<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 1st September 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</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 / ASMS </strong>and application notes by <strong>EST Analytical</strong> and <strong>Shimadzu!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Analysis of Phthalates Using GC/MS With Hydrogen Carrier Gas: The Importance of Reducing Interferences and Contamination&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_5977c_phthalates_hydrogen_gas_asms_2025_mp_359_en_agilent_d51f599179.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Due to the price of helium (He), many laboratories are looking for alternative carrier gases for their gas chromatography/mass spectrometry (GC/MS) methods. This work describes the evaluation of a single quadrupole GC/MS method for the analysis of 19 phthalates using hydrogen carrier gas and an EI source 1 . The method provides excellent peak shape, resolution, sensitivity, and a 13 min run time. Calibration curves were linear for 16 of the phthalates, with the remaining 3 alkoxy phthalates requiring a quadratic fit. Except for DINP and DIDP (mixtures of isomers), all compounds could be quantitated at low pg levels. Specific attention to the consumables used and their preparation before use is discussed and is important for reaching the lowest calibration levels.</p><h4><strong>Experimental</strong></h4><ul><li><strong>GC: </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+gc"><strong>Agilent 8890 GC</strong></a> with <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7693A"><strong>Agilent 7693A automatic liquid sampler</strong></a> and tray</li><li><strong>Column: </strong>Agilent HP-5MS UI 20 m x 0.18 mm id x 0.18 µm (p/n 19091S-577UI)</li><li><strong>MSD: </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977C+GC%2FMSD"><strong>Agilent 5977C Inert Plus GC/MSD</strong></a></li></ul><h4><strong>Conclusions</strong></h4><ul><li>The Agilent 5977C GC/MSD and 8890 GC, when used with the method described here, provide excellent peak shape, resolution, sensitivity, and a 13 min run time..&nbsp;</li><li>The combination of hydrogen carrier and the Agilent J&amp;W HP-5ms 180 µm diameter column allowed for reduced analysis time relative to helium and a 250 µm diameter column .&nbsp;</li><li>Calibration curves were linear for 14 of the phthalates from 1 to 1,000 pg. DMEP and DBEP required quadratic curve fits, and DMEP and DEHP were calibrated from 2.5 to 1,000 pg. DINP and DIDP were calibrated from 50 to 20,000 pg with a linear fit.&nbsp;</li><li>Specific attention to the consumables used and their preparation before use is important for reaching the lowest calibration levels.</li></ul><h3><strong>2. EST Analytical: The Determination of Flavors in E-Liquids Using Purge and Trap Concentration</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_E_Liquid_Compound_Sampling_Using_Purge_and_Trap_5c709b52f0.pdf"><strong>Full PDF for download</strong></a></li></ul><p>E-liquid can be composed of propylene glycol or vegetable glycerin alone or can be a combination of the two. Propylene glycol is less viscous and carries better flavor. It also acts as a preservative. However, it does produce less vapor and some people are allergic to it. Vegetable glycerin, on the other hand, is much denser, is super hypoallergenic and produces more vapor. The drawback to the vegetable glycerin is that it is not a preservative, so the vape liquid will not last as long. Both glycerin and propylene glycol readily dissolve in water, so preparing the samples to test by purge and trap was relatively easy. Conversely, as the E-liquid emitted a strong odor of the added flavors, only a small amount of the solution could be used for analysis. The volatile flavor components of the vape liquid were examined by dissolving the solution in water and sampling the water using purge and trap.</p><h4><strong>Experimental</strong></h4><p>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160"><strong>Evolution purge and trap concentrator </strong></a>was configured with a Vocarb 3000 trap. The trap was conditioned at 260ºC for one hour. The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159"><strong>Centurion WS syringe autosampler</strong></a> was set in water mode in order to run 5 ml samples. Next, samples were prepared using 10ul of vape solution dissolved in 100mls of de-ionized water. The parameters for the autosampler/purge and trap concentrator and the Gas Chromatograph/Mass Spectrometer (GC/MS) are outlined in Tables 1 and 2.</p><h4><strong>Conclusions</strong></h4><p>Since vape solution readily dissolves into water, purge and trap sampling proved to be an excellent technique for the determination of the volatile compounds in the E-liquids. Purge and trap sampling is an exhaustive sampling technique, so the results were very reproducible and provided the sensitivity to determine the lower level compounds in the solution. Furthermore, it was found that nicotine addition to the solution has an effect some of the compounds in the solution. So, the taste of the vape liquid is affected by the amount nicotine in the mix.</p><h3><strong>3. Shimadzu: Determination of Nitrobenzene Compounds in Nifedipine by GCMS&nbsp;</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_03_gcms_589_en_23eda751e7.pdf"><strong>Full PDF for download</strong></a></li></ul><h4><strong>User Benefits</strong></h4><ul><li>The direct dissolution protocol without pre-treatment, significantly enhancing analytical efficiency.</li><li>The specificity of the method is ensured by monitoring the characteristic ions of nitrobenzene compounds in selected ion monitoring (SIM) mode, which provides robust resistance to interferences.</li></ul><p>Nifedipine, a dihydropyridine calcium channel blocker with vasodilatory properties, is primarily indicated for the clinical management of hypertension and angina pectoris. Its synthetic route commences with 2-nitrotoluene as the starting material. Notably, the intermediate 2-nitrobenzyl alcohol, the byproduct 2- nitrobenzyl bromide, the reaction product 2-nitrobenzaldehyde, and potential impurities (3-nitrobenzaldehyde and 4- nitrobenzaldehyde) all contain nitrobenzene moieties, rendering them candidatesfor monitoring as potential genotoxic impurities. Previous studies have demonstrated that 2-nitrobenzaldehyde and 4-nitrobenzaldehyde exhibit mutagenicity in the Ames test, while 2-nitrotoluene has shown carcinogenicity in animal experiments. In accordance with the toxicological concern threshold (TTC) control approach specified in ICH M7, a threshold of 1.5 μg/day is recommended for genotoxic impurities in pharmaceuticals intended for lifelong administration. In this study, a method for the determination of six genotoxic impurities in nifedipine was developed using a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050"><strong>Shimadzu GCMSQP2050</strong></a> gas chromatography mass spectrometry. This method features simplified sample preparation, high sensitivity, and favorable repeatability, thereby enabling effective monitoring of the six nitrobenzene compounds as genotoxic impurities in nifedipine pharmaceutical.