<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 22nd July 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p>
<blockquote>
<h4>👉 <a href="https://gcms.labrulez.com/library"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></a></h4>
</blockquote>
<blockquote>
<p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p>
</blockquote>
<p>This week we bring to you poster presentations from <a href="https://gcms.labrulez.com/events/568"><strong>ASMS 2024</strong></a> by <strong>LECO</strong>, <strong>Agilent Technologies</strong>, and <strong>Thermo Fisher Scientific</strong>! And as a bonus two application notes from <strong>Shimadzu</strong> and <strong>Thermo Fisher Scientific</strong>.</p>
<blockquote>
<p>💡 <strong>+ 100 ASMS posters and presentations <a href="https://gcms.labrulez.com/library?mainauthorItems=284">available in the LabRulezGCMS library</a></strong> (unique search and filtering)</p>
</blockquote>
<h4><strong>1. LECO: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Long_Lifetime_Ion_Detector_GC_G_Cx_GC_TOFMS_MS_ASMS_24_LPSS_326_4c9e1fb7a1.pdf">A Novel Long-Lifetime Ion Detector for GC-TOFMS and GCxGC-TOFMS with Sub-Femtogram Detection Limits</a></strong></h4>
<ul>
<li>poster - ASMS 2024</li>
</ul>
<p><strong>Introduction:</strong> Ion detection efficiency and fast response times are critical aspects of the ion detectors used in time-of-flight mass spectrometry (TOFMS). With modern advancements in ionization, ion optics, and ion transfer efficiency, TOFMS systems are capable of generating high ion flux onto the ion detectors. Having an ion detector that is capable of maintaining optimal performance over a long period of time while accepting high amounts of ion flux is a significant challenge in development of TOFMS instrumentation. Improvements in detector life will minimize maintenance costs and improve TOFMS user experience. A novel long-lifetime ion detector was developed in partnership with El Mul Technologies for use in LECO’s Pegasus® BTX GC and GCxGCTOFMS. The system was thoroughly evaluated for sensitivity and robustness, including longevity of the detector.</p>
<p><strong>Conclusions:</strong> The Pegasus BTX GC(GCxGC)-TOFMS with a novel Long-Lifetime Ion Detector has demonstrated the following performance characteristics:</p>
<ul>
<li>Sub-2 fg IDL for GC-TOFMS and Sub-fg IDL for GCxGC-TOFMS </li>
<li>Linear dynamic range of 5 orders of magnitude in GC-TOFMS and 4 orders of magnitude in GCxGC-TOFMS</li>
<li>Robust operation: the detector bias remains consistent and BTX peak intensity remains consistent over long periods of time, even with large numbers of samples acquired and significant amounts of charge accumulation on the detector.</li>
</ul>
<h4><strong>2. Thermo Fisher Scientific: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/po_142_utilizing_hydrogen_pesticides_food_gc_ms_po142_asms2024_en_7ed0951b93.pdf">Utilizing hydrogen carrier gas for sensitive analysis of pesticides in food using gas chromatography mass spectrometry</a></strong></h4>
<ul>
<li>poster - ASMS 2024</li>
</ul>
<h5><strong>Abstract</strong></h5>
<p><strong>Purpose:</strong> To demonstrate the performance of the Thermo Scientifc HeSaverH2Safer kit for iConnect split-splitless (SSL) injection module for trace analysis of pesticides using H2 as a carrier gas as a safe and sustainable solution for laboratory operations.</p>
<p><strong>Methods:</strong> In this study, hydrogen was used as a carrier gas for GC-MS/MS analysis of trace levels of pesticides in food. The GC was fitted with a new hydrogen safer split/splitless injector, with chromatographic separation performed on a TG-5 SIL MS(30 m × 0.25 mm, 0.25 μm) capillary GC column. The chromatographic conditions applied ensured critical pair separation was achieved. The GC-MS/MS system was equipped.</p>
<h5><strong>Conclusions</strong></h5>
<ul>
<li>The use of the HeSaver-H2Safer technology allows for a safe and compliant use of hydrogen as an alternative carrier gas in GC/GC-MS applications without the need to install a hydrogen sensor and removes any risk of unwanted reactions with the sample in the hot SSL injector.</li>
<li>When used with hydrogen, the limited carrier gas consumption offered by the HeSaverH2Safer mode permits a very controlled system demand for hydrogen, making this solution ideal for laboratories working with hydrogen generators.</li>
<li>Migrating the GC-MS/MS method from helium to hydrogen requires an adaptation of method parameters to address (i.e., retention time shift and different fragmentation patterns).</li>
<li>97% of pesticides in baby food and 98% in honey showed a linear response in the concentration range 0.005–0.500 mg/kg and the relative standard deviation for N=5 repeats of each sample type at 0.01 mg/kg was equal or lower than 10% for 98% of the evaluated compounds with an advanced electron ionization (AEI) source to increase sensitivity for analyte detection. Quantification and assessment of critical regulatory requirements, such as linearity and sensitivity, were performed in a single software.</li>
</ul>
<h4><strong>3. Agilent Technologies: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/po_142_utilizing_hydrogen_pesticides_food_gc_ms_po142_asms2024_en_7ed0951b93.pdf">Analyzing Nitrosamines with Hydrogen Carrier Gas: GC/MS/MS Analysis of Nitrosamines in Sartan Drugs</a></strong></h4>
<ul>
<li>Poster Reprint - ASMS 2024</li>
</ul>
<p><strong>Introduction:</strong> The limited availability of helium has been a concern, leading to a growing interest in switching to alternative carrier gases like hydrogen. Hydrogen offers several advantages over helium1 , including faster run times and improved chromatographic resolution. Helium is commonly used as a carrier gas for analyzing nitrosamine impurities in pharmaceuticals. However, there are concerns that nitrosamines may react with hydrogen, forming unwanted byproducts. To ensure that using hydrogen as a carrier gas does not impact spectral quality, we evaluated its suitability for analyzing eight impurities:</p>
<ul>
<li>N-nitrosodimethylamine (NDMA),</li>
<li>N-nitrosomethylethylamine (NMEA),</li>
<li>N-nitrosodiethylamine (NDEA),</li>
<li>N-nitroso-ethylisopropylamine (NEIPA),</li>
<li>N-nitrosodiisopropylamine (NDIPA),</li>
<li>N-Nitrosodipropylamine (NDPA),</li>
<li>N-nitrosodi-n-butylamine (NDBA),</li>
<li>N-Nitrosopiperidine (NPIP).</li>
</ul>
<p>Hydrogen carrier gas was used with the 7000E and 7010 Series GC/TQ systems equipped with the HydroInert and HES ion sources respectively, assessing spectral quality, linearity, repeatability, recovery, and compliance with nitrosamine analysis regulations.</p>
<p>MassHunter 13 software suite provided the tools for data acquisition and processing to be performed under a unified compliance environment. OpenLab Electronic Content Management (ECM) XT includes native tools to facilitate compliance, including the ability to create users with affiliated permissions, the generation of audit trails, and remote data storage.</p>
<p><strong>Conclusions:</strong></p>
<ul>
<li>The 7000E and 7010 Series GC/TQ systems equipped with the HydroInert and HES, respectively, exhibited exceptional performance in determining eight nitrosamine drug impurities in sartan drug products and substances using hydrogen carrier gas.</li>
<li>The method was validated at 30 ppb with acceptable recovery and long-term repeatability. </li>
<li>The 7010 Series GC/TQ system enabled a smooth switch between helium and hydrogen carrier gas without compromising the performance of the methods. </li>
<li>Both the HydroInert and the HES sources facilitated achieving the necessary detection limits for the tested impurities.</li>
</ul>
<h4><strong>4. Agilent Technologies: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/po_142_utilizing_hydrogen_pesticides_food_gc_ms_po142_asms2024_en_7ed0951b93.pdf">Analysis of Essential Oils Using a Comprehensive GCxGC with a Reverse Flow Modulator Combined with High Resolution GC/MS</a></strong></h4>
<ul>
<li>Poster Reprint - ASMS 2024</li>
</ul>
<p><strong>Introduction:</strong> Essential oils are typically analyzed to determine their chemical composition contributing to flavor and quality as well as to evaluate their authenticity and identify adulterants. Essential oils are often complex samples with high number of volatile and semi-volatile components that include many isomers with highly similar spectra and close Retention Indices (RIs) when separated on a single column. Hence, a comprehensive GCxGC approach is preferable to achieve an appropriate chromatographic separation for this sample matrix. In this study we used comprehensive GCxGC coupled to a high-resolution accurate mass GC/MS to identify the essential oil  components. Here we also investigate approaches for comparison of the complex GCxGC essential oil data.</p>
<p><strong>Conclusions:</strong></p>
<ul>
<li>Several comprehensive GCxGC configurations and method using the high-resolution GC/Q-TOF and RFM were developed and optimized using a diesel sample. </li>
