD and triple quadrupole GC/MS systems address these hydrogen-related issues and improves performance with hydrogen carrier gas. The Agilent HydroInert source (Figure 1) with H2 carrier gas retains mass spectral fidelity and can allow users to continue to use existing helium-based mass spectral libraries.When adopting hydrogen for GC/MS analysis, there are several factors to consider. First, hydrogen is a reactive gas, and it may potentially cause chemical reactions in the inlet, column, and sometimes the MS EI source, which can change analysis results. To address potential issues in the MS source while using hydrogen, the HydroInert source was used. Additional information can be found in the Agilent technical overview of the HydroInert source.1 Second, for GC/MS applications, hardware changes in the gas chromatograph and mass spectrometer are recommended when switching to hydrogen carrier gas. The Agilent Helium to Hydrogen Carrier Gas Conversion Guide2 describes in detail the steps for conversion from helium to hydrogen carrier gas. Lastly, it is recommended that when working with flammable or explosive gases, laboratories maintain proper safety in gas handling and use. Further information on the safe use of hydrogen can be found in the Agilent Hydrogen Safety Manual3 and Hydrogen Safety for the Agilent GC System Guide.4,5Conclusion: Agilent HydroInert source longevity is dependent on application and method conditions. However, by using some of the best practices highlighted above, the longevity of HydroInert parts can be prolonged. The HydroInert source cannot be mechanically or chemically cleaned, thus when source parts show reduced functionality, replacement of the recommended parts above is required to restore functionality. Replacement intervals will be method- and application-dependent.<h4>4. <style type="text/css"></style>Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/AN_002784_Improvements_for_the_analysis_of_volatile_VOC_and_very_volatile_VVOC_organic_compounds_using_In_Tube_Extraction_Dynamic_Headspace_ITEX_DHS_and_cryogen_free_refocusing_4_bd362df5a5.pdf">Improvements for the analysis of volatile (VOC) and very volatile (VVOC) organic compounds using In-Tube Extraction- Dynamic Headspace (ITEX-DHS) and cryogen-free refocusing</a></h4><ul><li>application</li></ul>Goal: To demonstrate how the technological development of dynamic headspace extraction/enrichment techniques, such as ITEX-DHS (In-Tube Extraction-Dynamic Headspace) coupled to a cryogen-free refocusing in the PTV injector, enables the achievement of lower detection limits for volatile and very volatile organic compounds.Keywords: VOC, VVOC, water, dynamic headspace, ITEX-DHS, refocusing, PTV, TRACE 1610 GC, TriPlus RSH SMART autosamplerConclusion: The use of the ITEX-DHS technique for headspace enrichment coupled to cryogen-free refocusing into the PTV injector is a suitable approach for trace level analysis of VOC and VVOC in water samples, offering a clean method to comply with more stringent regulatory limits of quantitation.<ul><li>Combined with refocusing prior to transfer into the column and SIM acquisition mode, the ITEX-DHS technique achieves limits of quantification at low ppt levels and extrapolated limits of detection in the sub-ppt range, even for VVOC such as vinyl chloride, with high recovery precision (&lt;5% RSD) and a linear response over four orders of magnitude.</li><li>ITEX-DHS offers a flexible enrichment technique capable of handling low and high concentrated samples to comply with different sensitivity requirements.</li><li>The complete workflow, from method set up to data processing and reporting, can be fully controlled through Chromeleon CDS, which greatly facilitates operations on a day-to-day basis.</li></ul>

News from LabRulezGCMS Library - Week 36, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 9th September 2024? 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 to you applications by Agilent Technologies, Shimadzu, and Thermo Fisher Scientific and poster by LECO from ACS meeting!<h4>1. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_002952_gc_ms_isq_environmental_an002952_na_en_9738609742.pdf">Adhering to U.S. EPA Method 524.2 for the analysis of volatile organic compounds in drinking water</a></h4><ul><li>application</li></ul>Goal: Demonstration of a routine analytical method that meets the requirements outlined in U.S. EPA 524.2 for the quantitation of volatile organic compounds (VOCs) in drinking water, using the Teledyne LABS Tekmar Lumin Purge and Trap (P&amp;T) concentrator paired with the AQUATek LVA autosampler system along with a Thermo Scientific™ ISQ™ 7610 MS system coupled with a Thermo Scientific™ TRACE™ 1610 gas chromatograph (GC) and Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS). Method linearity, method detection limit (MDL), precision, and accuracy were assessed to evaluate method performance.Introduction: Analytical testing labs play a crucial role in monitoring surface, ground, and drinking water for volatile organic compounds (VOCs). Common by-products in the processing of household and industrial products, VOCs can contaminate water sources, potentially harming the environment and public health. To safeguard against this, labs use the U.S. EPA Method 524.21 to test water for the presence of VOCs, including four trihalomethane disinfection by-products. This procedure utilizes Purge and Trap (P&amp;T) procedures to remove VOCs with high volatility and low water solubility from water samples, followed by gas chromatography-mass spectrometry (GC-MS).Conclusion: The TRACE 1610 GC, the ISQ 7610 system, and the Tekmar Lumin P&amp;T with the AQUATek LVA autosampler system together offer benefits for executing U.S. EPA Method 524.2. The Tekmar Lumin P&amp;T concentrator enhances sample throughput through efficient trap cooling and moisture control, thus reducing peak interference and extending GC column life. The ISQ 7610 system’s VPI and ExtractaBrite ion source allow ionization source and analytical column replacement without venting the instrument, ensuring minimal downtime, and the XLXR™ detector offers extended linear dynamic range. The collective technology addresses routine VOC analysis challenges, ensuring robust sensitivity, maximized output, and consistent method compliance. The ISQ 7610 system equipped with the VPI coupled with the Tekmar Lumin P&amp;T and the AQUATek LVA autosampler exceeds all the requirements outlined in U.S. EPA Method 524.2 for analysis of VOCs in drinking water:<ul><li>Excellent linearity for all compounds was demonstrated with the %RSD of the calibration response factors passing all method requirements.</li><li>MDL and precision for seven 0.5 ppb standards showed no interference from excessive water and produced very reproducible results. The average MDL result for all 83 target compounds was 0.06 ppb with a precision of 4.06%.</li><li>The precision for n=31 samples over 189 injections displayed &lt;30% RSD accuracy for all compounds as the method requires. The average precision for all 83 target compounds and 2 surrogates gave a %RSD of 6.43% with an accuracy of 98% recovering the compounds. Individually, 4-bromofluorobenzene and 1,2-dichlorobenzene-d4 had a 7.68% RSD with an accuracy of 98% and 4.95% RSD and an accuracy of 95%, respectively, over 189 injections and almost four days of uninterrupted analysis.</li></ul><h4>2. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00706_en_f95bd4b605.pdf">Analysis of Denatured Fuel Ethanol with Brevis GC-2050 Using ASTM D5501</a></h4><ul><li>application</li></ul>User Benefits<ul><li>The compact design of the Brevis GC-2050 enables space-saving in the laboratory.</li><li>As an alternative gas for helium, hydrogen can be used as the carrier gas.</li><li>&nbsp;Analysis of ethanol and methanol in fuels based on ASTM D5501 is possible.</li></ul>IntroductionBioethanol has attracted attention as a form of renewable energy which can be obtained from biomasssuch as corn and sugar cane. ASTM D5501 provides a test method for determination of the concentrations of ethanol and methanol in fuels for concentrations of ethanol from 20 to 100 wt% and concentrations of methanol from 0.01 to 0.6 wt%.In this Application News article, measurements of the purity of ethanol containing gasoline as a denaturant as specified in ASTM D5501 were carried out with a Brevis GC-2050 gas chromatograph, using helium and hydrogen asthe carrier gases.ConclusionEthanol purity tests were carried out as provided in ASTM D5501 using a Brevis GC-2050 gas chromatograph. The splitter linearity test showed no inlet discrimination so that accurate qualitative analysis could be made for denatured fuel ethanol with the wide boiling range components regardless of whether helium or hydrogen was used as the carrier gas.<h4>3. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_aldehydes_beer_pal3_autosampler_5977c_gc_msd_5994_7633en_agilent_1fe3b8541c.pdf">Analysis of Aldehydes in Beer by Agilent PAL3 Autosampler and 5977C GC/MSD</a></h4><ul><li>application</li></ul>AbstractThis application note describes a method for quantitation of four aldehydes (hexanal, furfural, phenylacetaldehyde, and trans-2-nonenal) responsible for off-flavors in beer using an Agilent 8890/5977C GC/MSD with an Agilent PAL3 (SPME) autosampler. The method used fully automated, solvent-free extraction and on-fiber derivatization. The aldehyde compounds were derivatized with the derivatization agent O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) using the on-fiber derivatization procedure. The derivatization agent was first adsorbed onto an Agilent 65 µm PDMS/DVB fiber. Next, the fiber was inserted into a 20 mL headspace vial containing a 2 mL beer sample with agitation at 60 °C for 30 minutes. Both extraction and derivatization procedures were automatically performed using the PAL3 autosampler. The method demonstrated excellent sensitivity, with detection limits of 0.0009 µg/L for hexanal, 0.52 µg/L for furfural, 0.015 µg/L for phenylacetaldehyde, and 0.003 µg/L for trans-2-nonenal. The limits of the quantification for the four compounds were 0.003, 1.72, 0.05, and 0.01&nbsp;µg/L, respectively. The four aldehydes were successfully quantified in four beer samples purchased from a supermarket. Good repeatability was demonstrated with RSD &lt; 4.9% based on three replicate injections of the four beer samples for all four&nbsp;aldehydes.ConclusionThis application note describes the quantitative analysis of four aldehydes (hexanal, furfural, phenylacetaldehyde, and trans-2-nonenal) responsible for off-flavors in beer using an Agilent 8890/5977C GC/MSD with a PAL3 (SPME) autosampler. This method offers the advantages of full automation, rapid analysis, solvent-free extraction, and on-fiber derivatization. With this automated solution, excellent sensitivity was demonstrated for the detection of hexanal (0.0009 μg/L), furfural (0.52 μg/L), phenylacetaldehyde (0.015&nbsp;μg/L), and trans-2-nonenal (0.003 μg/L). Four different brands of beer were analyzed, with hexanal detected in the range of 0.45 to 1.56 μg/L, furfural in the range of 6.62&nbsp;to 50.37 μg/L, phenylacetaldehyde in the range of 6.64 to 10.51&nbsp;μg/L, and trans-2-nonenal in the range of 0.031 to 0.062&nbsp;μg/L. Good repeatability was demonstrated with RSD&nbsp;&lt;&nbsp;4.9% based on three replicate injections of the four beer samples for all four aldehydes.<h4>4. LECO: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/hf_acs21_lpss_284_c35134b9cd.pdf">Combining GC with MS and Olfactory Detection for a Variety of Food, Flavor, and Fragrance Analyses</a></h4><ul><li>Poster / ACS</li></ul>INTRODUCTIONGas chromatography (GC) coupled with mass spectrometry (MS) is an important tool for the characterization of a wide range of food, flavor, and fragrance samples. The components most likely to contribute to the aroma of a sample tend to be volatile and semi-volatile analytes, and GC-MS is well-suited for this type of analysis. Complex samples are effectively separated into the individual analyte components with GC. Time-of-Flight (TOF) MS detection provides important information towards the identification of these potentially important components of the sample with full m/z range data that can be library searched and that is also optimal for deconvolution algorithms. The incorporation of olfactory (O) detection with this data is particularly helpful for connecting the identified features with their contributions to the overall aroma or flavor. This type of sensory directed analysis highlights regions of interest and leads to specific analytes of interest for a focused review of the data. This combination of tools can separate and identify analytes and then determine those that are most important for contributing to the sensory characteristics of the sample. A variety of samples were analyzed with this combination of tools, and the benefits of using the information together are highlighted.CONCLUSIONSIn this work, the combination of a GC separation with MS and O for detection provided a powerful and efficient analytical platform to isolate individual analytes, identify those isolated analytes, and connect them to their sensory impacts. The olfactory data allowed for sensory directed analysis. In each case, the GC separation and full m/z range TOFMS data were crucial for determining the identification of the feature responsible for the characteristic aroma. This collection of tools was demonstrated for the characterization of the most aroma impacting components of a nutmeg essential oil, the distinction of sensory differences in cilantro, and the determination of an off-odor in beer.