</p><h4><strong>Analytical Conditions</strong></h4><p>The analytical conditions are shown in Table1. <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2050"><strong>GCMS-QP2050</strong></a> system was used for this Application News.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>A GC-MS method was established for the quantification of six nitrobenzene genotoxic impurities in nifedipine pharmaceuticals using a Shimadzu GCMS-QP2050 system. The calibration curves showed excellent linearity within the concentration range of 20-200 μg/L, with correlation coefficients (R&gt;0.999). Precision was evaluated through six replicate injections of the 50 μg/L standard solution, and the relative standard deviations (RSDs) of peak areas for all analytes were less than 4%. Spike recovery experiments were performed at three concentration levels (0.005, 0.01, and 0.032 μg/g) in actual matrices, resulting in recovery rates ranging from 95.85% to 117.64%. This method is characterized by simplified sample preparation, high sensitivity (IDLs of 0.263-0.496 μg/L), and good repeatability. Overall, it provides a validated analytical strategy for quality control monitoring of the target genotoxic impurities.</p>

News from LabRulezGCMS Library - Week 36, 2025

Synthesis and Identification of 3-Oxazolines in Cocoa

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 29th September 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies </strong>and<strong> EST Analytical, </strong>poster by<strong> Shimadzu </strong>and smart note by <strong>Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies: Equimolar Response to ASTM D5623 Relevant Sulfur Compounds</strong></h3><p><strong>Using an </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890+GC"><strong>Agilent 8890 gas chromatograph</strong></a><strong> and </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8355%C2%A0SCD"><strong>8355 sulfur chemiluminescence detector (GC/SCD)</strong></a></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_equimolar_response_astm_d5623_sulfur_compounds_5994_8562en_agilent_62a37181e4.pdf"><strong>Full PDF for download</strong></a></li></ul><p>For many years, the use of a sulfur-specific detector in the petroleum industry has been invaluable for accurately identifying low levels of sulfur-containing compounds in petroleum at various stages of production.<sup>1</sup> Many environmental and health requirements limit the amount of sulfur allowed in the final petroleum product. The presence of sulfur also has the potential to poison the catalytic processes that take place during petroleum refining.&nbsp;</p><p>Along with the determination of low sulfur levels in a petroleum sample, a detector may also need to measure high sulfur levels and total sulfur content. A detector with a high linear range is essential in making both low-level and high‑level determinations of sulfur in a petroleum sample.&nbsp;</p><p>In this application note, an Agilent 8355 SCD was used to measure 19 sulfur-containing compounds within a standard sample. The 8355 SCD is ideal for the widely used ASTM&nbsp;D5623 method<sup>2</sup> because of its ability to obtain linear and equimolar responses to sulfur compounds with minimal hydrocarbon interference. When comparing the equimolar response of analytes containing different numbers of sulfur atoms, the response should be double for the analytes containing two sulfur atoms compared to those with one&nbsp;sulfur atom.&nbsp;</p><p>Another advantage of the 8355 SCD is the ability to use it in tandem with an FID. This combination allows monitoring solvent elution through the GC system, assisting in the detection of the coelution of solvents with analyte peaks. These coelutions can cause peak distortion, which might be mistaken for activity issues within the GC system.</p><h4><strong>Methods&nbsp;</strong></h4><h5><strong>Instrumentation&nbsp;</strong></h5><p>Two <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890+GC"><strong>Agilent 8890 GC systems</strong></a> were equipped with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8355%C2%A0SCD"><strong>8355&nbsp;SCD</strong></a>. Both GC/SCD systems were run in the same manner to confirm equimolar results. A third GC system was also configured with a tandem flame ionization detector sulfur chemiluminescence detector (FID/SCD) to allow the determination of the solvent peak elution from the system. This third system also served as another confirmation of the equimolar results that were obtained from the other two GC/SCD systems. Sample introduction for all systems was completed with an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7693A+automatic+liquid+sampler"><strong>7693A automatic liquid sampler</strong></a> with a 5 µL syringe. The sample volume for each injection was 1.0 µL. All analyses were performed with a split/splitless inlet in split mode.&nbsp;</p><p>The GC/SCD parameters are provided in Table 1. Note that an Agilent DB-Sulfur SCD GC column (part number G3903-63002) was used in this study because of the low column bleed and excellent inertness and performance for sulfur compound analysis. When using the SCD, be aware that stationary phase bleed from the GC column can lead to fouling of the ceramic tubes within the detector. This phenomenon can cause poor SCD performance, such as decreased sensitivity, and may require more frequent maintenance. Proper GC column selection (such as the DB-Sulfur column) is important to ensure lower column bleed into the detector and will reduce fouling of ceramic tubes, reducing instrument downtime.