<li>Essential oils were analyzed using the optimized GCxGC approach, and the workflows for compound identification and statistical analysis were evaluated.</li>
</ul>
<h4><strong>5. Shimadzu: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/an_01_00746_en_e14cf49b7b.pdf">Greenhouse Gas Analyzer</a></strong></h4>
<ul>
<li>Application</li>
</ul>
<p><strong>User Benefits:</strong></p>
<ul>
<li>Simultaneously measures the 3 main greenhouse gases: CH₄, CO₂, and N₂O.</li>
<li>Offers short analysis cycle times and is equipped with an AOC-6000 Plus syringe injection system to analyze large numbers of samples.</li>
<li>Uses nitrogen as a carrier gas for lower running costs.</li>
</ul>
<p><strong>Introduction:</strong> Greenhouse gases are a major cause of climate change, and carbon dioxide, (CO₂), methane (CH₄), and nitrous oxide (N₂O) are considered the 3 primary greenhouse gases. Although CO₂ accounts for the majority of greenhouse gas emissions followed by CH₄, reducing CH₄ emissions is considered important because CH₄ has a warming effect that is more than twenty times greater than CO₂. At the United Nations Climate Change Conference (COP26) in November 2021, over 100 countries joined the Global Methane Pledge, which pledges by 2030 to reduce global CH₄ emissions by 30 % compared to 2020 levels. The Greenhouse Gas Analyzer is a gas chromatography system that has been developed by Shimadzu in collaboration with the National Agriculture and Food Research Organization (NARO) (Fig. 1). Measuring levels of CH₄, CO₂, and N₂O simultaneously in a single sample is difficult, but the Greenhouse Gas Analyzer has been designed to do this simultaneously, which reduces analytical errors and improves the sampling speed, giving researchers a valuable tool in reducing greenhouse gas emissions.</p>
<p>This Application News describes using the Greenhouse Gas Analyzer to simultaneously measure CO₂, CH₄, and N₂O levels.</p>
<p><strong>Conclusion:</strong> The Greenhouse Gas Analyzer can simultaneously measure 3 greenhouse gases in atmospheric air in a single analysis. Each analysis by the Greenhouse Gas Analyzer is performed in 8 minutes with an analysis cycle time of 10 minutes.</p>
<h4><strong>6. Thermo Fisher Scientific: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/an_002695_gc_triplus_rsh_smart_sample_prep_environ_an002695_na_en_77a5aa2300.pdf">An automated approach for the analysis of VOCs in drinking and surface water by using the TriPlus RSH SMART VOC Sample Prep Station</a></strong></h4>
<ul>
<li>Application - Environmental</li>
</ul>
<p><strong>Goal:</strong> The aim of this study is to demonstrate the suitability of the Thermo Scientific™ TriPlus™ RSH SMART VOC Sample Prep Station for the analysis of volatile organic compounds (VOCs) in drinking and surface water by using a fully automated sample preparation workflow.</p>
<p><strong>Keywords:</strong> Automated sample preparation, TriPlus RSH SMART Sample Prep Station, volatile organic compounds, VOCs, drinking water, surface water, gas chromatography, TRACE 1610 GC, single quadrupole mass spectrometry, ISQ 7610 GC-MS.</p>
<p><strong>Conclusions:</strong> The results of these experiments demonstrate that the automated sample preparation capability of the TriPlus RSH SMART VOC Sample Prep Station coupled to the ISQ 7610 GC-MS system provides an ideal solution for water testing laboratories looking to improve productivity and deliver confident results.</p>
<ul>
<li>Static headspace is a convenient solventless extraction technique for volatiles in water with almost no sample preparation required. </li>
<li>Unattended operations of up to 210 samples can be achieved with the automated calibration dilution and ISTD addition workflows.</li>
<li>The automated addition of fresh reagent just before the incubation increases the stability of ISTD/surrogates mix, therefore improving the accuracy of the quantitation of target analytes during data reprocessing.</li>
<li>The TriPlus RSH SMART VOC Sample Prep Station ensures increased sample integrity for highly reliable quantitative analysis, and reduced errors or possible cross-contaminations, maximizing the productivity of the laboratory. Additionally, it allows saving valuable analyst time and improving safety by limiting the user’s exposure to toxic chemicals. </li>
<li>The integrated control for both autosampler and GC-MS in a single CDS ensures a streamlined automated workflow from on-line sample preparation to sequence setup, data acquisition, and reporting. </li>
<li>Suitability of headspace sampling for analysis of VOCs was demonstrated with R2  &gt; 0.990, RRF %RSD &lt; 20%, and calculated amount within 20% of the spiked concentration. </li>
<li>Inter-day reproducibility was demonstrated by running three batches of samples bracketed with QCs. Average absolute peak area %RSD across the entire evaluation period was &lt;20%, the QC calculated amount was within 20% of the expected value, and the calculated recovery was within 70–130%, with the only exception of 1,2-dibromo-3-chloropropane for which the % recovery was 132. </li>
<li>Reliable quantitative analysis was achieved for drinking water samples and surface water samples analyzed in three different batches across six working days. All the sample results were compliant with the thresholds set by the current EU regulation.</li>
</ul>


News from LabRulezGCMS Library - Week 30, 2024

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 13th October 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you poster by <strong>Agilent Technologies / AOAC </strong>and<strong> </strong>application notes by<strong> EST Analytical, Shimadzu </strong>and <strong>Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies / AOAC: Analysis of Pesticides in Spices with Hydrogen Carrier Gas</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_pesticides_hydrogen_carrier_gas_aoac_2025_w007_en_agilent_280dd876d5.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Spices are considered as one of the most challenging matrices for analysis of pesticides. Usually, the sample analysis involves 5-10 fold dilution to reduce the matrix load. Thus, lower instrument detection limits need to be achieved. Use of hydrogen as carrier gas can further pose changes in terms of sensitivity. This work describes the suitability of the hydroinert and HES ion source to achieve the required sensitivity. Samples were extracted using QuEChERS based approach followed by dispersive cleanup. Linearity was evaluated against matrix matched standards within the range of 0.5-50 ng/mL. Correlation coefficient (r2) for calibration ranging between 0.5 -50 ng/mL was found above 0.95. Precision study was carried out by injecting 6 replicates of pre-spiked samples at 10 ng/g. The average relative standard deviation (%RSD) was &lt;20% with recoveries ranging from 72-125%. The advantages of the method include utilization of same retention time MRMs and collision energies. This allowed for easy transition from helium to hydrogen carrier gas.</p><h4><strong>Experimental</strong></h4><p>An Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC"><strong>8890 GC</strong></a> coupled to a 7000 (with HydroInert source) / <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7010+Triple+Quadrupole+GC%2FMS"><strong>7010 Triple Quadrupole GC/MS</strong></a> system equipped with High Efficiency Source (HES) was used. The GC system was equipped with a MultiMode Inlet (MMI) with air cooling and a back flushing system based on a Purged Ultimate Union controlled by a PSD module.</p><h4><strong>Results and Discussion&nbsp;</strong></h4><p>The oven temperature program used with H2 as the carrier gas was maintained identical to that used with He. The analytical method originally optimized for a 20- minute runtime using He was successfully adapted for H2. This ensured preservation of chromatographic resolution and retention time fidelity across carrier gas substitution, as evident from the elution order shown in Figure 3. The chromatograms indicate presence of high matrix load at initial 7 mins for all the spices. At RT 10-13 min, matrix load of and chilli was high. The matrix load from black pepper was very high throughout the runtime. Backflush of 7 min was used to remove the matrix.&nbsp;</p><p>Transitioning from He to H2 can often lead to reactions at the ion source resulting in spectral changes when compared with He. Therefore, EI sources with reduced or eliminated source reactivity such as HydroInert and HES is essential to minimize or prevent the undesirable insource reactions when using hydrogen. The tested mixture of pesticides were compared against the NIST library to ensure spectral fidelity. As evident form Figure 5, the library match percentages were acceptable and this the existing MRM database could be used for acquisition in MRM mode, without the requirement of any additional MRM development.