News from LabRulezGCMS Library - Week 37, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 16th September 2024? 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 to you applications and other documents by Agilent Technologies, Shimadzu, Thermo Fisher Scientific, and LECO!<h4>1. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c146_e452_c8a53d60a2.pdf">Database for GC-MS(/MS) Aroma Analysis - Smart Aroma Database</a></h4><ul><li>Brochure</li></ul>Provides Efficient and Accurate Aroma Analysis Using GC-MS(/MS)Information on more than 500 compounds that contribute to aroma is registered in Smart Aroma Database™, enabling the objective evaluation and analysis of aroma compounds using GC-MS(/MS).1. Automatically Detects Aroma Compounds from Scan Measurements with High Accuracy2. Easily Narrows Down the Compounds that Contribute to the Aroma3. Enables High-Sensitivity Target Analysis Using MRM and SIM4. Supports a Variety of Systems<h4>2. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/br_5q_gc_column_campaign_5994_7596en_agilent_baca38e505.pdf">Agilent J&amp;W DB-5Q and HP-5Q GC columns</a></h4><ul><li>Brochure</li></ul><h5>Get the Most from Your MS</h5>As mass spectrometry continues to push the boundaries of sensitivity and speed, you need a column that can do the same<ul><li>Agilent J&amp;W 5Q GC columns are designed to ensure optimal analyte delivery to your quadrupoles. They combine industry-leading ultra inert performance with ultra low-bleed technology, setting a new standard for GC/MS column reliability and productivity.</li><li>Ultra low-bleed performance enhances data accuracy with high spectral fidelity and stable baseline integration.</li><li>Ultra inert performance increases sensitivity for active, trace-level analytes and provides balanced deactivation for multiclass analyte panels.</li><li>Ultrafast conditioning and outstanding column durability improve uptime by minimizing the frequency of column changes.</li><li>Identical selectivity to current 5ms columns simplifies adaptation to existing retention time libraries and retention time locking.</li><li>Compatibility with any GC/MS system ensures a seamless fit for all Agilent GC platforms. Agilent J&amp;W 5Q GC columns are available in high-efficiency, hydrogen-compatible, and backflushing dimensions.</li></ul><h4>3. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/AN_002784_Improvements_for_the_analysis_of_volatile_VOC_and_very_volatile_VVOC_organic_compounds_using_In_Tube_Extraction_Dynamic_Headspace_ITEX_DHS_and_cryogen_free_refocusing_4_bd362df5a5.pdf">Improvements for the analysis of volatile (VOC) and very volatile (VVOC) organic compounds using In-Tube Extraction-Dynamic Headspace (ITEX-DHS) and cryogen-free refocusing</a></h4><ul><li>Application</li></ul>GoalTo demonstrate how the technological development of dynamic headspace extraction/enrichment techniques, such as ITEX-DHS (In-Tube Extraction-Dynamic Headspace) coupled to a cryogen-free refocusing in the PTV injector, enables the achievement of lower detection limits for volatile and very volatile organic compounds.IntroductionVolatile organic compounds (VOCs) are a group of organic chemicals with low vapor pressure that can easily evaporate into the air, even at room temperature. These compounds can originate from various sources, including industrial processes, vehicle emissions, and natural sources. While VOCs are often associated with air pollution, they can also contaminate water, thus posing potential risks to human health and the environment.1 VOCs can enter water through direct discharges, atmospheric deposition, or runoff from contaminated areas. Common VOCs found in water include benzene, toluene, ethylbenzene, and xylene (BTEX), as well as chlorinated compounds such as trichloroethylene (TCE) and tetrachloroethylene (PCE). These compounds can cause adverse health effects, ranging from short-term irritation to long-term chronic conditions, depending on the concentration and duration of exposure.Regulatory authorities all over the world have established limits to control the maximum amount of VOCs in drinking water, groundwater, or surface water (e.g., Safe Drinking Water Act (SDWA) in the USA or the European Directive 2008/105/EC).2,3 Therefore, monitoring and analyzing VOCs in water play crucial roles in identifying and addressing potential contamination issues, guiding remediation efforts, and ensuring compliance with water quality regulations.4Common methods to analyze VOCs in water include headspace, purge and trap, solid-phase microextraction, and liquid-liquid extraction as possible sample preparation techniques employed to extract and concentrate VOCs before GC-MS analysis. As technology advances, continuous improvements in analytical methods and instrumentation contribute to more accurate and efficient VOC analysis, enhancing the ability to safeguard water resources and public health.When dealing with drinking water testing, the limits of detection are particularly challenging, requiring an efficient enrichment before GC-MS analysis.In-Tube Extraction-Dynamic Headspace (ITEX-DHS) is a sample preparation technique for the extraction and preconcentration of volatile compounds from different matrices, such as water, soil, or biological samples. One of the key advantages of ITEX-DHS is its high sensitivity and selectivity for volatile compounds. It allows for the extraction of low concentrated analytes from complex matrices while minimizing interference from non-volatile matrix components. Additionally, the technique offers an automated and efficient sampling process through a robotic autosampler, making it suitable for unattended and time-sensitive analyses.ITEX-DHS has found applications in various fields, including environmental monitoring, food analysis, and forensic science. Its versatility makes it particularly valuable in situations where trace-level analysis of volatile compounds is crucial. An example of the use of ITEX-DHS for the detection of odorants in water at ng/L level is reported in a previous application note.5In this study, the performance of the ITEX-DHS sampling technique has been evaluated for trace level detection of volatile and very volatile compounds (VVOCs) in water, in combination with peak refocusing into a Programmed Temperature Vaporizer (PTV) injector, to enhance peak shape and signal-to-noise ratio.<h4>4. LECO: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PEGBTX_EXPAND_YOUR_PFAS_ANALYSIS_203_821_689_d24746e8bb.pdf">Expand Your PFAS Analysis - Screen for Targets and Identify Unknowns Simultaneously</a></h4><ul><li>Application</li></ul>Key Words: PFAS, GC-MS, HR-MS, TOFMS, Environmental Analysis, Pollutants, Emerging Substances, Non-target, NTS, ScreeningBackground and DescriptionResearch into the prevalence of er- and polyfluoroalkyl substances (PFAS)—also known as “forever chemicals” due to theirp high stability in our environment and food chain continues to grow. At the same time, regulatory control of these species in our water and food supplies continues to gain momentum. However, analysis of PFAS in complex environmental samples can be challenging due to the enormous number and variety of PFAS chemicals. New analytical methods must be developed to monitor PFAS in the environment.This application focuses on the rapidly expanding area of PFAS analysis and highlights how screening for known PFASnote targets, as well as discovering and identifying unknown PFAS chemicals, can be performed using high-performance GC-TOFMS. New libraries are being developed to facilitate the screening of these pollutants in samples.ConclusionMeeting the growing environmental research and regulatory needs for PFAS analysis requires the use of powerful technologies to screen for known targets and to detect and identify unknown PFAS candidates. Here, sub-nominal mass GC-TOFMS, allowed simultaneous, full mass range, highly sensitive target, and NTS screening for PFAS in Anti-Fog/Demisting products, detecting a variety of both known PFAS and unknown PFAS candidates. The use of accurate mass GC-HR-TOFMS technology with EI and CI capabilities facilitated strong tentative identifications of the unknowns to be a class of fluorotelomer ethoxylates (FTEOs). This approach, together with the results obtained, suggests these technologies are an ideal choice for screening and identification of volatile and semi-volatile PFAS, in an array of sample types in complex matrices.