</p><h4><strong>Results and discussion</strong></h4><h5><strong>Use of GC/FID for solvent elution determination&nbsp;</strong></h5><p>Determination of the solvent peak elution can be a challenge when using a sulfur-selective detector such as the SCD. Many times, the large, fronting solvent peak may coelute with analytes of interest, causing distortion of the analyte peak shape (peak tailing, fronting, or broadening) and poor chromatographic separation. This poor peak shape, caused by column overloading, can be mistaken for activity issues in the system or hydrocarbon interferences, leading to unnecessary troubleshooting or inlet/column maintenance. Determination of the solvent peak elution time is recommended to ensure that coelution does not occur with any of the analytes of interest. To confirm the solvent elution time, a tandem GC/FID/SCD system was used. The GC/FID/SCD system puts the FID in-line before the SCD analysis, allowing the user to obtain both FID and SCD signals from a single injection, thus confirming the solvent retention time and determining any solvent/analyte coelutions.&nbsp;</p><h4><strong>Conclusion&nbsp;</strong></h4><p>The Agilent 8355 sulfur chemiluminescence detector, paired with an Agilent 8890 GC, was evaluated by analyzing 19&nbsp;sulfur‑containing compounds relevant to ASTM D5623. The SCD met the specifications of the test method, including an equimolar response to the analyzed sulfur compounds and a wide range of linearity to a sulfur-containing standard. The 8355 SCD shows excellent area reproducibility, and when used in tandem with a flame ionization detector, the system can aid in the determination of solvent peak elution through the GC system.</p><h3><strong>2. EST Analytical: Reducing Carryover in Environmental Water Samples</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_Reducing_Carryover_in_Environmental_Water_Samples_6e5ba0a008.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In order to mitigate carryover, many environmental labs resort to running sample dilutions or adding blank samples after a highly contaminated sample. Both of these solutions are not ideal and can lead to a loss of analyte detection when diluting or a loss of profits when blank samples need to be run.</p><p>Since, the primary source of carryover for water samples is the sparge vessel, purge and trap manufactures have incorporated a rinsing step in which the sparge vessel is “washed” with hot water in order to clean up the volatile compounds that may still reside in the sparge vessel. Expanding on the idea of limiting volatile compounds in the sparge vessel, EST Analytical developed a patented process of heating the sparge vessel during the bake step of the purge and trap process (Patent Number: US 8,075,842 B1) . This engineering innovation essentially performs two bakes; as a result both the trap and the sparge vessel are “cleaned” at the same time. No other concentrator is or can be engineered to do this.</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/2160"><strong>EST Analytical Evolution concentrator</strong></a> and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159"><strong>Centurion WS autosampler</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?manufacturerItems=1&amp;search=5975C"><strong>5975C 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</strong></a> MS 30m x 0.25mm x 1.4µm column. Refer to Table 1 for the sampling method parameters and Table 2 for GC/MS parameters.</p><h4><strong>Conclusions</strong></h4><p>The Evolution purge and trap concentrator with its patented technique of heating the sparge vessel during the bake process proved to reduce carryover by almost half when comparing with hot water rinses alone. The advantages of reduced carryover are many. Primary among them is the ability to run more samples during the twelve hour tune window. This increase in productivity translates to more laboratory profits and better use of instrument time.</p><h3><strong>3. Shimadzu / AOAC: Analysis of PFAS in juice using Head-Space Solid Phase Microextraction-Gas Chromatography/Mass Spectrometry (HS-SPME GCMS)</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/aoac_2025_t010_9967ebebff.pdf"><strong>Full PDF for download</strong></a></li></ul><p>PFAS contaminate water and food through packaging that can leach volatile PFAS from plastics and inks or coatings. This work developed a headspace SPME GCMS method to analyze six volatile PFAS classes in juices. The United States Food and Drug Administration has tested for PFAS in a broad range of foods and beverages as part of its Total Diet Study. Juice matrices differ in flavor, sugar, as well as manufacturing practices, and packaging, with the latter two potentially introducing PFAS contamination. The former differences between products can impact PFAS detection.</p><h4><strong>Materials and Methods</strong></h4><p>The SPME method used in this study is based on a method published by Bach et.al. (2016). An HS-SPME method is used to improve method performance when analyzing complex aqueous samples over direct immersion. The optimized parameters of the instrument method for the targeted PFAS are listed in table 1.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-TQ8040+NX"><strong>Shimadzu GCMS-TQ8040 NX triple quadrupole instrument</strong></a>, configured with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=AOC-6000+Plus+SPME"><strong>AOC-6000 Plus SPME</strong></a> unit, was used to measure PFAS in different juice samples. Without isotope dilution, matrix effects caused recoveries to fall outside of acceptable criteria. Method blanks showed no detectable PFAS, and calibration demonstrated excellent linearity (R² ≥ 0.993). This HS-SPME GCMS-TQ8040 NX method demonstrated quantitative capability for analyzing nanogram-per-liter PFAS compounds in complex juice matrices. This application highlights a simple, fast, robust, precise, and accurate workflow for measuring volatile PFAS in challenging matrices.</p><h3><strong>4. Thermo Fisher Scientific: Safe use of carrier hydrogen for air monitoring with Multi-Gas TD-GC-MS</strong></h3><ul><li>Other document (smart note)</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/sn_003958_gc_single_quad_gc_ms_isq_7610_environmental_sn003958_na_en_8216fc7021.