</p><h4><strong>Conclusions</strong></h4><p>Agilent GC/TQ systems with HydroInert and HES sources delivered consistent sensitivity and spectral fidelity using hydrogen carrier gas, without re-optimizing MRM transitions or collision energies. Retention times and elution order were preserved across complex spice matrices. The systems achieved LOQs of 2.5 to 5 ppb after five-fold dilution, even in heavily loaded matrices like black pepper, confirming reliable quantitation in high-background spice samples.</p><h3><strong>2. EST Analytical: A Single Calibration Method for Water AND Soil Samples Performing EPA Method 8260</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_A_Single_Calibration_Method_for_Water_AND_Soil_Samples_Performing_EPA_Method_8260_27f8b93aad.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In order to run Method 8260 samples, a bromofluorobenzene (BFB) tune standard, matrix blank, calibration standard, and laboratory control standard all have to be run and pass method requirements every twelve hours. With the exception of the BFB standard, the other standards and blank matrices have to correspond to the samples to be analyzed. Due to this constraint, the analyst is required to run another three samples if the matrix is changed within the twelve hour time window. Moreover, the calibration must also match the sample matrix. These requirements are very time consuming and can limit laboratory profits. This application note will demonstrate a patented automated water sampling mode using the soil sampling station of the autosampler thus eliminating the need to have separate calibrations and standards for waters and soils.</p><h4><strong>Experimental</strong></h4><p>The sampling system used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159"><strong>EST Analytical Centurion WS autosampler</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160"><strong>Evolution concentrator</strong></a>. The concentrator was affixed with a Vocarb 3000 trap and connected to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7890A"><strong>Agilent 7890A GC</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?search=5975"><strong>5975 inert XL MS</strong></a>. The GC was configured with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=9&amp;search=Rxi-624+Sil+MS"><strong>Restek Rxi-624 Sil MS </strong></a>30m x 0.25mm x 1.4µm column. The experiments were run using the extraction mode of the Centurion WS. Refer to Table 1 for the sampling method parameters and Table 2 for GC/MS parameters.</p><h4><strong>Conclusion</strong></h4><p>The patented sampling process of the Centurion WS proved to be a reliable and accurate sampling method for running water samples in the soil mode. The curve linearity and method detection limits both met USEPA Method 8260 requirements, and the precision and accuracy results were excellent. The water extraction option offered with the Centurion WS will save laboratories time and money because only one set of standards, curves, etc. is required for both water and soil samples.</p><h3><strong>3. Shimadzu: Measurement of Volatile Organic Compounds in Water by Headspace GC-MS with Nitrogen Carrier Gas</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00907_en_077ab0a675.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Due to the health issues associated with volatile organic compounds (VOCs), standards and regulations are established for VOC levels in water. VOCs are preferably measured by methods that involve simple sample pretreatment, and headspace GC-MS is one of these methods commonly used to measure VOC levels. GC-MS is normally performed with helium carrier gas, but helium gas could require more cost and lead time to obtain for analytical use every year. There is a need for a GC-MS analysis method that can be performed using relatively inexpensive and readily available nitrogen carrier gas. While nitrogen carrier gas results in inferior analytical sensitivity compared with helium carrier gas, trap mode sampling can salvage the reduction of the sensitivity. This Application News presents an example measurement of VOCs in water using nitrogen carrier gas performed on the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050"><strong>GCMS-QP2050</strong></a> gas chromatograph mass spectrometer and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=HS-20+NX"><strong>HS-20 NX headspace sampler</strong></a> in trap mode.</p><h4><strong>Samples and Analysis Conditions&nbsp;</strong></h4><p>Standard solutions were prepared by diluting 25 standard VOC mixture in methanol to 1, 2.5, 5, 10, 25, 50, 100, and 250 mg/L. The standard solutions were combined with internal standards 1,4-dioxane-d8 at 100 mg/L, fluorobenzene at 12.5 mg/L, and pbromofluorobenzene at 12.5 mg/L.</p><ul><li><strong>GC-MS: </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050"><strong>GCMS-QP2050</strong></a></li><li><strong>Head Space Sampler: </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=HS-20+NX"><strong>HS-20 NX</strong></a></li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>VOC levels in water were measured using an HS-20 NX in trap mode and a GCMS-QP2050 with nitrogen carrier gas. Trap mode allowed VOCs to be measured in water with a high degree of sensitivity, even with nitrogen carrier gas.</p><h3><strong>4. Thermo Fisher Scientific: Enhanced trace moisture analysis in organic solvents using GC with multi-channel VUV detection</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003954_gc_luma_detector_trace_1610_industrial_pharma_an003954_na_en_c29f4875a6.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Monitoring water content in organic solvents is essential across various industries, notably in pharmaceutical manufacturing, where excess moisture can compromise active ingredient stability. Traditionally, Karl Fischer titration has been the benchmark technique, offering broad quantification capability. However, KF is limited by side reactions, reagent sensitivity, and incompatibility with high-throughput workflows. It also relies on hazardous solvents and extensive manual steps.&nbsp;</p><p>Gas chromatography provides an alternative means of quantifying water when paired with an appropriate detector. While FID and TCD have been used, they lack the selectivity and sensitivity required for trace moisture detection. Ionization-based detectors like PDD improve detection but suffer from dynamic range limitations.</p><p>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=LUMA%E2%84%A2+VUV+detector"><strong>LUMA™ VUV detector </strong></a>(VUV Analytics, Inc.) overcomes these drawbacks by employing vacuum ultraviolet absorbance in the 118–240 nm range, where water exhibits strong and selective absorption. Unlike other GC detectors, LUMA combines universality, spectral selectivity, and ease of use in a single platform.&nbsp;</p><p>This work illustrates a GC method using a LUMA Multi-Channel VUV Absorbance detector to analyze moisture in acetonitrile from 250 ppb up to percent levels. This approach has several advantages over traditional techniques like Karl Fischer titration, including superior sensitivity for the analysis of trace levels of water in acetonitrile as well as percent levels. The achievable limit of detection for water in acetonitrile is 250 ppb, with method linearity over 0.25–100 ppm producing R² ≥ 0.999.&nbsp;</p><h4><strong>LUMA detector highlights&nbsp;</strong></h4><ul><li><strong>Detection range: </strong>125–1,050 nm VUV-UV-VIS&nbsp;</li><li><strong>Channel configuration:</strong> Up to 12 discrete absorbance bands simultaneously acquired&nbsp;</li><li><strong>Sensitivity: </strong>Low-ppb to percent level in a single method&nbsp;</li><li><strong>Installation: </strong>Compact, uses any carrier gas and no vacuum pumps&nbsp;</li><li><strong>Software integration: </strong>Fully controlled via Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)&nbsp;</li></ul><p>These capabilities enable detection of water and organic solvents in a single injection—dramatically simplifying workflows in quality control laboratories.</p><h4><strong>Experimental&nbsp;</strong></h4><p>The LUMA detector can be easily installed on a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/483"><strong>Thermo Scientific™ TRACE™ 1600 Series GC</strong></a> and controlled in <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Chromeleon CDS</strong></a>, providing method settings, data acquisition, and reporting in a single software platform.</p><p>GC-VUV separation using the LUMA Multi-Channel Vacuum Ultraviolet Absorbance detector was based on a previously described method by VUV Analytics.¹ Method conditions for this experiment are described in Table 1.</p><p>A commercially available 100 ppm KF standard (water in xylene) was used to determine sensitivity, linearity, and repeatability. To minimize the impact of environmental moisture in this experiment, the same solution has been used to simulate different water levels through varying split ratios and injection volumes.&nbsp;</p><p>Seven concentration levels (0.25–100 ppm) were created using adjusted split ratios as summarized in Table 2. Five replicate injections were made at each level.