News from LabRulezGCMS Library - Week 38, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 23rd September 2024? 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 to you applications by Agilent Technologies, Shimadzu, Thermo Fisher Scientific, and a presentation by LECO!<h4>1. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_09_SSK_019_en_5e1bde719c.pdf">Analysis of Epichlorohydrin in Water using HS- GC/MS</a></h4><ul><li>Application</li></ul>User Benefits<ul><li>Water samples can be analyzed with a simple preparation.</li><li>Using a headspace autosampler, the analysis of epichlorohydrin in water quality can be performed conveniently.</li></ul>IntroductionEpichlorohydrin (ECH) is primarily used in the production of various resins (epoxy, ion exchange, etc.) and synthetic glycerin. Additionally, it is used as a stabilizer for carbon containing products in surfactants, plasticizers, dyes, and pharmaceuticals1). Some studies have demonstrated that damage to the nasal passages, respiratory tract and kidneys occurred in rodents exposed to epichlorohydrin. It has been observed that exposure to ECH induced a high nasal cancer response in rats, therefore, the United States Environmental Protection Agency (EPA) has classified epichlorohydrin as a “probable” human carcinogen (Group B2).According Water Pollutants of Water Environment Conservation Act, the permissible discharge limits of ECH in water were 0.03 to 0.3 mg /L by the classified area. The test method for ECH analysis in water is "Epichlorohydrin-Solvent Extraction/Gas Chromatography-Mass Spectrometry (ES 04608.1)" as the official test method of water pollution.2)The ES 04608.1 was used to extraction method with a large volume of solvent, it caused high consumption of solvent and long time of preparation. To solve these disadvantages, analysis of ECH in water in this application was performed using HS-20 NX headspace sampler without sample pretreatment.This application demonstrates the validation of a method for analysis of ECH in water samples using HS-GC/MS (Fig. 1) to meet the demanded levels of ES 04608.1 in Korea.ConclusionsThis Application news demonstrated the use of a Shimadzu GCMS-QP2020 NX coupled HS-20 NX for measurement of ECH in water. The proposed analytical method was with good validation parameters, such as linearity, MDL, LOQ, accuracy and precision which was satisfied the criteria of standard method (ES 04608.1) in Korea.<h4>2. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_ethylene_oxide_2_chloroethanol_8890_7010_gcms_5994_7720en_agilent_337dc4394d.pdf">Estimation of Ethylene Oxide and 2-Chloroethanol in Spices and Oilseeds Using QuEChERS Extraction and GC/MS/MS</a></h4><ul><li>Application</li></ul>AbstractThis application note demonstrates the use of an Agilent 8890 GC system coupled with an Agilent 7010 GC/MS triple quadrupole mass spectrometry system to detect and quantify ethylene oxide (EtO) and 2-chloroethanol (2-CE) simultaneously in foodstuffs such as flaxseed, cumin powder, and red chili powder. Sample preparation was done using QuEChERS extraction and a dispersive cleanup process followed by injection into GC/MS/MS through liquid injection. A limit of quantification (LOQ) of 10 ppb for both compounds was achieved in matrix. Average recoveries ranged from 75 to 86% for both compounds.IntroductionEtO is used to sterilize foods to eliminate insects and bacteria, such as salmonella. Ethylene chlorohydrin, or 2-CE, is a derivative produced by the reaction of EtO with chlorine ions present in foodstuff. Use of EtO is banned in the European Union (EU) due to its carcinogenic and toxic properties.Previously, methods for analysis of EtO (EtO and 2-CE) have been developed that include acidic conversion of EtO to 2-CE. These methods are time-consuming, labor-intensive, and require large quantities of harmful solvents. Due to the volatile nature of EtO, sample preparation is crucial. In December 2020, the EU Reference Laboratories (EURL) for Residues of Pesticides recommended a single-residue method for the analysis of EtO and 2-CE in sesame seeds using QuEChERS extraction followed by GC/MS/MS analysis. The method adopted in this work demonstrates the use of an automated liquid sampler for sample introduction to the 8890 GC system coupled with a 7010 GC/MS triple quadrupole mass spectrometry system.ConclusionAn accurate and rugged method was developed which meets the requirements of the EURL for a single-residue method that uses QuEChERS extraction followed by GC/MS/MS analysis for the analysis of EtO and 2-CE in flaxseed, cumin powder, and red chili powder. The LOQ of the method was demonstrated at 10 ng/g for all the tested matrices. Repeatable results are found for 6 successive replicates of matrix-based standards at 10 ng/g concentration levels for EtO and 2-CE. Excellent recoveries were obtained for both EtO and 2-CE in all tested matrices at 20 and 50 ng/g spiked concentration levels. Thus, this study demonstrates the usefulness of the developed method for the routine analysis of food samples for EtO and 2-CE at trace levels.<h4>3. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/An_advanced_integrated_GC_MS_MS_and_LC_MS_MS_workflow_for_the_comprehensive_analysis_of_pesticide_residues_in_food_a5878f2c6b.pdf">An advanced integrated GC-MS/MS and LC-MS/MS workflow for the comprehensive analysis of pesticide residues in food</a></h4><ul><li>Application</li></ul>GoalAnalysis of proficiency test (PT) samples to demonstrate the benefits of combining GC-MS/MS and LC-MS/MS with the innovative Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS) for improving laboratory efficiency in the analysis of multi-class pesticide residues in food.Keywords: Pesticide residues analysis, comprehensive pesticides workflows, QuEChERS, LC-MS/MS, GC-MS/MS, Chromeleon CDS, cross-confirmation, targeted quantitation, automated data review.BackgroundAccording to the World Health Organization, more than one thousand different pesticides are used to protect crops from pests to increase crop yields and to minimize deterioration of agricultural products during post-harvest storage and transportation. However, inappropriate use of pesticides can result in contamination of the food supply, making it essential to define and monitor pesticide residue targets to protect consumer health, support trade, and establish food regulatory control.1Consequently, laboratories are tasked to develop methods to detect, correctly identify, and quantitate hundreds of different pesticides and their transformation products in hundreds of different sample matrices, in compliance with Maximum Residue Levels (MRLs) set by regulatory bodies.Data analysis of pesticide residues in food typically requires numerous performance checks including retention time, ion ratios, calibration curves, recovery, and precision. Data review of thousands of data values in a single chromatographic run and checking compliance against quality control criteria such as the EC SANTE guidelines2 are some of the most time-consuming tasks in pesticides analysis.Therefore, it is essential that workflows cover a broad pesticides scope, are sensitive and robust, and are as productive and efficient as possible to achieve compliance with regulations while meeting business goals such as return on investment (ROI), sample turnaround times, and cost-per-sample targets.An innovative approachIn response to this challenge, new pre-configured “out of the box” pesticide workflows based on the latest Thermo Scientific™ GC-MS/MS and LC-MS/MS instruments and Chromeleon CDS 3 have been specifically designed for multi-class pesticides analysis.These solutions include the hardware, software, built-in instrument acquisition methods, and customizable data processing methods including view settings and report templates, along with details of sample extraction and consumables for fast implementation.This new approach, which enables the detection, identification, and quantitation of up to 700 pesticides by GC-MS/MS and LC-MS/MS, combines results in a unique software user interface to confirm the identity of residues quickly and accurately, especially those amenable by both techniques.This automated cross-confirmation increases confidence in the data by minimizing the risk of false positive and false negative results while increasing productivity by reducing the need for repeat sample injections when either the LC-MS/MS or GC-MS/MS analysis is subject to interference. This is especially the case for more difficult samples that contain high amounts of matrix co-extractives.Proof statementLaboratories are often required to undertake blind analysis of PT samples containing an unknown number of unspecified pesticides. Assessing PT samples is an independent and more realistic test of the laboratory’s methods and procedures.In this application brief, the analysis of PT samples was undertaken to evaluate the analytical performance of the new integrated GC-MS/MS and LC-MS/MS pesticides workflow and to illustrate the benefits of the new software features.<h4>4. LECO: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/O_12_Characterization_and_Quantitative_Hydrocarbon_Group_Type_Analysis_of_Plastic_Derived_Pyrolysis_Oils_by_G_Cx_GC_TOFMS_FID_0a253a5d5e/O-12-Characterization-and-Quantitative-Hydrocarbon-Group-Type-Analysis-of-Plastic-Derived-Pyrolysis-Oils-by-GCxGC-TOFMS-FID.pdf">Characterization and Quantitative Hydrocarbon Group-Type Analysis of Plastic-Derived Pyrolysis Oils by GCxGC-TOFMS/FID</a></h4><ul><li>Presentation / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/218">MDCW</a></li></ul>Outline<ul><li>Pyrolysis Oils Characterization Workflow</li><li>Plastic-Derived Pyrolysis Oil Samples</li><li>Choosing a GCxGC system</li><li>Benefits of the Pegasus BT 4D MS</li><li>Benefits of the Paradigm Shift System</li><li>Choosing a GCxGC column set…</li><li>Mapping out the GCxGC Space</li><li>Group-Type Analysis of Pyrolysis Oils</li><li>ChromaTOF TILE</li><li>Areas of Interest + PCA</li><li>Comparing Trends of Multiple Features</li><li>Benefits of the Pegasus HRT+ 4D</li><li>Benefits of the Multi-Mode Source (MMS)</li><li>Pegasus HRT+ 4D Data Processing Workflows</li><li>High-Resolution, Accurate Mass Data</li><li>Mass Defect: Nitrogen-Containing Species</li><li>Mass Defect: Sulfur-Containing Species</li><li>Leveraging High Resolution Mass Accuracy</li><li>Conclusion</li></ul>