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Monitoring volatile organic air compounds, also known as hazardous air pollutants (HAPs), is crucial for maintaining air quality in urban and industrial environments due to their significant health risks. The growing concerns about these potentially dangerous volatile organic compounds in ambient air, particularly in urban areas and from industrial emissions, have led to the development of numerous national and international regulations. The use of Thermal Desorption (TD) coupled with GC-MS is the analytical technique of choice to enrich volatile organic compounds from air and quantify them at trace levels.1 In gas chromatography, the choice of carrier gas is pivotal for the separation and detection of VOCs. Helium has traditionally been the preferred carrier gas for analyzing volatile organic air toxics due to its inertness and performance benefits. However, hydrogen is becoming increasingly popular due to economic and supply considerations. Each carrier gas has unique advantages and challenges, and the choice should be guided by specific analytical requirements, cost constraints, and safety protocols. As the demand for sustainable and cost-effective solutions grows, hydrogen is expected to play a more significant role in monitoring hazardous air pollutants in urban and industrial settings.</p><p>Thermal Desorption is an established way to analyze VOCs in a wide variety of sample types. This smart note highlights the use of the new Multi-Gas TD system (Markes International) that allows a safe use of carrier hydrogen for the analysis of VOCs in air, enhancing operational flexibility and supporting more sustainable laboratory practices.&nbsp;</p><h4><strong>Experimental&nbsp;</strong></h4><p>In this study, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=7&amp;search=TD100-xr"><strong>Markes TD100-xr™ Multi-Gas system</strong></a>, coupled with the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/486"><strong>Thermo Scientific™ TRACE™ 1610 gas chromatograph</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/484"><strong>Thermo Scientific™ ISQ™ 7610 single quadrupole mass spectrometer,</strong></a> was employed to accurately detect and quantify compounds for effective air monitoring. This combination leverages several technological advancements to optimize analytical performance and operational efficiency.</p><p>The comparison between helium and hydrogen carrier gas was carried out using the same analytical column. The method conditions for all analytes could be easily transferred. Flow rates were adjusted using the split ratio calculator available in the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76"><strong>Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)</strong></a> Instrument Method Wizard (Figure 1) to maintain the same split level and therefore the same amount of transferred sample. A further factor facilitating rapid adoption of hydrogen carrier gas in laboratories is that existing columns and consumables can be used without restrictions.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>The use of the Markes TD100-xr Multi-Gas system combined with the ISQ 7610 GC-MS for the analysis of VOC in air allows for a safe use of carrier hydrogen, making it a viable alternative to helium and offering an effective solution for laboratories facing the challenges of helium scarcity and rising costs, while maintaining the accuracy and reliability of VOC detection and quantification.&nbsp;</p><ul><li>The comparative analysis clearly confirmed that using hydrogen carrier gas in gas chromatography offers substantial benefits over helium. The significant reduction in retention time, as shown by the 60% decrease for 1,2,3-trichlorobenzene, leads to faster analysis without compromising the separation efficiency.&nbsp;</li><li>Enabling shorter analysis time, hydrogen enhances laboratory productivity, reduces costs, and contributes to more sustainable practices.&nbsp;</li><li>The results also indicate that both helium and hydrogen can be used effectively as carrier gases without impacting the response linearity for the VOC compounds under evaluation. Laboratories can confidently use hydrogen as an alternative to helium for quantitative analysis, ensuring accurate and reliable analytical results.</li><li>When using multiple carrier gases, the ISQ 7610 NeverVent technology is key to easily switching from helium to hydrogen and back to helium with no venting required, making this operation very quick and safe.&nbsp;</li></ul><p>In conclusion, coupling the Markes TD100-xr Multi-Gas system with the ISQ 7610 single quadrupole GC-MS offers a robust and flexible solution for air monitoring. This integration enhances operational efficiency, reduces costs, and maintains high data integrity, making it an invaluable tool for modern analytical laboratories.</p>

News from LabRulezGCMS Library - Week 40, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 6th 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>application notes by<strong> EST Analytical </strong>and<strong> Shimadzu </strong>and brochure by <strong>Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies / AOAC: Method Translation for the Analysis of Vanilla Extracts Using a Compact, Single Channel GC-FID and Carrier Gas Switching Module</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_vanilla_single_channel_gcfid_carrier_gas_aoac_2025_w020_en_agilent_17c7d568c9.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Vanilla is a flavor variety that has been heavily impacted by changes in consumer habits as well as by supply and demand of vanilla beans used to produce high-quality vanilla extracts. Unfortunately, these market conditions, increase the likelihood of adulteration in vanilla extracts by use of aroma chemicals that are not naturally occurring. Common adulterants are coumarin (C), ethyl vanillin (EV), eugenol (E), and guaiacol (G).2,3 Adulteration impacts the standard of identity for vanilla extracts established by the U.S. FDA; therefore, flavor companies rely on QC labs to implement reliable and sensitive analysis techniques for screening incoming raw ingredients against expected purity standards before the ingredient can enter a flavor formula on the manufacturing floor. Screening is typically executed with gas chromatography (GC)- based methods adapted from those used in a R&amp;D lab. However, differences in column length, diameter, and phase can make it seem challenging to harmonize GC methods across the R&amp;D and QC functions within a company due to the different analysis objectives of the respective laboratories.&nbsp;</p><h4><strong>Experimental Goals</strong></h4><ul><li>Demonstrate the ease of the Agilent Method Translator in harmonizing GC methods for multiple columns and gases&nbsp;</li><li>Establish method precision, linearity, and resolution on standards of vanilla-like adulterants using the translated methods&nbsp;</li><li>Successfully showcase the method translation using store-bought extracts to verify the integrity of the fastest GC method on samples containing matrix&nbsp;</li><li>Screen for and quantify any vanilla adulterants in the samples of vanilla extracts with the goal of detecting no adulterants using the fastest GC method.