</p><h4><strong>Key application benefits&nbsp;</strong></h4><ul><li>Replaces Karl Fischer titration for routine moisture analysis&nbsp;</li><li>Simultaneous quantification of water and organic solvents&nbsp;</li><li>Ideal for pharmaceutical QA/QC and regulatory environments&nbsp;</li><li>Fast, automated workflows with no vacuum or specialty gases&nbsp;</li></ul><p>This workflow is aligned with recent trends toward hybrid analytical techniques that reduce resource consumption and speed up decision-making in GMP labs.&nbsp;</p><h4><strong>Conclusion</strong></h4><p>The LUMA multi-channel VUV detector offers a transformative approach to moisture analysis in volatile organic solvents. It provides both trace-level sensitivity and wide dynamic range— enabling labs to consolidate workflows, eliminate time-consuming titrations, and enhance data reliability.&nbsp;</p><p>By expanding GC capability to encompass water detection, LUMA bridges a long-standing gap in chromatographic technology, delivering measurable gains in efficiency and analytical scope.&nbsp;</p><ul><li>The detector operates in the 125 nm to 1,050 nm region of the spectrum, where nearly all compounds absorb, making it a universal GC detector.&nbsp;</li><li>The detector associates high sensitivity to high selectivity thanks to the simultaneous acquisition of 12 channels with different spectral range in the VUV spectrum.&nbsp;</li><li>Working with up to 12 channels, the detector allows the determination of multiple analytes in a single injection. For example, water, solvents, and a range of impurities including potential genotoxic impurities (PGIs).&nbsp;</li><li>In addition to having high sensitivity and selectivity, the LUMA detector is easy to use; it is controlled by Chromeleon CDS, fitting well into existing laboratory workflows, and does not require a vacuum pump or separate special carrier gases.</li></ul>

News from LabRulezGCMS Library - Week 42, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 17th November 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you applicaton notes by <strong>Agilent Technologies, EST Analytical </strong>and <strong>Shimadzu!</strong></p><h3><strong>1. Agilent Technologies: Accurate Identification and Quantification of Pesticide Residues in Ghee</strong></h3><p><strong>Analysis by QuEChERS with GC/MS/MS using the Agilent 8890 GC and Agilent 7010 GC/TQ</strong></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_pesticide_ghee_gc_5994_8399en_agilent_1cbd787002.pdf"><strong>Full PDF for download</strong></a></li></ul><p>India is one of the largest producers of milk, contributing about 23% of global milk production.<sup>1</sup> The dairy processing sector includes a wide range of products, such as milk, butter, cheese, ghee, yogurt, flavored milk, lactose-free dairy products, and value-added products like ice creams and yogurts. Amongst these, ghee production is significant because of its popularity, low cost of production, and versatile use. According to the Food Safety and Standards Authority of India (FSSAI), ghee is mentioned as a "product obtained exclusively from milk, cream or butter by a process that almost completely removes water and non-fat solids; it has a specially developed flavor and physical structure".<sup>2</sup> Milk‑producing animals can be exposed to pesticides through their diet, such as feed and fodder containing pesticide residues, or through the direct application of pesticides for controlling ectoparasites on their bodies, in animal sheds, and in milk processing areas. Due to their persistent and lipophilic nature, pesticides tend to accumulate in the fat-rich tissues of animals. The FSSAI has specified maximum residue levels (MRLs) for 55 pesticides, and a tolerance limit of 0.01&nbsp;mg/kg for the remaining pesticides for which an MRL has not been&nbsp;fixed.&nbsp;</p><p>Ghee consists of 98.9% fat, irrespective of the animal source. Among the short- and medium-chain saturated fatty acids, all samples contain butyric (C4:0), caproic (C6:0), caprylic (C8:0), and capric acid (C10:0).<sup>3</sup> Since its introduction, the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=QuEChERS"><strong>QuEChERS method</strong></a> has been widely used for the analysis of pesticides in several matrices. Some modifications to the original QuEChERS method have been introduced to ensure efficient extraction of pH-dependent compounds, to minimize degradation of susceptible compounds (such as base- and acid-labile pesticides), and to expand the spectrum of matrices covered. Ghee matrix has a very high lipid load, making it a difficult commodity for analysis pesticide residues. The primary challenge lies in obtaining an extract that contains the target analytes while minimizing the amount of fat. Co-extracted lipids in the extracts can be removed, to a high degree, by a freezing-out step or a C18 cleanup.&nbsp;</p><p>During sample extraction, the sample is often diluted. To obtain a quantification limit of 0.01 mg/kg, the instrument should be able to detect the residues at a lower concentration. This application note addresses these requirements by combining a sample preparation technique covering multiclass pesticides, target-specific multiple reaction monitoring (MRM) data acquisition, and efficient software to simplify quantitative analysis. The Agilent 7010 triple quadrupole GC/MS system enabled trace-level detection and confident quantitation of 150 pesticides in ghee.</p><h4><strong>Experimental&nbsp;</strong></h4><h5><strong>Equipment&nbsp;</strong></h5><p>An Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC"><strong>8890 GC</strong></a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7010+GC%2FTQ"><strong>7010 GC/TQ</strong></a> system equipped with high efficiency source was used for the analysis. The GC system was equipped with a multimode inlet with air cooling and midcolumn backflush based on an Agilent purged Ultimate union controlled by a pneumatic switching device. The method parameters are displayed in Table 1.</p><h4><strong>Conclusion</strong></h4><p>The limits of quantitation (LOQs) for the target list of over 150 compounds ranged from 2.5 to 5 mg/kg for the ghee matrix. To minimize interferences from the ghee matrix, numerous multiple reaction monitoring (MRM) transitions were employed. This approach helped to accurately identify and quantify the target compounds despite the complex sample matrix. The samples were diluted five-fold to ensure that the analytes were within the required detection range of the instrument. This dilution also helped in reducing the matrix effects, leading to more reliable results. The average analyte recoveries were between 70 and 130%, indicating that the method has good accuracy and precision. This range of recoveries demonstrates the method’s robustness and suitability for routine analysis of these compounds.</p><h3><strong>2. EST Analytical: Analysis of Coffee Flavors by Purge and Trap Sampling</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_Analysis_of_Coffee_Flavors_by_Purge_and_Trap_Sampling_ca25beef60.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Most of us who drink coffee know our preferences. We know which blend we like, what strength and definitely what we like in our coffee. However, most of us do not think about the flavors that go into our coffee that help us define our preferences. Coffee manufacturers, on the other hand are working diligently to create a new blend or a more satisfying flavor that would make us want to choose their coffee over another maker.&nbsp;</p><p>This study will look at four different blends of coffee and some of the compounds that contribute to the flavor of the blend. Using purge and trap sampling, the flavor compounds were purged out of the coffee and trapped onto an adsorbent trap. The analytes were then transferred to a Gas Chromatograph/Mass Spectrometer (GC/MS) for analysis. The study focused on six flavor compounds. The spicy smoky aroma of 2-methylfuran, the spicy caramel, almond odor of 5-methylfurfural, the buttery scent provided by the addition of 2,3-butanedione and 2,3- pentanedione and the impact of the two and three methyl butanals giving the dark chocolate malty flavor to the coffee.</p><h4><strong>Experimental:&nbsp;</strong></h4><p>The EST Analytical <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160"><strong>Encon Evolution Purge and Trap Concentrator</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159"><strong>Centurion WS Autosampler </strong></a>were interfaced to a GC/MS. The Centurion WS was run in the soil mode and the purge and trap concentrator was configured with a Vocarb 3000 (K) analytical trap. The column selected for this study was an Rtx-1 60m x 0.25mm x 1µm. Listed in Tables 1 and 2 are the experimental parameters used for this study.