News from LabRulezGCMS Library - Week 39, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 30th September 2024? 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 to you applications by Agilent Technologies, Waters Corporation, and Thermo Fisher Scientific, and a poster from <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/296">ASMS</a> by Shimadzu!<h4>1. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/TP_093_Analysis_of_PFAS_in_Water_Final_05292024_8fa9fcb27d.pdf">Analysis of Volatile PFAS in Water Using Head-Space Solid Phase Microextraction- Gas Chromatography/Mass Spectrometry (HS-SPME GC/MS)</a></h4><ul><li>Poster / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/296">ASMS</a>&nbsp;</li></ul>Introduction&nbsp;Per- and Polyfluoroalkyl Substances (PFAS) are environmental pollutants with recognized health and environmental concerns due to their probable toxicity, persistence, and ubiquitousness throughout the environment, and consumer and industrial products. PFAS encompass a large family of chemicals with varying physicochemical properties. These properties not only affect their toxicity and environmental fate, but also complicates chemical analysis.In this work, a Head-Space Solid Phase Microextraction-Gas Chromatography/Mass Spectrometry (HS-SPME GCMS) analytical method was developed to analyze six classes of volatile PFAS in water. This HS-SPME method presents the advantage of simplifying sample extraction and handling for the analysis of volatile PFAS in water, hence, minimizing operational costs, potential errors, and risk of sample-cross contamination.ConclusionThis study demonstrated the use of a Shimadzu GC/MS-QP2020 NX single quadrupole instrument configured with the AOC-6000 Plus multifunctional autosampler and an automated head space solid phase microextraction unit for measurement of volatile PFAS compounds in water. Linear calibration curves were obtained for all compounds (R 2 ≥ 0.993 and RF %RSD &lt; 20 %). The HS-SPME GC/MS-QP2020 NX method demonstrated qualitative and quantitative capability of analyzing PFAS compounds.<h4>2. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003028_gc_ms_isq_epa_vocs_an003028_na_en_7646797ef5.pdf">Analysis of volatile organic compounds in drinking water according to U.S. EPA Method 524.4</a></h4><ul><li>Application</li></ul>GoalDemonstration of an analytical method that meets the requirements outlined in U.S. EPA Method 524.4 for the quantitation of volatile organic compounds (VOCs) in drinking water, using the Teledyne LABS Tekmar Lumin Purge and Trap (P&amp;T) concentrator paired with the AQUATek LVA autosampler system along with a Thermo Scientific™ ISQ™ 7610 MS system coupled with a Thermo Scientific™ TRACE™ 1610 gas chromatograph (GC) and Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS). Target analyte linearity, method detection limit (MDL), minimum report level (MRL), and mid-point precision and accuracy were assessed to evaluate method performance.Keywords: EPA, U.S. EPA 524.4, VOCs, phthalates, trace analysis, gas chromatography, single quadrupole mass spectrometry, selected ion monitoring, sensitivity, GRO, THM, volatiles, environmental lab, environmental sample analysis, analytical testing laboratories, ISQ 7610 MS, TRACE 1610 GC, GC-MS.IntroductionVolatile organic compounds (VOCs) are man-made contaminants in various products that pose environmental and public health risks. These compounds are regulated in drinking water, and laboratories follow regulations including U.S. EPA Method 524.2.1 A previous application note described U.S. EPA Method 524.2,2,3 which is the most common method for VOC water testing in the USA. U.S. EPA Method 524.4 is an updated method that allows for nitrogen to be used as the purge gas, thus reducing helium consumption, and is now being more widely used. Targeting 75 VOCs, this method differs by offering more method parameter flexibility but stricter quality control, including the stringent calculation of the minimum reporting level for evaluating calibration checks.Implementing U.S. EPA Method 524.4 can present multiple challenges for laboratories. Striking a balance between optimized method conditions and meeting the acceptance criteria, like detection limit requirements for various compound concentrations, is pivotal. Another major hurdle is managing the water matrix to minimize GC-MS system water introduction, which could lead to detrimental effects and delay sample reporting, thereby increasing public safety risks. Ultimately, maintaining consistency in test results to avoid sample reanalysis is crucial. Another factor for laboratories to consider is the fluctuating cost of helium, which is the analytical gas of choice for this analysis. Reducing the use of helium—a limited resource—will enable the laboratory to reduce operational costs and increase profitability.The following evaluation describes the use of the ISQ 7610 GC-MS system coupled with a TRACE 1610 GC with the Thermo Scientific™ HeSaver-H2Safer™ split/splitless injector and Teledyne LABS Tekmar Lumin P&amp;T concentrator paired with the AQUATek LVA autosampler for U.S. EPA Method 524.4.ConclusionThe combined solution of the TRACE 1610 GC coupled with the ISQ 7610 system and the Tekmar Lumin P&amp;T concentrator with the AQUATek LVA autosampler system successfully addresses the challenges of VOC analysis and provides a robust, sensitive solution needed for ensuring maximized sample throughput and regulatory method compliance for U.S. EPA Method 524.4.<ul><li>Excellent linearity for all compounds was demonstrated with the linear regression (r²≥0.995) of the calibration response factors passing all method requirements.</li><li>MDL and precision for seven 0.5 ppb standards showed no interference from excessive water and produced very reproducible results.</li><li>The precision for n=30 samples over 245 injections displayed &lt;30% RSD for all compounds as the method requires and an average recovery of 91%.</li><li>Utilizing HeSaver-H2Safer technology reduced helium consumption for the method by 4 times, which provides a significant cost savings.</li></ul><h4>3. Waters Corporation: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008298_en_db4158391c.pdf">Extractables Analysis of Nasal Spray Devices Using Gas Chromatography and High- Resolution Mass Spectrometry With Soft Ionization</a></h4><ul><li>Application</li></ul>AbstractDue to concern about the safety of components from plastic, it is crucial to screen for and identify potential extractables and leachables (E&amp;L) in pharmaceutical packaging and medical devices. For volatile, and semi-volatile compounds, gas chromatography-mass spectrometry (GC-MS) with electron ionization (EI) is typically used. Compounds are determined using scientific libraries; however, where compounds are not listed or where the sensitivity of EI-MS is not sufficient, the identification process becomes challenging.Here, we describe an E&amp;L screening experiment using gas chromatography and a quadrupole time of flight high-resolution mass spectrometer (QToF-HRMS) with atmospheric pressure gas chromatography (APGC) for soft ionization. A data independent acquisition (DIA) strategy is utilized to aid screening and elucidation which are combined in a screening software solution.Benefits<ul><li>GC-QToF MS with APGC as an orthogonal technique to LC-QToF-MS allows for comprehensive compound coverage with increased sensitivity compared to typical EI techniques</li><li>The UNIFI™ application within the waters_connect™ platform provides customized workflows to simplify screening and structural elucidation in complex datasets</li><li>The Xevo™ G3 QTof Mass Spectrometer enables confident identification of E&amp;L components in complex matrices through novel ion optics and detection system which maximize transmission</li><li>Soft ionization using the APGC™ source allows for the detection of molecular ions from which elemental compositions can be derived to aid compound identification and confirmation&nbsp;</li><li>MSE, a data independent acquisition, increases confidence in identifications when screening against a library and provides additional information to aid structural elucidation</li></ul>Conclusion&nbsp;When undertaking E&amp;L screening analyses it is important to use a range of analytical techniques to account for different compound chemistries. GC-QToF MS with APGC as an orthogonal technique to LC-QToF-MS allowed for comprehensive compound coverage with increased sensitivity compared to typical EI techniques. Due to the soft ionization of APGC, the intact molecular ion is often present in the spectra. This combined with a data independent acquisition, MSE mode, utilizes full spectral acquisition of the accurate mass information of both precursor and fragment ions.This approach boosts confidence in component identifications when screening against an MS/MS library, while minimizing false positives. For instance, in the LC-QToF-MS there were just under 40 potential compounds matches in sample E48 after considering factors such as retention time match, mass accuracy below 3 ppm, and the presence of at least one fragment ion. A further 38 compound matches in sample E48 were tentatively identified using GC-QToF MS with APGC, with mass accuracy below 3 ppm, and the presence of at least one fragment ion.MSE data also aids in the structural elucidation of unknown substances by utilizing accurate mass and corresponding fragment ions, facilitating comprehensive characterization. This data increases confidence in identifications of components and assists with structural elucidation of unknowns to ultimately aid full characterization. For example an unknown with protonated m/z 284.2703 was tentatively identified as a N-(2-(1-piperazinyl)ethyl)decanamide (mass error 2.33 ppm) by the software.For the extractables analysis of nasal sprays the UNIFI application within the waters_connect platform provided SST benchmarking, screening against a library, summary plots to identify trends, filtering of AET levels, binary compare mode to isolate relevant unknowns, and a Discovery Tool for elucidation of unknowns.<h4>4. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_voc_rubber_gasket_extracts_gc_msd_5994_7777en_agilent_6a0a6bf7d0.pdf">Analysis of Volatile Compounds Identified in Rubber Gasket Extracts Using GC/MSD and High-Resolution GC/Q-TOF</a></h4><ul><li>Application</li></ul>AbstractChemicals that are part of polymeric container closure systems (CCS) and drug delivery systems have the potential to migrate into drug products during manufacturing, storage, transport, and delivery, and must be identified in the final products to ensure their safety.This application note presents a rubber gasket extractables study using a unit mass resolution gas chromatography/mass selective detector (GC/MSD) and a high-resolution gas chromatography/quadrupole time-of-flight (GC/Q-TOF) mass spectrometer to establish a process for identifying GC-amenable extractables and leachable (E&amp;L) compounds.IntroductionElastomeric gaskets, plungers, and O-rings are common sources of leachable compounds in the manufacturing, storage, and delivery of drug products. E&amp;Ls derived from elastomeric components may impact the stability and efficacy of small and large molecule drug products1, and therefore need to be characterized thoroughly. Exposure to some E&amp;L chemicals, such as phthalates and nitrosamines, even at low levels, may cause safety concerns.2 Chemicals derived from the elastomer manufacturing process typically include accelerators, activators, antioxidants, fillers, plasticizers (including phthalates), mold release agents, and other additives3 that may leach into the final product. Some additives present in elastomer packaging materials may also contain polycyclic aromatic hydrocarbons (PAHs)4 and aliphatic hydrocarbons.GC/MS is a commonly used technique for analyzing volatile and semivolatile organic compounds in the E&amp;L space. This study demonstrates the capabilities of GC/MSD to identify GC-amenable compounds present in a solvent extract of a rubber gasket by leveraging chromatographic deconvolution in combination with retention index (RI)-based filtering. Adding a high-resolution accurate mass GC/Q-TOF into the E&amp;L workflow provided a higher number of identified chemicals. It also increased confidence in compound identification and enabled structure elucidation of unknown compounds.The study was performed in the Network Workstation configuration using Agilent OpenLab Electronic Content Management (ECM) XT as the data repository. This configuration enabled tools that facilitate compliance with various national and EU electronic record regulations, including audit trails, user authentication, role-based permission controls, and remote data storage.5ConclusionThe GC/MSD is an effective and accessible tool for the analysis of volatile and semivolatile compounds in complex E&amp;L extracts. The established workflow includes deconvolution and an RI-based library search with the data acquisition performed in a compliant environment.The high-resolution Agilent 7250 GC/Q-TOF enabled the identification of additional components with increased confidence, as well as structure elucidation of the unknown compounds.Furthermore, using the novel ultra-low bleed Agilent J&amp;W DB-5Q GC column resulted in a significant decrease in background, which helps in the identification of late-eluting compounds.