</li></ul><h4><strong>Experimental&nbsp;</strong></h4><ul><li><strong>GC System:</strong> <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8850+GC"><strong>Agilent 8850 GC</strong></a> with <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7693A+Automatic+Liquid+Sampler"><strong>7693A Automatic Liquid Sampler</strong></a></li></ul><h4><strong>Conclusions</strong></h4><h5><strong>Method Translation</strong></h5><ul><li>The method translator tool provided an easy conversion of a 50-minute-long method to one that is &lt; 5 minutes resulting in a speed gain of 10-fold and 14-fold, for He and H2 carrier gases, respectively (Figures 2 and 3)&nbsp;</li><li>Resolution of analytes were &gt;4 on the 60 m and &gt;3.5 on the 10 m DB-1 columns (Table 2)</li><li>Precision was &lt;1.85% RSD and &lt;2.5% RSD for He and H2 carrier, respectively (Table 3)</li><li>Linearity was demonstrated from 10 ppm to 100,000 ppm for He and H2 carrier with R2 ranging from 0.9997 to 1.0000&nbsp;</li></ul><h5><strong>Carrier Gas Switching</strong></h5><ul><li>He and H2 carrier gases were alternated line by line in a sequence table for increased analytical efficiency and higher throughput while demonstrating the flexibility the helium conservation module provides its users while also eliminating manual changes to plumbed gases at the GC EPC Module.</li></ul><h3><strong>2. EST Analytical: Optimizing 8260 Sample Throughput - Solutions for the Determination of Bromomethane by Purge and Trap</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_Solutions_for_the_Determination_and_Stability_of_Bromomethane_by_P_and_T_App_Note_Rev_2_177c75d029.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The United States Environmental Protection Agency’s (USEPA) Method 8260 has an extensive list of compounds of interest. In order to purge and trap these analytes, there needs to be an analytical trap able to trap these compounds and desorb them to the Gas Chromatograph/Mass Spectrometer (GC/MS) both accurately and efficiently. Due to the broad range of compounds on the Method 8260 list, there are many issues to take into account. Purge efficiency, molecular weight, volatility, and water are among the most problematic issues. The purge and trap concentrator and analytical trap must be able to account for all of these concerns.&nbsp;</p><p>The most commonly used analytical trap is the Vocarb® 3000 due to its ability to trap and desorb the extensive analyte list both effectively and correctly. However, the Vocarb® 3000 trap is not without its drawbacks. One of which is Bromomethane degradation in the trap over time. This application will examine the Vocarb® 3000 and a custom trap along with the optimum trap temperature parameters for the stability of Bromomethane.&nbsp;</p><h4><strong>Experimental</strong></h4><p>The purge and trap concentrator used for this study was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160"><strong>EST Analytical Evolution</strong></a>. The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159"><strong>Centurion Water and Soil autosampler</strong></a> equipped with the syringe option was employed as the autosampler. Separation and analysis of the volatile compounds was performed by the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7890A"><strong>Agilent 7890A Gas Chromatograph (GC) </strong></a>and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977B"><strong>5977B Mass Spectrometer</strong></a> (MS). 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 Rxi624 Sil MS</strong></a> 30m x 0.25mm x 1.4µm column. The purge and trap parameters and analytical traps used for this study are listed in Tables 1 and 2 while Table 3 details the GC/MS parameters.</p><h4><strong>Conclusions</strong></h4><p>Initially, all of the traps and heating parameters used in the EST Analytical Evolution met USEPA method 8260 requirements and could be used in the laboratory. However, the custom trap and the higher temperature desorb and bake showed a lower response when compared to using a lower temperature desorb and bake. Furthermore, over time, the custom trap and higher temperature desorb and bake displayed lower recoveries of Bromomethane which could in turn affect the continuing calibration standards. The Vocarb® 3000 trap with the lower temperature desorb and bake proved to be the optimum method for sampling USEPA Method 8260 compounds. The technique met all of the method requirements and exhibited the best response and stability not only for Bromomethane but also for the rest of the extensive compound list.</p><h3><strong>3. Shimadzu: Quantitative Analysis of Furan and Alkylfurans in Processed Food Using Headspace GC-MS</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_00906_en_878a49b98e.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Furan and alkylfurans are aromatic compounds with a fivemembered ring structure. Furan and some alkylfurans, such as 2-methylfuran, 3-methylfuran, and 2,5-methylfuran (furan with a hydrocarbon chain attached), are found in processed food. They are generated through a variety of pathways during heat treatment of the food. Some countries have studied these compounds and concluded they are a health concern. 1) At present, no country has set permissible levels for furan or alkylfurans in food. But since they are harmful substances that are generated unintentionally during the processing of food, analyzing them is becoming increasingly important. In this Application News, the levels of furan and alkylfurans in commercially available processed food were measured.</p><h4><strong>Equipment&nbsp;</strong></h4><p>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 has a compact design for a smaller installation footprint. When combined with 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>, the GCMSQP2050 can simply and accurately measure furan and alkylfuran levels in processed food. The DuraEase ion source, which is specifically designed for durability and ease of maintenance, also providesreduced maintenance requirements.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>In this Application News, headspace GC-MS analysis was used to measure levels of furan and alkylfurans in processed food. Analysis of standard samples produced good results in terms of separation, calibration curve linearity, and repeatability. Analyzing food samples and comparing the results obtained by the external standard method and the standard addition method showed that the matrix effects differed depending on the sample.