</p><h4><strong>Conclusion:&nbsp;</strong></h4><p>The lightest roast had the most buttery and dark chocolate/malty flavors while the darkest roast had more of the smoky flavor. Surprisingly, the darkest roast and the medium roast had similar proportions of the flavor compounds with the exception of the smoky flavor. While the light roast had large amounts of the flavors tested for, the chromatography of the light roast was much simpler than that of the darker roasts. Overall, the Encon Evolution Purge and Trap Concentrator in conjunction with the Centurion WS Autosampler proved to be an excellent system for sampling coffee. The results were reproducible and provided a lot of information on the flavors of the respective coffees.</p><h3><strong>3. Shimadzu: Analysis of Ethanol in E10 Gasoline Using Polyarc Microreactor for GC</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_01033_en_d4ee66bd4f.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The flame ionization detector (FID) can detect almost all organic compounds, and the sensitivity of the obtained chromatograms displays a correlation with concentration and number of carbon atoms in the compound. However, as a weakness of FID, its sensitivity decreases when an organic compound contains oxygen atoms, asin the case of alcohols.&nbsp;</p><p>The Polyarc microreactor improvessensitivity for alcohols and other compounds containing oxygen atoms (hereinafter, oxygenated compounds), allowing calibration using a single compound. Research and use of biofuels has accelerated in recent years, and more sensitive quantitative analysis of oxygenated compounds in multiple compoundsis now required.&nbsp;</p><p>This Application News introduces an example of an analysis of a sample simulating E10 gasoline, in which 10 % ethanol by volume concentration was added to gasoline, demonstrating that enhanced sensitivity for oxygenated compounds can be achieved by adding Polyarc to the instrument configuration. The accuracy of the quantitative analysis was also verified using a general standard sample (alkane).</p><h4><strong>Polyarc Microreactor</strong></h4><p>Polyarc is a post-column type microreactor that is introduced between the column and the detector (FID). The organic compounds separated and eluted by the column are decomposed to methane by the Polyarc reactor in a two-stage oxidationreduction reaction (Fig. 1). Since the decomposed methane is detected by the FID, the uniform sensitivity for the carbon number can be obtained, regardless of the type of functional groups in a sample.</p><h4><strong>Effective Carbon Number</strong></h4><p>As mentioned above, the sensitivity of the FID detector varies depending on the types of functional groups in organic compounds. The detection sensitivity by the FID can be estimated based on the concept of the effective carbon number (ECN), which is an index showing how many carbon atoms in a compound function effectively. Depending on the type of functional groups contained in a compound, the carbon ratio in the molecule changes, and this causes changesin the sensitivity ofthe FID. For example, both ethane (C2H6) and ethanol (C2H5OH) contain the same number of carbon atoms of 2, but the sensitivity of the FID for ethanol is only 75 % of itssensitivity for ethane because the primary hydroxyl group (-OH) behaves as -0.5 carbon atoms in terms of its contribution to the ECN. This meansthe ECNof ethanol is 1.5. Table 1 shows several examples of other functional groups with ECNslowerthan the number of carbon atoms.</p><h4><strong>Analysis Conditions</strong></h4><p>In this Application News, sensitivity for ethanol when the Polyarc was added and when using only the FID was compared using an E10 sample, in which 10 v/v% ethanol was added to gasoline, simulating a biofuel which has attracted attention in recent years, and quantitativity for ethanol was confirmed. In the quantitative analysis, it was also carried out by the external standard method using a hydrocarbon (dodecane; C12) with a concentration of 1 w/v% as a standard sample. The analytical instrument was a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GC-2030"><strong>GC-2030</strong></a> (SPL/FID) model gas chromatograph with the Polyarc added (Fig. 2). Table 2 shows the analysis conditions.</p><h4><strong>Conclusion</strong></h4><p>E10 gasoline was analyzed using an FID detector and an added Polyarc microreactor, confirming that oxygenated compounds can be analyzed with high sensitivity. This study also confirmed that a uniform reaction of organic compounds can be obtained in the FID, and peak broadening can be suppressed by standardizing the response of sensitivity. Table 6 introduces several of the advantages that are possible by adding the Polyarc microreactor. The Polyarc converts all organic compounds to methane having the same number of carbon atoms (mol), enabling highsensitivity detection for compounds with low detection sensitivity by FID alone. In addition, since sensitivity is standardized, quantitation is possible using only one arbitrary calibration curve, regardless of the type of analysis compound. As a result, it is now possible to analyze compounds that were difficult to analyze by FID until now.</p>

News from LabRulezGCMS Library - Week 47, 2025

<p><strong>A highly sensitive and selective method was developed for quantifying nano- and microplastics (NMPs) in water, sediments, and biological tissues using pyrolysis gas chromatography coupled to triple quadrupole mass spectrometry. Dynamic multiple reaction monitoring and internal standard calibration enabled nanogram-level quantification of 12 common polymers following matrix-specific sample preparation.</strong></p><p>The method addressed matrix interferences through tailored cleanup strategies, signal enhancement with calcium carbonate, and correction of lipid-derived interferences for major polymers. Application to environmental samples from the Gulf of Mexico and the Texas coast demonstrated reliable detection of NMPs across diverse matrices, supporting high-throughput monitoring of plastic pollution.</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.5c05604"><strong>Rapid and Sensitive Quantification of Nano- and Microplastics in Water, Sediment, and Biological Tissue by Pyrolysis-Gas Chromatography Tandem Mass Spectrometry with Dynamic Reaction Monitoring</strong></a></h4><p>M. Bryan Gahn*, Marcus Wharton, Asif Mortuza, David Hala, Christopher D. Marshall, Karl Kaiser*</p><p>Anal. Chem. 2026, 98, 1, 633–641</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acs.analchem.5c05604">https://doi.org/10.1021/acs.analchem.5c05604</a></p><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/"><strong>CC-BY 4.0</strong></a></h6></blockquote><p><strong>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.</strong></p><p>Global plastic production has surged over the past half-century, rising from approximately 1.3 Mt in 1950 to approximately 359 Mt in 2018. <a href="javascript:void(0);">(1)</a> This increase has led to a growing concern regarding plastic pollution, particularly nano and microplastics (NMPs). Microplastics are generally defined as plastic particles with a maximum dimension of ≤ 5 mm, while nanoplastics typically range from 1 to 1000 nm in size. <a href="javascript:void(0);">(2)</a> NMPs encompass a wide variety of polymer particles that originate either from direct manufacture (e.g., microbeads and synthetic textiles) or from environmental degradation processes (e.g., photooxidation and mechanical abrasion) of larger plastic debris (i.e., macroplastics, &gt;5 mm). <a href="javascript:void(0);">(3)</a></p><p>NMPs are ubiquitous in the environment. They have been detected from Antarctic coast sediments to Arctic ice sheets, the summit of Mt. Everest to the depths of the Mariana Trench, and have been found in organisms across all trophic levels, including humans. <a href="javascript:void(0);">(4−10)</a> The pervasive presence of NMPs has raised significant ecological and human health concerns. NMPs can act as vectors for environmental pollutants. Hydrophobic organic contaminants (e.g., PCBs and PAHs) readily adsorb onto their surfaces, and plastics additives such as phthalates and flame retardants can leach into surrounding media (e.g., water, sediment, tissue). <a href="javascript:void(0);">(11)</a> Even without associated harmful chemicals, the physical presence of NMPs can lead to increased production of reactive oxygen species in cells, resulting in an inflammatory response. <a href="javascript:void(0);">(12)</a> Given the widespread NMP pollution and its complex ecological ramifications, there is a critical need for more robust high-throughput quantitative methods to accurately assess NMPs in diverse matrices.</p><p>Numerous analytical techniques have been employed for the detection and quantification of NMPs, which often combine traditional microscopy with advanced spectroscopic and molecular approaches. <a href="javascript:void(0);">(13)</a> These methods yield either estimates of particle counts or mass-based concentrations normalized to sample volume or weight. Prior to analysis, most methods require extensive chemical or enzymatic digestion and subsequent cleanup steps to isolate plastic particles and reduce matrix complexity. <a href="javascript:void(0);">(14,15)</a> Particle count-based methods encompass optical microscopy, laser diffraction particle size analysis, scanning electron microscopy, flow cytometry, and Fourier-transform infrared (FTIR) and Raman spectroscopy. <a href="javascript:void(0);">(16)</a> These methods provide quantitative estimates of particle abundance across the entire size spectrum of NMPs, and some can also differentiate between plastic types.