News from LabRulezGCMS Library - Week 40, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 7th October 2024? 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 to you applications by Agilent Technologies, Thermo Fisher Scientific, and Shimadzu!<h4>1. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_09_SSK_018_en_98b51ec6ac.pdf">Analysis of Organophosphorus Pesticides in Drinking Water using SPME-GCMS</a></h4><ul><li>Application</li></ul>User Benefits<ul><li>The inspection items of Organophosphorus pesticides (Diazinon, Parathion, Phenitrothion, Phenthoate, and EPN) in water quality can be analyzed simultaneously.</li><li>The automation of fiber conditioning, pretreatment, and sample injection of SPME is possible using AOC-6000 Plus</li></ul>IntroductionOrganophosphorus pesticides (OPs) are a class of insecticides based on organophosphorus compounds. It is widely used to control insects on crops in the pesticide market. OPs disrupt the nervous system by ingestion and contact. These are a toxic substance that cause headaches, dizziness, nausea and convulsions. Because of the side effects of these OPs, in Korea, residual standards are also operated in the water quality environment field. In the past, solvent extraction was used as a pretreatment method for water quality testing, but this required excessive solvent use and complex extraction processes. Therefore, the simpler Solid Phase Micro Extraction (SPME)-Gas Chromatography-Mass Spectrometry (ES 05501.5) method has been revised and published by the National Institute of Environmental Research (NIER) [1].This application news describes the suitability of OPs analysis using SPME automatic injection (AOC-6000 Plus) and GCMS-QP2020 NX for Diazinon, Parathion, Phenitrothion based on the Environmental Standards for drinking water pollution, and Phenthoate, EPN based on the Official test standards for environmental pollution.ConclusionThis application news is to analyze five types of OPs according to the Standard for Quality Test of Drinking Water. The suitability of the analysis was confirmed using Shimadzu AOC-6000 Plus and GCMS-QP2020 NX.All components showed good linearity with the R2 value of 0.998 or higher in the concentration (0.1-10) μg/mL range. MDL, LOQ, accuracy, and precision were excellent at (0.03 to 0.06) ng/mL, (0.10 to 0.20) ng/mL, (87.6 to 108.2), and (2.2 to 4.9), respectively, and were found to satisfy the method criteria.Based on these results, it was confirmed that the use of AOC-6000 Plus and GCMS-QP2020 NX can automate fiber conditioning, pre-treatment and GC injection, making it more convenient to analyze and obtain excellent analysis results.<h4>2. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_semivolatile_organic_compounds_analysis_5994_7686en_agilent_5c1d579274.pdf">Novel Column Chemistry Raises the Bar on Sensitivity and Data Accuracy in the Analysis of Semivolatile Organic Compounds</a></h4><ul><li>Application</li></ul>AbstractAs ionization sources continue to advance, lowering limits of detection and increasing confidence in analyte identification, column technologies can also be used in conjunction to push the practical limits of sensitivity and data accuracy. Increases in the detection of analyte response also result in unwanted increases in the detection of background noise. Gas chromatography/mass spectrometry (GC/MS) column technology that lowers interfering column bleed ions and elevated bleed baselines, maintains peak shape for active compounds, and can withstand aggressive thermal cycling can greatly enhance the performance and productivity of GC/MS methods. This application note examines how column attributes like bleed, inertness, and thermal stability can further benefit the sensitivity and accuracy of an MS. This study illustrates achievable data parameters, like sensitivity limits at trace levels, retention time consistencies, and data accuracy for active semivolatile organic compounds (SVOCs), when the Agilent 7010D triple quadrupole GC/MS (GC/TQ) system is used.IntroductionGovernmental regulatory authorities have established method and performance criteria for GC/MS measurement of SVOCs that are identified as pollutants in environmental and industrial matrices. The United States Environmental Protection Agency (U.S. EPA) method 8270, for example, contains a list of over 200 compounds, some of which can be susceptible to unwanted chemical activity in the instrument flow path, resulting in data quality degradation. If the performance criteria of method 8270 are not met, system maintenance is often needed, such as liner replacement followed by column trimming or replacement, resulting in unplanned instrument downtime.Monitoring of the DFTPP tuning standard, which contains 4,4'-DDT, pentachlorophenol, and benzidine, validates the suitability of the flow path and monitors when maintenance should be performed. The breakdown of 4,4'-DDT to 4,4'-DDE, and 4,4'-DDD, as well as the tailing factors of benzidine and pentachlorophenol, tests the flow path inertness, indicating the activity of susceptible acidic and basic analytes. GC columns contribute the largest surface area in the sample flow path and, therefore, are a critical factor in controlling interferences in the analytical path. Agilent Ultra Inert (UI) GC liners, along with an inert GC column phase, can improve the robustness of SVOCs analyses.1Stationary phases used in GC/MS analysis of SVOCs are typically comprised of liquid polymers with a polysiloxane backbone. When heat is applied to the column during routine use, the terminal end of the stationary phase polymer can bend back and attack itself; this is called "backbiting." Ring structures, which are thermodynamically stable, are liberated from the stationary phase, increasing background noise and raising the baseline; this can be problematic for low signal-to-noise (S/N) analytes. Peak integration can become less repeatable, lowering quantitation accuracy. In addition, the increase in freed ring structures—which fragment in the ion source—and analytes can cause spectral interference in extracted mass spectra and decrease the qualitative score of a library spectral hit. The Agilent J&amp;W HP-5Q and DB-5Q GC columns have an increased thermal stability at upper temperature limits, allowing for less spectral interference, lower levels of column bleed, and better data quality, especially for heavier analytes that may suffer from issues with lower S/N.2The new Agilent high-efficiency ion source (HES) 2.0, as seen in Figures 1 and 2, is equipped with a novel dipolar RF lens that redirects carrier gas and low mass ions by &gt; 95%. The deflected ions land on adjacent lenses and are pumped out before entering the mass analyzer, providing reduced noise and extended instrument robustness while maintaining sensitivity. A ramped RF amplitude versus mass is implemented to avoid spectrum tilt. The reduction of noise allows for a further increase of sensitivity to attogram-level detection limits. Built-in intelligence features such as SWARM autotune and early maintenance feedback further enhance instrument performance and diagnostic capabilities. The DB-5Q GC column and the HES 2.0 work in concert to increase the robustness of difficult analyses such as that of SVOCs.3,4ConclusionThis application note demonstrates that the Agilent J&amp;W DB-5Q GC column can exceed the performance requirements of EPA method 8270. Agilent Ultra Inert chemistry across the sample flow path will maintain peak symmetry of problematic analytes, leading to improved limits of detection and accurate integration. Ultralow-bleed chemistry stabilizes baselines and reduces interfering bleed ions. High-temperature stability allows for the repeated temperature cycling needed for high throughput methods, even when analyzing heavy, complex soil matrices. The matching selectivity of the J&amp;W DB-5Q compared to the Agilent J&amp;W DB-5ms UI allows for seamless adoption, including compatibility with existing retention time locking libraries. The analytical performance of the DB-5Q coupled with the upgraded Agilent HES 2.0 allows for optimal sensitivity, as well as the ability to perform targeted and nontargeted analyses in tandem.<h4>3. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Sl001922_Reduction_of_helium_usage_for_the_analysis_of_pesticide_residues_in_botanical_dietary_supplements_using_GC_MS_MS_with_the_He_Saver_H2_Safer_dd76c52679/Sl001922-Reduction-of-helium-usage-for-the-analysis-of-pesticide-residues-in-botanical-dietary-supplements-using-GC-MS-MS-with-the-HeSaver-H2Safer.pdf">Reduction of helium usage for the analysis of pesticide residues in botanical dietary supplements using GC-MS/MS with the HeSaver-H2 Safer technology</a></h4><ul><li>Application</li></ul>IntroductionConsumer interest in botanicals has grown considerably over the past few years as they are considered to contribute to overall health and wellbeing. Supplements are the most popular botanical products sold over the counter in pharmacies, groceries and online stores, therefore, manufacturers must ensure that the raw materials are safe for consumption. Pesticides are chemicals used for crop protection against a variety of pests such as weeds, fungi, rodents, and insects. Because of their extensive use, pesticides can be found in the air, soil, water, and ultimately in the food chain. Despite their use being highly regulated, misuse of pesticides can lead to unwanted contamination of food or other plant-based consumer products, and have possible impacts on both human and environmental health.When analyzing pesticides, GC-MS/MS is employed to detect trace levels. Helium is the most common carrier gas used for gas chromatography thanks to its high chromatographic efficiency and inertness. Recent price rises in helium and supply issues caused by shortages have led GC manufacturers, researchers, and analysts to investigate possible mitigation options that entail either switching to alternative carrier gases or reducing the helium consumption. The Thermo Scientific™ HeSaver-H2Safer™ carrier gas saving technology 1 offers an innovative and smart approach to dramatically reduce carrier gas consumption, especially during GC operation. It consists of a modified SSL body connected to two gas lines: whereas an inexpensive gas (e.g., nitrogen or argon) is used for inlet pressurization, analyte vaporization and transfer to the analytical column, the selected carrier gas (e.g., helium or hydrogen) is used only to supply the chromatographic column for the separation process, with a limited maximum flow rate. When used with helium as carrier gas, the limited consumption helps to mitigate shortage issues while maintaining GC-MS performance without the need for instrument method re-optimization otherwise required in case of migration to a different carrier gas.In this analysis a Thermo Scientific™ TRACE ™ 1610 gas chromatograph equipped with two Thermo Scientific™ iConnect™ split/splitless injectors, one operating as a standard SSL and the other one upgraded to work in HeSaver-H2Safer mode using argon as pressurizing gas, was coupled to the Thermo Scientific™ TSQ™ 9610 triple quadrupole mass spectrometer and used to run a direct comparison to demonstrate consistency in the analytical results. Details regarding the standards, reagents and the sample preparation used in this study are reported in a previous application note.SummaryThe HeSaver-H2Safer technology offers the advantage of nearly 4 times reduced helium gas consumption, without compromising GC-MS performance for the analysis of residual pesticides in botanical supplements, through a smooth and simple upgrade of a standard iConnect SSL injector module.<ul><li>The transition from the injection phase using an inexpensive pressurizing gas to the separation process using the best carrier gas is extremely fast (within a few milliseconds), ensuring a rapid gas replacement into the column and, thus, analogous performance compared to the use of a standard SSL injector.</li><li>Existing validated methods can be used unchanged with consistent analytical performance in terms of injection repeatability, analyte transfer, linearity, recovery and robustness.</li><li>Moreover, the HeSaver-H2Safer technology provides additional advantages, such as discharging the pressurizing gas only through the split line for the majority of the time, protecting the column from possible contaminants.</li><li>The Helium Gas Saver Calculator allows for easy and immediate estimation of helium cylinder lifetime and cost savings when using the helium-saver technology.</li></ul>