</p><h3><strong>4. Thermo Fisher Scientific: Everything You Need in a GC Detector: VGA-100 Gas Chromatography Detector for TRACE 1600 Series GC</strong></h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/br_003592_gc_vuv_detector_vga_100_isomers_br003592_na_en_0a48830aff.pdf"><strong>Full PDF for download</strong></a></li></ul><h4><strong>Performance synergy—the VGA-100 detector and the </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/483"><strong>TRACE 1600 Series GC</strong></a><strong>&nbsp;</strong></h4><p>VUV absorbance and gas chromatography offer a perfect match, joining insights on light absorption in the VUV range with each compound’s unique gas phase absorption features. The innovative VUV absorption technology of the VGA-100, combined with the robust and reliable performance of the Thermo Scientific™ TRACE™ 1600 Series gas chromatograph, offers a powerful analytical solution to support timecritical laboratory demands.&nbsp;</p><p>Harnessing breakthrough gas chromatography technology, VGA-100 provides unmatched precision and data quality with faster results and higher sample volume. Experience analytical insights with a system designed for ease of use that delivers accurate, reportable results across a diverse range of industries.</p><h4><strong>Explore the benefits of VUV technology&nbsp;</strong></h4><p>The unique capabilities of the VGA-100 detector for the TRACE 1600 Series GC help solve common challenges, such as correct isomer identification, poor selectivity, long method run times, analyte co-elution, burdensome data processing and analysis, and method scalability to production environments.&nbsp;</p><h5><strong>Expand detectable compounds.&nbsp;</strong></h5><p>Access to a wider range of analytes with enhanced sensitivity towards impurities as well as accurate sample profiling, thanks to the combined universal and selective response of the VGA-100 detector.&nbsp;</p><h5><strong>Unambiguous identification.&nbsp;</strong></h5><p>The VGA-100 universal mass-sensitive detector delivers comprehensive data for robust analysis. Data provided in 3D (time, wavelengths, and intensity) supports reliable identification through spectra that can be matched to a dedicated library, including isomers discrimination.&nbsp;</p><h5><strong>Ease of use and maintenance.&nbsp;</strong></h5><p>Robust and easy to set up and operate, the VGA‑100 requires minimal maintenance, with no vacuum pumps required. An intuitive design supports high demands for throughput and compliance, supporting the needs of both research and quality control laboratories.&nbsp;</p><h5><strong>Faster analysis.&nbsp;</strong></h5><p>Obtain rapid and accurate results with the advanced capabilities of VUV technology, complemented by the fast and efficient chromatographic separation of the TRACE 1600 Series GC.&nbsp;</p><h5><strong>VUV Analyze Software for push-button simplicity&nbsp;</strong></h5><p>The advanced post-acquisition processing capabilities of VUV Analyze™ Software (VUV Analytics, Inc.) allows laboratories to generate meaningful results with just the push of a button. This cutting-edge software platform swiftly analyzes complex chromatographic and spectral data, delivering method-specific results and reports. By automating the analysis process, VUV Analyze Software significantly streamlines and speeds up each run while minimizing errors, leading to greater confidence in results.</p>

News from LabRulezGCMS Library - Week 41, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 5th January 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, EST Analytical </strong>and<strong> Shimadzu!</strong></p><h3><strong>1. Agilent Technologies: Ultrasensitive and Powerful GC/MS/MS for Analyzing Multipesticides in Black Pepper and Dried Tea</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_gcms_ms_black_pepper_5994_8783en_agilent_4b1cc85920.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Pesticides play a vital role in safeguarding crops and are indispensable in most farming settings to secure high yields.1 Regulatory authorities, including the Codex Alimentarius and the European Commission mandate the monitoring and reporting of pesticide residues found in or on food product.2 The analysis of pesticides in food faces several major challenges, such as the variety of pesticide classes, the complexity of different food matrices, the effects of these matrices, and the detection of target analytes at low&nbsp;concentrations.3&nbsp;</p><p>According to the EU's SANTE/11312/2021 guidelines, black pepper and dried tea are considered among the difficult or unique commodity matrices for multiresidue pesticide analysis.4 The matrix interferences are complex and diverse, including carbohydrates, fats, piperine, terpenoids (for black pepper)5 , and caffeine (in dried tea). "For dried tea, matrix interferences include polyphenols, pigments, polysaccharides, alkaloids, free amino acids, high caffeine levels, and&nbsp;catechins".6&nbsp;</p><p>In addition to affecting the analyte signals, matrix interferences can cause the system to become contaminated more quickly. This leads to a rapid decline in the sensitivity of the analytical instrument, and necessitates frequent maintenance, significantly reducing laboratory productivity. These are the current challenges faced by laboratories when analyzing pesticides in difficult and complex matrices.&nbsp;</p><p>To overcome these challenges, Agilent offers a robust solution with its backflush and JetClean self-cleaning ion source technologies integrated into the high-sensitivity 7010B GC/TQ system. Backflush technology prevents high‑boiling contaminants from reaching the detector, reducing the need for frequent maintenance and extending column life.7 This ensures consistent performance and minimizes downtime, thereby enhancing laboratory productivity.&nbsp;</p><p>With JetClean technology, your lab can significantly increase instrument uptime, as fewer manual cleanings are needed, maximizing productivity. This technology helps maintain data quality by ensuring a clean ion source, which guarantees run-to-run reproducibility. Additionally, JetClean enhances operator convenience through automated cleaning, requiring virtually no user intervention.8 Combined with the ultrasensitivity of the 7010B GC/TQ system, these technologies provide precise and reliable analysis of pesticides in complex matrices such as black pepper and dried tea. Agilent’s comprehensive approach effectively mitigates matrix interferences, preserves instrument sensitivity, and significantly boosts overall efficiency in pesticide analysis.