</p><p>Thermal decomposition coupled with gas chromatography–mass spectrometry (GC-MS) is an increasingly utilized technique for the analysis of NMPs. <a href="javascript:void(0);">(17,18)</a> Pyrolysis-based methods thermally decompose plastic polymers in samples under oxygen-free conditions at temperatures exceeding 500 °C generating characteristic volatile fragments. These fragments are then separated by gas chromatography and detected by mass spectrometry with high sensitivity and specificity. As with other analytical techniques, pyrolysis-GC-MS (PyGC-MS) performance can be improved by incorporating sample cleanup steps prior to analysis to remove interfering organic and inorganic constituents. Matrix interference can often lead to misidentification of plastic polymer types and disrupt the pyrolysis process, ultimately compromising analytical accuracy and precision. <a href="javascript:void(0);">(19)</a> For example, lipids in biological tissues can yield similar combustion products to those of polyethylene (PE), polypropylene (PP), and nylon-66 (N-66). <a href="javascript:void(0);">(20)</a></p><p>Improvements that enable more reliable quantification of NMPs at ultralow concentrations by PyGC-MS include optimized sample treatment methodologies that include the addition of reactants to improve pyrolysis efficiency of plastic polymers, and the application of advanced mass spectrometric methods. Quantification of NMPs at trace levels is often constrained by the minimum weight limits of analytical balances, as calibration relies on the mass of particulate standards. This limitation has been addressed by using inert fillers, such as calcium carbonate (CaCO<sub>3</sub>) or clean quartz sand that are mixed with plastic standards to produce weighable calibration standards down to the nanogram level. While single-quadrupole mass detectors are widely used due to their simplicity and low cost, they offer limited sensitivity and are less sensitive in complex matrices. <a href="javascript:void(0);">(21)</a></p><p>The application of time-of-flight and orbitrap mass spectrometry, as well as modern triple-quadrupole mass detectors, promises improved sensitivity and specificity of NMP quantification in complex matrices. These highly selective detectors enable precise mass determination, reducing ambiguity in peak identification and enhancing the ability to differentiate plastics from natural organic matter commonly present in environmental samples. Time of flight and orbitrap mass spectrometers support untargeted screening and identification of emerging or unknown plastic-related compounds, while triple-quadrupole instruments excel in targeted quantification with high throughput and reproducibility, which are advantageous features for routine monitoring. <a href="javascript:void(0);">(22−24)</a> Compared to traditional methods such as FTIR or Raman spectroscopy, modern mass spectrometric approaches are better equipped to address the challenges posed by complex sample matrices, diverse plastic compositions, and trace-level concentrations, making them essential tools for future NMP analysis. <a href="javascript:void(0);">(25,26)</a></p><p>Here we present a novel analytical method for the identification and quantification of NMPs in diverse environmental matrices that include marine waters, sediments, and biological tissues by using pyrolysis gas chromatography coupled with triple quadrupole mass spectrometry (PyGC-qQq-MS). Depending on the sample matrix, NMPs were concentrated through filtration, extraction, or digestion prior to analysis. Gas chromatography with qQq-MS detection using dynamic multiple reaction monitoring (DMRM) mode with an internal standard yielded significantly improved selectivity and sensitivity, enabling accurate and precise quantification of plastic polymers. Method validation demonstrated the robust performance of the method across diverse sample types, with reliable detection of NMPs at amounts of 1–126 ng and in the presence of significant matrix interference.</p><h4><strong>Experimental Section</strong></h4><h5><strong>Pyrolysis GC/MS qQq-MS Analysis</strong></h5><p>Pyrolysis gas chromatography was carried out with a Frontier Auto-Shot AS-2020E sampler and an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=42&amp;search=EGA%2FPY-3030D"><strong>EGA/PY-3030D multishot pyrolyzer</strong></a> connected to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+gc"><strong>Agilent 8890 GC</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7010B"><strong>7010B qQq-MS</strong></a>. Prior to pyrolysis at 600 °C, GF/F with particulates from water samples or digested tissues were spiked with PFS, which served as an internal standard. Filters were then transferred to Frontier Eco Cups and topped with 5 mg of CaCO<sub>3</sub> and quartz wool to ensure proper packing. Redissolved sediment extracts were transferred directly into the Eco Cup LFs, dried under a gentle stream of N<sub>2</sub>, and packed with CaCO<sub>3</sub> and quartz wool.</p><h4><strong>Results and Discussion</strong></h4><h5><strong>Pyrograms</strong></h5><p>The method was optimized to yield characteristic pyrolytic products of plastic polymers that were well resolved on a Frontier Ultra Alloy 5 column with a linear temperature program. Pyrograms of surface water, vertebrate and invertebrate tissue, and sediment samples, alongside a standard plastic mixture are shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.5c05604#fig3">Figure 3</a>. Pyrolysis temperature was optimized to ensure efficient volatilization of polymers, and specific product ions were chosen to minimize matrix influence that can generate pyrolysis products with similar mass spectra. For each polymer, precursor and product ions were selected to minimize interference from natural polymers and characteristic fragmentation reactions. For polymers that primarily undergo depolymerization (e.g., PE, PP, PS, PMMA), the selected precursor ions corresponded to characteristic oligomeric or monomeric pyrolysis products, and the quantifier ions were derived from simple bond cleavages or rearrangement reactions. For example, PS pyrolysis products included mono, di-, and trimeric units with different retention times. Mono- and dimeric fragments had retention times and mass spectra that overlapped with matrix peaks of similar mass ions, whereas the trimeric PS fragment eluted without interference from matrix components.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Anal_Chem_2026_98_1_633_641_Figure_3_Pyrograms_of_A_Calibration_standard_composed_of_homogenized_mixture_containing_12_plastics_of_interest_ee999a5a40.jpg" alt="Anal. Chem. 2026, 98, 1, 633–641: Figure 3. Pyrograms of (A) Calibration standard composed of homogenized mixture containing 12 plastics of interest; (B) Surface water samples collected in Galveston Bay (2019); (C) Mullet muscle tissue collected in Galveston Bay (2021); (D) Oyster tissue collected in Galveston Bay (2021); (E) Benthic sediment collected from Matagorda Bay (2023)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Anal_Chem_2026_98_1_633_641_Figure_3_Pyrograms_of_A_Calibration_standard_composed_of_homogenized_mixture_containing_12_plastics_of_interest_ee999a5a40.jpg 130w," sizes="100vw" width="1500" height="1798"></p><h5><strong>QqQ-MS Detection and Quantification</strong></h5><p>Optimal DMRM parameters for the detection of plastics were established using pure polymer standards (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.analchem.5c05604#tbl1">Table 1</a>). Characteristic and abundant molecular precursor ions were identified for each plastic polymer and evaluated against natural polymers to minimize matrix interference. Fragmentation ions derived from these precursor ions were selected based on characteristic fragmentation reactions. The more abundant product ion was used for quantification, whereas the secondary ion was employed as the qualifier to monitor potential coelution with matrix compounds. Fragment losses usually corresponded to the loss of polymer subunits or dehydration reactions. Operating in DMRM mode improved sensitivity by maximizing acquisition time for each targeted analyte. Ratios of quantifier to qualifier ion (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.analchem.5c05604/suppl_file/ac5c05604_si_001.pdf">Table S2</a>), together with retention times, ensured both compound identification and confirmation.