News from LabRulezGCMS Library - Week 41, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 14th October 2024? 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 to you applications by Agilent Technologies, Thermo Fisher Scientific, and posters by Shimadzu and LECO!<h4>1. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/aoac_2024_9_m031_d1063f34df.pdf">Interlaboratory comparison study of two gas chromatography injection techniques viz. liquid and dynamic headspace for trace level quantification of Ethylene Oxide (EtO) and 2-Chloroethanol (2-CE) in ginger powder sample by using tandem mass spectrometry</a></h4><ul><li>Poster / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/292">AOAC</a></li></ul>PurposeEtO is one of the most widely produced chemicals worldwide. It is colorless, odorless, flammable gaseous cyclic ether with boiling point of 10.4°C. It has a very strong antibacterial property. Due to its small size, it shows a high diffusivity and strong penetrating properties and is thus very effective in the disinfestation / disinfection of food commodities. EtO is highly carcinogenic, mutagenic and genotoxic impurity for living being. The US National Institute of Health (NIH) classified EtO as “known to be a human carcinogen based on sufficient evidence of carcinogenicity from studies in humans, including epidemiological studies and studies on mechanisms of carcinogenesis.” Considering carcinogenicity and no acceptable threshold for exposure, no Acceptable Daily Intake (ADI) was established for EtO.2-CE, which is one of the prominent metabolite of EtO is also considered to be genotoxic and potentially carcinogenic. Given the inconclusive toxicological picture of 2-CE, it was decided by regulatory authorities to follow the precaution approach and consider 2-CE equally toxic to EtO. Hence it is very important to quantitate EtO and 2-CE in food matrices at trace levels. EU-MRLs (Maximum Residue Levels as per European Commission) for EtO and 2-CE are summarized in Table 1.Various methods have been presented in EURL-SRM-Analytical Observation Report for the analysis of EtO and 2-CE. The choice of the analytical approach depends on both the analytes and the matrix to be analyzed. So, it is important to have a detailed comparison study of different analytical approaches to ensure robustness, reliability and accuracy of the method for the quantification of EtO and 2-CE.This study covers the comparison between liquid injection technique and dynamic headspace injection technique using different extraction processes for ensuring highest extraction efficiencies. Incurred sample is used for this study.Conclusion<ul><li>In comparison between liquid and HS-Dynamic mode, it is evident that HS Dynamic has advantage in method optimization for accurate recoveries. Liquid extraction needs multiple trials to ensure complete extraction of analytes, majorly depending on matrix. Similarly, temperature and extraction time also plays a critical role</li><li>Quantification of EtO and 2-CE impurities in ginger powder sample was successfully performed by using Shimadzu GCMS-TQ8050 NX with AOC-20i/s and HS-20 NX dynamic headspace samplers</li><li>HS Dynamic requires less sample preparation, demonstrates high recovery due to closed system, high accuracy and easy method optimization</li></ul><h4>2. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_phosphine_cereals_spices_8697_headspace_8890_7010c_5994_7859en_agilent_c8f2d8fe74.pdf">Estimation of Hydrogen Phosphide (Phosphine) Residues in Cereals and Spices Using the Agilent 8697 Headspace Sampler and GC/MS/MS</a></h4><ul><li>Application</li></ul><h5>Abstract</h5>This application note demonstrates the use of an Agilent 8890 GC system coupled with the Agilent 8697 headspace sampler and Agilent 7010 GC/TQ to detect and quantify hydrogen phosphide (phosphine) residues in rice and red chili powder. The sample was inserted into a headspace vial and Milli-Q water was added. The vial was crimped and loaded into the headspace sampler, followed by GC/MS/MS analysis. The limit of quantification of 5 ng/g was achieved in rice and red chili powder matrices. Average recoveries ranged from 80 to 110% in various recovery experiments.<h5>Introduction</h5>Fumigants are gases used for controlling pests in stored food products.1 Cereals are mainly disinfected by hydrogen phosphide (commonly known as phosphine) and liberated from stable salts such as zinc phosphide or aluminum phosphide.1 Phosphine is a colorless gas that is used as a fumigant worldwide because of its rapid diffusion and extreme volatility.1 Despite these desirable properties, trace amounts of phosphine may persist in foods several months after treatment and can cause severe health problems.1Due to its high volatility, phosphine is not amenable to club with common multiresidue methods for pesticide residue analysis in food. Thus, special single-residue methods must be applied.2 Previously, methods for the analysis of phosphine have been developed that highlight the use of the Tenax-filled inlet liner along with cryogenic cooling to preconcentrate the phosphine prior to chromatographic separation. These methods require heavy analytical configurations that include a liquid nitrogen handling system. In EU legislation, maximum residue limits for phosphine in foodstuffs range from 0.01 to 0.1 mg/kg, depending on the commodity (Commission Regulation (EC) No. 149/2008).2The method adopted in this application note demonstrates the use of the 8697 headspace sampler for sample introduction to the 8890 GC system coupled with the 7010 GC/TQ.&nbsp;Column configurationTo prevent single, loose particles of the PLOT column stationary phase from entering the ion source of the mass-sensitive detector (MSD), a restriction capillary (1 m × 0.15 mm) was inserted between the PLOT column and the MSD using a purged Ultimate union. This configuration also helps in column replacement without venting the mass spectrometer.<h5>Conclusion</h5>An accurate and rugged method was developed which meets the requirements of the European Union reference laboratory (EURL) for maximum residue limits of phosphine in foodstuffs. This ranges from 0.01 to 0.1 mg/kg, depending on the commodity (Commission Regulation (EC) No 149/2008) for the analysis of phosphine in rice and red chili powder. The LOQ of the method was demonstrated at 5 ng/g for all tested matrices. Repeatable results were found for four successive replicates of matrix-based standards at 20 ng/g concentration levels. Excellent recoveries were obtained in all tested matrices at 10 ng/g spiked concentration levels. Thus, this study demonstrates the usefulness of the developed method for routine analysis of food samples for phosphine analysis at trace levels.<h4>3. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003105_gc_ms_tsq_9610_dioxins_furan_feed_an003105_na_en_26c691ad68.pdf">Trace analysis of polychlorinated dibenzo-p-dioxins/ dibenzofurans using GC-MS/MS in accordance with EU Regulations 2017/644 and 2017/771 for food and feed</a></h4><ul><li>Application</li></ul>GoalTo demonstrate the suitability of the Thermo Scientific™ TSQ™ 9610 triple quadrupole GC-MS/MS system with Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS) software for the routine and regulatory compliance testing of polychlorinated dibenzo-p-dioxins and polychlorinated dibenzo-p-furans (PCDD/Fs) in food and feed samples in accordance with Commission Regulations (EU) 2017/644 and 2017/771.IntroductionPolychlorinated dibenzo-p-dioxins/dibenzofurans (PCDD/F), or dioxins as they are commonly referred to, are classified as persistent organic pollutants (POPs) under the Stockholm Convention. Due to their chemical stability and high fat solubility, these chemicals can accumulate within food chains and pose exposure/health risks to humans through consumption of food items (i.e., diary, meat, and fish). Regulations are in place to monitor food and feed for the presence of dioxins to protect the population.1 Current maximum levels allowable for PCDD/Fs in food and feedstuffs are at the pg·g-1 concentration range due to the toxicity risk they pose.2,3 However, the European Commission has announced plans to lower the current maximum levels in certain feedstuffs in 2024 based an updated risk assessment.4 As of 2014, a change of EU regulations permitted the use of gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) for the analysis of food and feed as an alternative to GC–high-resolution mass spectrometry (GC-HRMS).5,6 With the proposed lowering of some maximum levels, performance of current instrumentation to achieve these targeted limits must be assessed.Achieving these targeted limits places further stress on laboratories in maintaining consistent sensitivity to detect the trace levels of dioxins in difficult food matrices. Another challenge for analysts is the time-consuming data assessment based on regulatory requirements for PCDD/F analysis. Often the necessary tools for PCDD/F quantification (i.e., isotopic dilution quantification) and reporting of regulatory requirements (ion ratio, calibration, and response factor deviation)7,8 do not exist within a single software. This requires analysts to export to external packages (i.e., Microsoft™ Excel™ ) to perform critical calculations leading to transcription errors and added time for reporting. In addition, laboratories must ensure they produce consistent data throughout the analytical run to avoid reanalysis or re-extraction when sample/extract material is limited.In this analysis, the performance of the TSQ 9610 triple quadrupole GC-MS/MS system equipped with the Thermo Scientific™ NeverVent™ advanced electron ionization (AEI) source was used to demonstrate compliance for regulatory limits for PCDD/F in food and feed samples in accordance with EU Regulations. Food and feed samples were provided by the European Union Reference Laboratory for halogenated Persistent Organic Pollutants in feed and food (EURL POPs) (Germany) and Wageningen Food Safety Research, in their capacity as National Reference Laboratory for POPs (NRL POPs, The Netherlands). These samples contained known trace levels of dioxins previously confirmed at the respective institutes or in international proficiency tests. The aim of this analysis was to ensure results were consistent with the previously determined concentrations in food and feed matrices and meet current compliance with the EU regulations.ConclusionThe results of these comprehensive experiments demonstrate that the TSQ 9610GC-MS/MS system, configured with the NeverVent AEI source and controlled using Chromeleon CDS software together with the Dioxin Analyzer eWorkflow, can deliver reliable regulatory-compliant performance for the quantification and confirmation of PCDD/Fs food and feedstuffs:<ul><li>Femtogram level sensitivity performance for ultra trace level determination of PCDD/F within food and feed samples.