</p><p>This application note describes a detailed approach for the simultaneous quantification of 284 pesticides in black pepper and dried tea samples. Agilent's solution for complex matrices demonstrates the sensitivity of the 8890 GC/7010B GC/TQ and confirms its robustness when using backflush and JetClean techniques.&nbsp;</p><h4><strong>Experimental and chemicals</strong></h4><h5><strong>GC/TQ parameters&nbsp;</strong></h5><p>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890"><strong>8890 GC</strong></a>/<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7010B"><strong>7010B GC/TQ systems</strong></a> (Figure 1) were optimized for wide calibration range performance. Equipped with an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7693A"><strong>7693A automatic liquid sampler </strong></a>and a 150-position tray, the GC operated in temperature‑programmed splitless injection mode with a multimode inlet. Detailed instrument parameters can be found in Table 1. Data acquisition was in dynamic MRM (dMRM) mode, enabling analysis of 284 pesticides with 1233 MRM transitions and up to 74 concurrent MRMs (see Figure 2). Retention time was synchronized with the Agilent Pesticides and Environmental Pollutants (P&amp;EP) 4.0 MRM Database, streamlining method&nbsp;setup.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This application note describes an approach for the analysis of multipesticides in complex and distinctive matrices, including black pepper and dried tea using the Agilent 8890 GC/7010B GC/TQ. The comprehensive solution successfully addresses the challenges encountered when analyzing multipesticides in difficult matrices such as black pepper and dried tea. The high sensitivity of the 7010B GC/TQ enables the application of deep dilution methods. Additionally, the use of backflush technology combined with the Agilent JetClean self-cleaning ion source ensures system stability and robustness, enhancing the operational efficiency of testing laboratories and reducing equipment downtime during&nbsp;maintenance.</p><h3><strong>2. EST Analytical: Static Headspace Sampling of Volatile Organic Compounds</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Flex_8260_by_Static_Headspace_7ddf2e4157.pdf"><strong>Full PDF for download</strong></a></li></ul><h4><strong>Discussion</strong></h4><p>Purge and trap sampling involves purging the VOCs out of the matrix and trapping the analytes onto an analytical trap, the trap is then desorbed to the GC/MS. This process has a number of pros and cons. On the positive side, purge and trap is more sensitive. It is also the recommended sampling technique for USEPA Methods. Furthermore, the advent of autosampling systems has simplified sample preparation. However, purge and trap does have some negatives, including active sites, worries about foaming samples, and trap degradation.</p><p>Static headspace sampling, on the other hand, is much simpler than purge and trap sampling. For this sampling technique, the sample is brought to equilibrium and a portion of the headspace is transferred to the GC/MS for separation and analysis. The simplicity of this technique is a definite pro. Moreover, this sampling process does not develop active sites, has no need for an analytical trap and the linear calibration range can be much higher than that of purge and trap sampling. Conversely, samples need to be manually prepped thus, losing their sample integrity. Additionally, the detection limits are higher for a number of compounds. Finally, some of the analytes do not partition into the headspace well enough and need method optimization.&nbsp;</p><p>In recent years, GC/MS systems have become much more sensitive. The advent of SIM/Scan acquisition techniques has made low level detection a much simpler proposition. This analysis will focus on the headspace sampling and analysis of over 50 volatile organic compounds.&nbsp;</p><h4><strong>Experimental</strong></h4><p>The sampling system used for this analysis was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2162"><strong>EST Analytical FLEX autosampler</strong></a> fitted with a 2.5ml headspace syringe. An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890+GC"><strong>Agilent 7890 GC</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5975"><strong>5975 MS</strong></a> were used for separation and analysis. The GC was configured with a Restek Rxi 624 Sil MS 30m x 250mm x 1.4µm column and a SKY 2mm x 6.5 x 78.5 splitless inlet liner. The MS was run in SIM/Scan mode. Refer to Tables 1 and 2 for the analysis and sampling parameters.</p><h4><strong>Conclusions</strong></h4><p>Static headspace sampling in conjunction with SIM/Scan acquisition proved to be a good alternative to purge and trap sampling for a number of USEPA Method 8260 compounds. The curve %RSD results showed the linearity of the curve to meet the USEPA Method 8260 requirement of 15% or better. The method detection limits of all the compounds tested also passed method requirements. Lastly, the precision and accuracy of the autosampling and analysis system was excellent, with the average precision at less than 6% RSD and the average %recovery at just over 101%.</p><h3><strong>3. Shimadzu: Aromatic Component Analysis of Gasoline According to ASTM D5580 Using the Brevis GC- 2050 Gas Chromatograph</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_01024_en_039b304288.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Aromatics, such as toluene and xylene, are sometimes added to gasoline to improve the octane number. Measuring the levels of these aromatics is essential for quality control in gasoline production. It is also important for environmental protection, in particular, for reducing emissions of benzene, a hazardous substance, as well as for sustainable energy use that reduces the environmental impact of gasoline while maintaining its performance.</p><p>ASTM D55801) is a standard test method that uses gas chromatography to measure aromatics in gasoline. Gasoline aromatics can be separated more effectively by switching between two gas chromatography columns of different polarities and venting non-aromatic components from the system. This Application News describes using the Brevis GC2050 gas chromatograph to determine aromatics in gasoline by applying ASTM D5580.