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Anal_Chem_2026_98_1_633_641_Table_1_Plastic_Polymer_Abbreviations_d796d20f8b.jpg" alt="Anal. Chem. 2026, 98, 1, 633–641: Table 1. Plastic Polymer Abbreviations, Relative Retention Times (RRT), Characteristic Ions, and Limit of Detection (LOD)" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Anal_Chem_2026_98_1_633_641_Table_1_Plastic_Polymer_Abbreviations_d796d20f8b.jpg 213w," sizes="100vw" width="1073" height="784"></p><p>Quantification of plastics was based on internal standard calibration using PFS as the internal standard. PFS was dissolved in toluene and added to the sample prior to pyrolysis. The use of deuterated polystyrene as an internal standard was explored; however, extensive hydrogen–deuterium exchange occurred during pyrolysis, leading to pyrolysis products with variable D/H content. <a href="javascript:void(0);">(31)</a> Similarly, attempts to use brominated polystyrene were unsuccessful, as bromine was readily lost from the polymer chain during pyrolysis, resulting in products indistinguishable from those of PS and others.</p><p>Calibration at &lt;1 mg plastic mass was accomplished using plastic standards dispersed in CaCO<sub>3</sub>. The most consistent results were achieved with commercially available standard kits (e.g., Frontiers), which contain homogeneously distributed plastic polymers in CaCO<sub>3</sub>. Attempts to prepare homogeneous mixtures of plastic polymers in CaCO<sub>3</sub> by ball milling finely ground plastics with CaCO<sub>3</sub> yielded less consistent results than commercial standards.</p><h4><strong>Conclusion</strong></h4><p>This study developed and validated a robust analytical workflow for the detection and quantification of NMPs across a diverse range of environmental matrices. The method demonstrated high sample throughput, robust compensation of matrix interference, and high precision and accuracy. This was accomplished through efficient sample cleanup procedures, internal standard calibration, tandem mass spectrometry, and a correction for lipid interference in the detection of PE, PP, and N-66. The applicability of the method was demonstrated on marine surface waters, sediments and soils, and muscle tissue of fishes and oysters. Results revealed quantifiable concentrations of plastics in all sample types emphasizing the pervasive and persistent nature of plastics in the environment and their bioaccumulation potential across trophic levels. This method provides a critical tool for studying NMPs in the environment, ecological risks, and potential impacts on human health.</p>

Rapid and Sensitive Quantification of Nano- and Microplastics in Water, Sediment, and Biological Tissue by Pyrolysis-Gas Chromatography Tandem Mass Spectrometry with Dynamic Reaction Monitoring

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 31st August 2026? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies</strong>, <strong>Shimadzu, Thermo Fisher Scientific </strong>and presentation by<strong> MDCW / Liège University!</strong></p><h3><strong>1. Agilent Technologies: Extend the time window for the detection of low level anabolic‑androgenic steroids and their metabolites</strong></h3><p><strong>Steroid profiling, screening, and confirmatory analysis using the </strong><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=10&amp;search=7010"><strong>Agilent&nbsp;7010 GC/MS mass spectrometer</strong></a></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/5991_9045_EN_Doping_Control_App_Note_1_13dde5f053.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>Doping laboratories want to have lower detection limits to be able to identify and quantitate illegal drugs for a longer time window between doping and urine sample collection. This Application Note describes how the doping control lab in Kreischa, Germany used the Agilent 7010 Triple Quadrupole GC/MS System (TQ) for enhanced targeted detection of anabolic‑androgenic steroids in urine samples. The 7010 TQ enabled higher sensitivity, longer maintenance-free intervals, and more stable operation than earlier models, and satisfied all measurement specifications required by the World Anti‑Doping Agency (WADA). The 7010 TQ GC/MS ion source produces more ions, and provides exceptional sensitivity for the detection of low intensity metabolites weeks after drug ingestion. However, this higher sensitivity may lead to saturation of endogenous components naturally present at higher concentrations. This method provides a sensitive and robust operation over a wide concentration range, permitting the detection of low-concentration exogenous species in the presence of high‑concentration endogenous species, which can vary with ethnicity.</p><h4><strong>Experimental</strong></h4><p>The <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=10&amp;search=7010"><strong>Agilent 7010 GC/TQ system</strong></a> consists of an <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=10&amp;search=7890"><strong>Agilent 7890 GC</strong></a> with multimode inlet and backflush, an<strong> Agilent 7993A</strong>, and the Agilent 7010 TQ mass spectrometer.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>Based on the method optimization and thorough testing at the Kreischa lab, an Agilent 7010 GC/MS-based protocol was developed. This protocol fulfills the screening and confirmation requirements of steroid measurements in doping control labs. With this method, it is possible to detect traces of exogenous anabolic steroid metabolites while quantifying small concentrations of testosterone and epitestosterone typical in Asian populations. It permits the measurement of high‑abundance endogenous steroids such as androsterone and etiocholanolone in the same injection, while analyzing testosterone/epitestosterone and androsterone/etiocholanolone ratios without suppression.&nbsp;</p><p>The backflush capability of the system protects the analytical column, and consequently the mass spectrometer, by removing heavy matrix components. This allowed more than 6,000 samples to be analyzed on the same column without requiring ion source cleaning or filament change. It also demonstrated that the higher, 130&nbsp;eV electron energy did not sacrifice the filament lifetime. It performed reliable measurements of both trace (0.2&nbsp;pg on‑column) and high (10,000&nbsp;pg on‑column) concentration analytes in the same run.&nbsp;</p><p>The method validation revealed that the exceptional sensitivity offered by the 7010 GC/MS can be used to:&nbsp;</p><ul><li>Improve the trace detection ability of the method&nbsp;</li><li>Reduce the amount of sample&nbsp;injected&nbsp;</li><li>Extend maintenance-free intervals</li></ul><h3><strong>2. MDCW / Liège University: The Century Mix: updates and cool projects</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/DG_1_Dimandja_Stefanuto_34c4a66c3d.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>The presentation <strong>“The Century Mix: updates and cool projects”</strong> introduces the Century Mix, a standardized reference mixture developed for comprehensive two-dimensional gas chromatography (GC×GC). The mixture contains <strong>100 compounds representing a broad range of chemical classes</strong>, including alkanes, alcohols, ketones, esters, lactones, phthalates, and aromatic compounds. Stability was a key criterion in compound selection, and the mixture was developed through cross-laboratory collaboration for <strong>column characterization, method assessment, and quality control</strong>. Its structured chromatographic behavior also makes it useful for studying how different compound classes behave in GC×GC separations.</p><p>A major part of the work examined the <strong>factors influencing retention indices (RI) in GC×GC systems</strong>, which are important for reliable compound annotation in non-targeted analysis. An inter-laboratory study involved <strong>11 GC×GC systems</strong> using cryogenic, Peltier, and flow modulation, different detectors, and both normal and reversed column configurations. Principal component analysis showed clear grouping according to normal versus reversed orthogonality, confirming the strong influence of stationary-phase configuration. A subsequent design-of-experiments study evaluated <strong>140 combinations</strong> of temperature ramp rate, carrier-gas flow rate, modulation period, and secondary-oven temperature offset.</p><p>The results showed that the influence of experimental conditions is strongly <strong>compound dependent</strong>. Of the compounds evaluated in the statistical model, 33 showed RI variation that could be linked to the investigated parameters, whereas 43 did not follow the model well. Compounds such as quinoline, phthalates, lactones, terpenes, and some aromatic compounds showed particularly pronounced effects. For quinoline, for example, the model explained about <strong>93% of RI variability</strong>, with differences of approximately 75 RI units across the tested conditions, while 2-hexanone showed considerably weaker dependence. Overall, <strong>temperature ramp rate and flow rate emerged as particularly important parameters</strong>, although the magnitude of their effect depended on compound chemistry and column configuration.