</li><li>Check standard performance was within quantitation and ion ratio thresholds for regulatory method compliance at femtogram levels.</li><li>Accurate and precise quantitation at maximum levels and action thresholds for PCDD/F in food and feed.</li><li>Chromeleon CDS software, version 7.3, provides an integrated platform, with the ability to automatically setup, easily acquire, process and report compliant data in a fully regulated environment, eliminating the need for using external spreadsheet programs.</li><li>Chromeleon eWorkflows, available from Thermo Fisher Scientific also provide error-free execution of each analysis to meet standard operating procedure (SOP) requirements, further simplifying the user experience.</li></ul><h4>4. LECO: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Basil_Comparison_GC_G_Cx_GC_TOFMS_LHF_MDCW_24_LPSS_315_Joe_Binkley_4223f2122d/Basil_Comparison_GC_GCxGC_TOFMS_LHF_MDCW24_LPSS-315-Joe-Binkley.pdf">Characterization and Comparison of Basil Before and After Drying Using GC, GCxGC, and TOFMS</a></h4><ul><li>Poster</li></ul>INTRODUCTIONGC and MS are well-established techniques for the characterization of food, beverage, and flavor samples. Extending the analytical separation to two dimensions with comprehensive two-dimensional gas chromatography (GCxGC) enhances the peak capacity, allows for exploring more complex samples, and allows for determining more individual analytes within complex samples. TOFMS adds to these benefits and often leads to the identification for these isolated analytes, supporting non-target analyses where analytes of interest and importance can be determined through data evaluation. When coupled together, the benefits are often greater than the sum of the individual techniques.Software tools that compare sets of GCxGC samples facilitate these analyses and can effectively reveal useful information from the rich data. In this work, we evaluate the aroma characteristics for basil before and after drying. This type of characterization can be useful for quality control, product development, and batch comparisons, as well as understanding the sensory profile changes associated with curing.CONCLUSIONSIn this work, LECO’s TGM800 was used to determine the moisture level of fresh and cured basil samples and LECO’s Pegasus BT4D GCxGC-TOFMS with ChromaTOF Tile were used to highlight differences between the chemicals which contribute to the sensory profiles of fresh and cured basil. This provided a better understanding of the aroma characteristics of these samples. Many differences were observed between the samples and the analytical tools used in this work were crucial for their determination.

News from LabRulezGCMS Library - Week 42, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 21st October 2024? 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 applications by Agilent Technologies, Thermo Fisher Scientific, and Shimadzu and a presentation by <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/131">James Little - Mass Spec Interpretation Services</a>!<h4>1. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_04_ad_0308_en_e9ef3dfd0c.pdf">Ethylene Oxide and 2-Chloroethanol in Various Rice Samples by Dynamic Headspace and GC- MS/MS</a></h4><ul><li>Application</li></ul>User Benefits<ul><li>Simple sample preparation procedure, direct sample analysis</li><li>Sample recovery within 70 % to 130 % without matrix-matched calibration curves</li></ul>IntroductionEthylene oxide (EO) is sometimes used as a fumigant on food products to control pests and insects during storage and transportation. However, residue of EO might remain in the products, raising concerns about the potential health risks associated with it. Therefore, it is essential to monitor and analyze ethylene oxide levels in food product to ensure compliance with safety regulations and protect consumer health. In this study, both ethylene oxide (EO) and 2-chloroethanol (2-CE) in rice were analyzed. 2-CE, a potential byproduct of EO fumigation, is also a compound of interest due to its toxicity and potential health implications. By utilising dynamic headspace and GC-MS/MS, precise and sensitive detection of both EO and 2-CE residues in rice samples can be achieved. The limit of quantitation is 5 ng/g with area %RSD (n=5) for EO and 2-CE at 5.6 % and 4.9 %, respectively. The spike recovery study at concentrations of 10 ng/g, 25 ng/g and 100 ng/g yielded recoveries within 70 %-130 %. This comprehensive analytical approach enables accurate quantification and identification of these compounds, significantly contributing to the overall safety and quality assurance of the food supply chain.ConclusionAn internal standard method was successfully developed for the analysis of EO and 2-CE in rice using HS-20 NX Trap with GCMS-TQ8050 NX. The dynamic headspace technique and GC-MS/MS were employed, simplifying the sample preparation process and maximizing the sensitivity. Good linearity (R2 value &gt; 0.997) and recovery within 70 % to 130 % were achieved for all the samples analyzed in this experiment, even without the use of matrix-matched calibration curves.<h4>2. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/cs_003090_gc_ms_orbitrap_exploris_exposomics_cs003090_na_en_974ecd6971.pdf">Supporting exposomics research with the Orbitrap Exploris GC 240 mass spectrometer</a></h4><ul><li>Application</li></ul>What is exposomics?The exposome, which is defined as the cumulative effect of environmental exposures and corresponding biological responses, helps to provide a comprehensive measure for evaluating non-genetic causes of disease. Exposomics is the study of the exposome that seeks to understand and quantify the totality of a human's lifetime exposure to various environmental factors, including chemical, physical, and biological agents. In essence, it involves assessing and analyzing the complex interactions between environmental exposures and an individual's genetic makeup, lifestyle, and other factors to understand their impact on human health and disease. By examining the cumulative effects of multiple exposures over time, exposomics provides valuable insights into the underlying mechanisms of disease development and can inform strategies for prevention and intervention.1SummaryThe ability to measure the complexity of the exposome has been limited by the available analytical technology to detect complex exposures patterns at varying concentrations. By using untargeted approaches with high-resolution mass spectrometry, it is possible to detect and identify ongoing exposures that may have not been expected or characterized.<ul><li>High-resolution, full scan mass spectrometry using Orbitrap technology provides a solution for:</li><li>Detection and quantification of compounds using an untargeted full scan acquisition that is both highly selective and sensitive.</li><li>Identification and elucidation of the chemical composition of unknown compounds.</li><li>Retrospective analysis of samples long after data acquisition.</li></ul>The combined capability of both the Orbitrap Exploris GC 240 mass spectrometer and Compound Discoverer software with spectral libraries is an excellent tool to support exposomics research.<h4>3. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_pesticides_botanicals_captiva_5994_7361en_agilent_53a42de795.pdf">Comparison of Sample Preparation Methods for Pesticide Analysis in Botanical Dietary Supplement Materials</a></h4><ul><li>Application</li></ul>AbstractThis application note presents a novel streamlined sample preparation method for liquid chromatography/triple quadrupole mass spectrometry (LC/MS/MS) and gas chromatography/triple quadrupole mass spectrometry (GC/MS/MS) multiresidue pesticide (over 440) analysis. This treamlined sample preparation enables analysis in botanical dietary supplement (BDS) materials using the EMR mixed‑mode passthrough cleanup with Agilent Captiva EMR with Carbon S cartridges. Various BDS samples are extracted by traditional QuEChERS extraction, followed by appropriate Captiva EMR cartridge cleanup. The selected Captiva EMR cartridges, based on the BDS sample matrix complexity and pigment intensity, include Captiva EMR–GPD for green tea and peppermint tea, Captiva EMR–LPD for barberry root, and Captiva EMR–GPD + EMR–GPF for curcumin complex. The developed method provides a simple and unified sample preparation workflow for both LC/MS/MS and GC/MS/MS pesticide detection. This method demonstrates acceptable performance, i.e., recovery of 70 to 120% and RSDs &lt; 20%, in representative BDS samples for over 82% of the total 447 pesticides analyzed. Compared to the traditional approach that requires multiple sample preparation methods, the newly developed method demonstrates a more one‑size‑fits‑most approach for efficient cleanup. This approach increases the instrument uptime and reduces both consumables and labor resources. The direct comparison of new method versus old method on actual samples analysis demonstrates acceptable equivalence on reporting results.ConclusionA simple, rapid, and reliable method using Agilent Bond Elut QuEChERS extraction followed by EMR mixed‑mode passthrough cleanup using Agilent Captiva EMR with Carbon S cartridges was developed. The results of this method were verified for over 440 pesticides in botanical dietary supplement extracts and products by LC/MS/MS and GC/MS/MS. The EMR mixed‑mode passthrough cleanup method provided a convenient and simplified cleanup method after sample extraction for selective and efficient matrix removal in BDS matrices and acceptable quantitation recovery and reproducibility in large panel pesticide quantitation. The detailed proficiency test confirmed the acceptable method performance for practical sample analysis.The ability to streamline sample preparation into a single method allows for a reduction in the total amount of sample preparation consumables and reduces the preparation time. The reduced organic solvent, especially the toxic solvent used per sample, made the entire procedure greener while being more people and environmentally friendly. Also, having one sample to be prepped in a single day allows for much greater traceability regarding shared analytes between LC and GC analyses. This single sample preparation also helps simplify the results and documentation. Consolidating sample preparation documentation into a single packet, as opposed to two packets, minimizes time spent by reviewing staff.<h4>4. <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/companies/131">James Little - Mass Spec Interpretation Services</a>: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/quant_handout_98c5b2fea8.pdf">KnowItAll Quantitative Software for EI GC-MS</a></h4><ul><li>Application</li></ul>Table of content:<ul><li>Files Used for Demonstration</li><li>More Information on Files from North Dakota Website</li><li>Final Result Page from Demonstration</li><li>Quantitation Workflow</li><li>Wiley KnowItAll Training Resources</li></ul>&nbsp;

News from LabRulezGCMS Library - Week 43, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 28th October 2024? 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 applications by Agilent Technologies, Thermo Fisher Scientific, and Shimadzu!<h4>1. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_00_00095_en_c6eed5e008.pdf">Analysis of Major Psychoactive Compounds in Nutmeg Using GC-MS/MS</a></h4><ul><li>Application</li></ul>AbstractNutmeg is a spice used in a variety of recipes that can be easily purchased by anyone. Among younger people, however, excessive consumption of nutmeg powder for recreational purposes is increasing, causing hallucinogenic effects. However, there are few reports on toxic or comatose-fatal blood levels and their changes over time in cases of nutmeg poisoning. Therefore, an analytical method using GC-MS/MS was devised and applied to a case of nutmeg poisoning in order to determine the blood concentrations of the main psychoactive substances (safrole, myristicin, and elemicin) in nutmeg and their change over time. The limit of detection (LOD) and limit of quantification (LOQ) of the constructed method were 0.14 to 0.16 ng/mL and 0.5 ng/mL (the lowest point of the calibration curve), respectively. Calibration curves showed good linearity, with R2 = 0.996 to 0.997 for all substances in the range of 0.5 to 300 ng/mL. The accuracy for QC (low 1 ng/mL, medium 120 ng/mL, and high 240 ng/mL) and LOQ (0.5 ng/mL) was %RSD 2.4 to 11 % for diurnal variation (n = 5) and %RSD 1.5 to 11 % for diurnal variation (6 days). A systematic error of -2.6 to 2.1 % was obtained.IntroductionNutmeg, the dried seed of Myristica fragrans, has been used as a spice and for medicinal purposes all over the world since ancient times and is widely sold at low prices. Because nutmeg contains safrole, myristicin, and elemicin (Fig. 1) as the major psychoactive compounds, they are sometimes intentionally consumed in large amounts to induce hallucinations or intoxication8)-10). In addition, intoxication by unintentional misuse of nutmeg has recently become a problem. In addition to hallucinogenic effects, too much nutmeg is associated with clinical symptoms such as nausea, vomiting, abdominal pain, agitation, drowsiness, dizziness, tachycardia, blurred vision, dry mouth, and flushing5), 9), 11)-14). However, the majority of nutmeg overdose cases are mild and unlikely to be fatal14), 15). Symptoms of nutmeg poisoning usually begin 2 to 8 hours after ingestion11), 15), 16) and subside within a few days3), 5), 9), 11), 13), 15)-17). Only two deaths worldwide have been linked to the consumption of nutmeg15), 18).In a recent study, biological samples were collected from volunteers who ingested nutmeg powder to identify metabolites of major psychoactive substances19)-23). However, although many cases of nutmeg poisoning have been reported to date, there have been no reports evaluating the blood levels and half-lives of major psychoactive substances, such as safrole, myristicin, and elemicin, during poisoning. Therefore, we developed an analytical method for three psychoactive substances using GC-MS/MS, measured the blood levels of these main substances in patients with nutmeg poisoning, and evaluated their changes over time.ConclusionUsing a MonoSpin® extraction kit in combination with a GC–MS/MS system, a simple method was devised to detect and quantify safrole, myristicin, and elemicin in human serum. This method was validated and applied successfully to a case of nutmeg poisoning. For this patient, the method quantified the time-course changes and half-life of safrole, myristicin, and elemicin in serum. It is believed that this method will help to provide additional blood-concentration data for nutmeg poisoning cases as well as more accurate toxicokinetic parameters.<h4>2. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_fatty_acid_methyl_ester_analysis_8890_gc_fid_luma_5994_7849en_agilent_677241bc1b.pdf">Analysis of 37 Fatty Acid Methyl Esters on the Agilent 8890 GC Using FID and LUMA Detectors</a></h4><ul><li>Application</li></ul>IntroductionThe analysis of fatty acid methyl esters (FAMEs) is used to characterize lipids in foods, including oils, meats, seeds, and other products. The fatty acid composition of fats is a complex mixture of saturated, monounsaturated, and polyunsaturated compounds with various carbon chain lengths.1 Because the roles of fatty acids in the body vary depending on their structure, it is necessary to conduct detailed compositional analyses of the fatty acids contained in foods. The analysis of fatty acid composition in food is standard in many governmental, quality control (QC), and contract research laboratories worldwide.The nutrition labels on food products include much of this information, detailing food composition to help consumers make informed choices.3 Gas chromatography-flame ionization detection (GC-FID) is a commonly used method for analyzing the fatty acid composition in foods. In this application brief, an analysis of a neat 37-component FAME mix standard was conducted using an Agilent 8890 GC system equipped with an FID and LUMA vacuum ultraviolet (VUV) detector. For comparison, several branded oils were also purchased and analyzed.ConclusionThese results show the advantages of using the LUMA detector coupled with an Agilent 8890 GC system and FID for FAMEs testing. By combining the robustness of the FID and the UV spectral power of the LUMA, users can be confident in their results.<h4>3. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003254_gc_helium_hydrocarbon_oil_index_water_soil_an003254_na_en_4b0ceb0e48.pdf">Dual injection for Hydrocarbon Oil Index (HOI) determination in water and soil with helium carrier gas conservation</a></h4><ul><li>Application</li></ul>GoalThe aim of this application note is to demonstrate the performance of a high-throughput and cost-effective method for the determination of the Hydrocarbon Oil Index (HOI) also known as Total Petroleum Hydrocarbon (TPH), in water and soil samples by using a dual injection configuration and conserving helium gas.IntroductionPetroleum products are complex mixtures of hundreds of hydrocarbon compounds, ranging from light, volatile, short-chained organic compounds to heavy, long-chained, branched compounds. Petroleum hydrocarbons can enter the environment through industrial accidents, spills, or leaks, and as by-products from commercial or private uses. Contamination of water and soil is a growing concern as lighter TPH fractions float in water and form thin surface films, whereas the heavier fractions accumulate in the sediment at the bottom of the water, affecting bottom-feeding fish and organisms. TPH released in soil can evaporate into the air, dissolve into the groundwater, and move away from the spillage area, contaminating the drinking water supplies, or remain bound to the soil particles for a long period, thus reducing the usability of land for development.To protect public health from toxic effects due to TPH exposure, many European countries and the United States have made the determination of the content of mineral oils and petroleum products in water and soils a compulsory requirement for quality certifications. Because there are so many petroleum products, it is not practical to measure each one individually, therefore the total amount of all hydrocarbons found in a sample of soil, water, or air is usually monitored.1The United States Environmental Protection Agency (U.S. EPA), the International Organization for Standardization (ISO), as well as the Italian Institute of Environmental Protection and Research (ISPRA) have published several methods (U.S. EPA 8015 D,2 ISO 16703:2011,3 ISO 14039:2004,4 ISO 9377:20005, ISPRA Doc. N. 46/14,6 ISPRA Doc. n. 04/117) that can be considered when analyzing TPH in water and soil using gas chromatography coupled to flame ionization detection.The Hydrocarbon Oil Index (HOI) represents the total amount of compounds that can be extracted from the sample (potable water, surface water, and wastewater) with a non-polar solvent. The extracted compounds must not absorb on Florisil™ and must elute between n-decane (C10) and n-tetracontane (C40) when analyzed by GC on a non-polar column. Such fraction includes heating oils, diesel fuels, kerosene, lubricants, and transmission fluids.In this work, the Thermo Scientific™ AI/AS 1610 autosampler in the Gemini configuration for simultaneous dual injections combined with the Thermo Scientific™ HeSaver-H2 Safer™ carrier gas saving technology was employed to increase the sample throughput and double the productivity while reducing helium consumption and cost per analysis. Method compliance in terms of sensitivity, recovery (C40/C20 ratio), linearity and precision were evaluated for quantitative assessment of the HOI in water and soil samples.Conclusions<ul><li>The Hydrocarbon Oil Index analysis in water and soil is a routine test for environmental laboratories. Robust solutions offering time- and cost-saving opportunities are key to maintain laboratory efficiency and face increasing workloads.</li><li>The TRACE 1610 GC with a dual channel SSL-FID and the AS 1610 autosampler in the Gemini high-throughput configuration can double the number of samples through simultaneous injections, while Chromeleon CDS allows easy management of instrument control, data processing, and reporting for both channels.</li><li>The system performance exceeds the regulatory requirements in terms of recovery, repeatability, linearity, and limit of quantitation, well below the minimum acceptable hydrocarbon contamination.</li><li>The system robustness helps minimize maintenance for extended instrument uptime with consistent results over longer sequences.</li><li>The innovative HeSaver-H2 Safer technology used on both channels provides a significant reduction of the helium gas consumption, also during sample analysis, extending 4.5-fold the cylinder lifetime and providing a significant cost savings to the laboratory.</li></ul>

News from LabRulezGCMS Library - Week 44, 2024

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