</p><p>The Century Mix is therefore being developed not only as a characterization mixture but also as a tool for <strong>system quality control and more reliable retention-index prediction</strong>. Repeated standardized QC measurements demonstrated very low RI variability and can be used to monitor system stability, experimental effects, and potential instrument drift. The broader goal is to better understand the fundamental chemistry governing GC×GC retention and ultimately improve method development, data processing, and identification of unknown compounds by combining high-quality separations, mass spectra, and predicted retention information.</p><h3><strong>3. Shimadzu: Determination of Free and Total Glycerol and Mono-, Di-, and Triglyceride Contents in Biodiesel According to EN 14105</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/an_05_sca_180_055_en_9b8677ed6a.pdf"><strong>Full PDF for download</strong></a></li></ul><h4><strong>User benefits</strong></h4><ul><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=1&amp;search=2060"><strong>Nexis GC-2060</strong></a> offers reliable analysis of biodiesel samples regarding their free and total glycerol and mono-, di-, and triglyceride contents, using hydrogen as a cost-effective carrier gas&nbsp;</li><li>Hydrogen carrier gas can be used safely through built-in safety measures</li><li>The multi-mode injection unit (MMI) allows selection of the preferred injection mode – direct (simple OCI) or convenient splitless PTV mode – both delivering excellent instrument performance in line with the standard’s requirements</li></ul><p>Playing a vital part in countries’ efforts to lower greenhouse gas emissions, biofuels can be manufactured from various feedstocks such as vegetable oils, animal-derived fats, and recycled cooking oils. Biodiesel production predominantly uses rapeseed, soybean, and palm oils. Because feedstocks are so varied, ongoing quality monitoring is essential - since the raw material’s quality greatly influencesthe final biodiesel quality.&nbsp;</p><p>The EN 14105:2024 describes the determination of free and total glycerol contents and mono-, di-, and triglyceride contents in biodiesel by means of gas chromatography with flame ionization detection (GC-FID). Injection shall be performed via on-column injector or an equivalent device<sup>1</sup>.&nbsp;</p><p>This study shows the analysis of biodiesel originating from rapeseed, soybean, and palm oil using the Nexis GC-2060 gas chromatograph and its multi-mode injection unit (MMI).</p><h4><strong>Configuration and Analysis Conditions</strong></h4><p>Gas chromatograph <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=1&amp;search=2060"><strong>Nexis GC-2060</strong></a> with multi-mode injection unit (MMI), flame-ionization detector (FID) and autosampler <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=1&amp;search=AOC+-30i"><strong>AOC -30i</strong></a>.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>Nexis and AOC are trademarks of Shimadzu Corporation or its affiliated companies in Japan and/or other countries.. Nexis GC-2060 provides reliable analysis of biodiesel samples for glycerol and glyceride contents according to EN 14105:2024 across the commonly used feedstocks. It supports hydrogen as a cost-effective carrier gas, while the multi-mode injection unit (MMI) offers selection of the injection mode based on user preference: direct mode representing simple on-column (OCI) analysis or splitless programmed temperature vaporization (PTV) mode as a convenient alternative that delivers comparable performance.</p><h3><strong>4. Thermo Fisher Scientific: Streamlined static headspace GC–MS approach for detection of impurities in recycled PET</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/an_004458_gc_ms_impurities_recycled_pet_an004458_na_en_6cb2435671.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Polyethylene terephthalate (PET) is a widely used thermoplastic polymer valued for its strength, low weight, durability, and adaptability. Owing to these properties, it is extensively applied in packaging, textile fibers, and electronic components. PET is particularly suitable for recycling because it can be melted and reshaped multiple times with minimal loss of performance, and it is easily recognizable by the recycling code “1” (♳). The recycling of PET involves several stages, including collection, sorting, transport, processing, washing, pelletizing, and remanufacturing into new products [1]. However, during these steps, contaminants such as plasticizers, residual monomers, and degradation byproducts may be introduced.&nbsp;</p><p>The presence of such substances can pose potential risks to both environmental and human health, making the identification and characterization of contaminants in recycled PET essential for evaluating material quality and safety. Among the non-intentionally added substances (NIAS), benzene, acetaldehyde, and limonene are of particular relevance. Benzene is a recognized carcinogen and represents a serious health concern if present in PET. It may form as a degradation product of PET, with the reaction catalyzed by acidic compounds released at high temperatures by polymer impurities such as polyvinyl chloride (PVC). Poor temperature control or overheating can increase benzene formation as a degradation byproduct. Acetaldehyde, another degradation product of PET generated during bottle manufacturing, can alter the sensory properties of bottled beverages. Limonene, a flavor compound commonly present in soft drinks, may be absorbed into recycled PET and subsequently migrate into packaged beverages, potentially affecting product quality.&nbsp;</p><p>Gas chromatography coupled to headspace sampling is a fast and simple technique that enables the extraction of volatile and semivolatile compounds from solid and liquid samples without the need for time-consuming sample preparation.&nbsp;</p><p>In this study, headspace sampling coupled to single quadrupole mass spectrometry was used to assess the overall quantitative performance for analysis of acetaldehyde, benzene, and limonene in recycled PET packaging.&nbsp;</p><p>The capability of the Thermo Scientific™ ISQ™ 7610 single quadrupole GC–MS of combining the simultaneous acquisition of both single ion monitoring (SIM) and full scan (FS) allowed for sensitive targeted analysis as well as screening of unknown contaminants possibly present in recycled PET bottles.</p><h4><strong>Experimental&nbsp;</strong></h4><p>In all experiments, a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/64"><strong>TriPlus 500 HS autosampler</strong></a> was coupled to a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/486"><strong>Thermo Scientific™ TRACE™ 1610 Gas Chromatograph (GC)</strong></a>, configured with a Thermo Scientific™ iConnect™ Split/splitless Injector Module (iConnect-SSL), and connected to an <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/484"><strong>ISQ 7610 single quadrupole mass spectrometer</strong></a>.&nbsp;</p><p>The separation of the target analytes was achieved using a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1751"><strong>Thermo Scientific™ Trace GOLD™ TG-624 SILMS capillary column</strong></a>, 60 m x 0.25 mm x 1.4 µm (Part No. 26059-3330). This column provides a low to mid polarity phase with high thermal stability (maximum operating temperatures up to 320 °C) and high inertness, enabling Gaussian peak shapes for analysis of volatile organics. The TriPlus 500 HS autosampler is connected directly to the analytical column, removing the use of a long external transfer line. In this configuration, the SSL injector module is used only for the pneumatic control of the carrier gas and split flow.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>The results presented in this work demonstrate that headspace coupled to GC–MS provides a suitable and simple solution for analysis of contaminants in rPET, with no complex sample preparation required.&nbsp;</p><ul><li>The capability of combining FS with SIM acquisition allows for qualitative and quantitative analysis, increasing confidence in compound identification through spectral comparison with NIST library and allowing for the detection of possible analyte co-elution.&nbsp;</li><li>The TriPlus 500 HS autosampler provides highly repeatable solventless extraction from solid samples with absolute area counts RSD &lt; 5%, permitting reliable and consistent quantitative data.&nbsp;</li><li>The ISQ 7610 single quadrupole GC–MS demonstrates an extended linear response (≥ 4–5 orders of magnitude) with R2 ≥ 0.997, calculated amounts within ± 20% the expected value, and ion ratio deviation ≤ 15% across the calibration curve.&nbsp;</li><li>Sensitivity was demonstrated with overall calculated LOD ≤ 0.03 ng/µL.</li><li>Chromeleon CDS helps ensure data integrity, traceability, and effective data management from instrument control to the final report streamlining analysis and data review processes.</li></ul></div></div></div></div></div></div></section></div></div></div></div></div></div></section>

News from LabRulezGCMS Library - Week 36, 2026

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