</p><h4><strong>Equipment Configuration and Analytical Conditions&nbsp;</strong></h4><p>The system comprises a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Brevis+GC-2050"><strong>Brevis GC-2050 gas chromatograph</strong></a>, an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=AOC-30"><strong>AOC-30</strong></a> for sample injection, and a VB-30-S heated valve box. Aromatics were determined using two sets of Analysis Conditions that were tailored to measure different components (Table 1). Note that the timing of the flow path switching and other conditions needs to be adjusted according to the columns being used and the operating environment.</p><h4><strong>Determining Aromatics in Gasoline&nbsp;</strong></h4><p>A gasoline sample was prepared by adding 2 to 10 wt% aromatics and 10 wt% of an internal standard (2-hexanone) and then analyzed under Analysis Conditions A and Analysis Conditions B. Fig. 2 shows the chromatograms obtained under each set of Analysis Conditions. Despite gasoline containing large amounts of hydrocarbons, oxygenates, and other impurities, these impurities did not appear as peaks in the chromatograms, and only the aromatics added to the gasoline were detected. These results verify the utility of using flow path switching to effectively utilize the characteristics of two different columns.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>A flow path switching valve was installed on a Brevis GC-2050 gas chromatograph to enable the determination of gasoline aromatics (benzene, toluene, ethylbenzene, p/m-xylene, oxylene, and C9+ aromatics) according to ASTM D5580.&nbsp;</p><p>This system can switch between different columns during analysis to determine specific aromatics from among the many compounds present in gasoline. Analysis was performed under two sets of conditions, each using different flow path switching times. This method met the requirements for linearity and reproducibility described in ASTM D5580. The timing of flow path switching can also be adjusted to allow the targeted determination of oxygenates in gasoline. The ability to perform multiple analyses on a single system means the Brevis GC-2050 offers even greater functionality as a compact gas chromatograph.</p>

News from LabRulezGCMS Library - Week 02, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 15th June 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 brochure by <strong>Agilent Technologies, </strong>application note<strong> </strong>by<strong> Shimadzu</strong>, presentation by <strong>MDCW / Institut d’Investigació Sanitària Pere Virgili </strong>and poster by<strong> Waters Corporation!</strong></p><h3><strong>1. Agilent Technologies: </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8860B"><strong>Agilent 8860B Gas Chromatograph</strong></a></h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ds_8860_gas_chromatograph_5994_9066en_agilent_f4d445178f.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8860B"><strong>Agilent 8860B gas chromatograph</strong></a> delivers reliable, repeatable performance for routine analyses, combining proven GC expertise with simplified operation. A bright color touchscreen provides quick access to system setpoints, configuration details, flowpath information, and live signal plots to easily monitor run progress. For deeper control, the built‑in Agilent GC Assist interface—optimized for tablets, PCs, and mobile devices—offers advanced system intelligence, including remote status checks, self‑guided diagnostics, maintenance tools, and method and sequence&nbsp;editing. The 8860B supports full electronic pneumatics control (EPC) or electronic pneumatics regulation (EPR), enabling precise, automated or electronically adjusted gas management. Both EPC and EPR use robust 7th‑generation microchannel architecture, designed for superior protection against contaminants and improved long-term reliability.</p><h4><strong>GC system capabilities&nbsp;</strong></h4><ul><li><strong>Retention time repeatability: </strong>&lt; 0.03% or 0.003 minutes&nbsp;</li><li><strong>Area repeatability:&nbsp;</strong><ul><li>&lt; 1.0% RSD&nbsp;</li><li>The 8860B display comes with physical start/stop buttons for manual analysis&nbsp;</li><li>Easy access to maintenance and service modes from the GC&nbsp;Assist interface, including autonomous leak checks&nbsp;</li><li>The GC Assist interface provides remote connectivity enabling you to monitor your smart GC system, check system logs, and perform diagnostics tests, from inside or outside the laboratory&nbsp;</li><li>Atmospheric pressure and temperature compensation are built into every system, so results do not change, even when the laboratory environment does.</li></ul></li><li><strong>Simultaneously supports&nbsp;</strong><ul><li>Two inlets&nbsp;</li><li>Three detectors &nbsp;</li><li>Support for up to any combination of three valves total:&nbsp;<ul><li>Up to four heated gas sample valves&nbsp;</li><li>Up to two liquid sampling valves&nbsp;</li></ul></li><li>Dual sample introduction capabilities:&nbsp;<ul><li>Supports two <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7693A"><strong>7693A</strong></a> autoinjectors with capacity for 16&nbsp;sample vials&nbsp;</li><li>Supports one 7693A autoinjector and automatic sampler tray with capacity for 150 sample vials&nbsp;</li><li>Supports one 7650A autoinjector with capacity for 50 sample vials with one 7693A with capacity for 16&nbsp;sample vials&nbsp;</li><li>Supports one <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=PAL3"><strong>PAL3</strong></a> autosampler&nbsp;</li></ul></li></ul></li><li><strong>Instrument dimensions&nbsp;</strong><ul><li><strong>Height:</strong> 49 cm (19.2 in)&nbsp;</li><li><strong>Width:</strong> 58 cm (22.9 in), 68 cm with side-mounted detector&nbsp;</li><li><strong>Depth</strong>: 54 cm (21.3 in)&nbsp;</li><li><strong>Typical weight</strong>: 51 kg (112 lb)</li></ul></li></ul><h3><strong>2. MDCW / Institut d’Investigació Sanitària Pere Virgili: GcDUO: A Batch Processing Framework Integrating PARAFAC and PARAFAC2 for GC×GC-MS Data Analysis</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/O_10_Llambrich_54914668f8.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>The presentation introduces <strong>GcDUO</strong>, an open-source batch-processing framework developed for the analysis of comprehensive two-dimensional gas chromatography–mass spectrometry (GC×GC-MS) data. The tool was designed to address one of the main challenges in GC×GC-MS workflows: extracting meaningful chemical information from highly complex multidimensional datasets while reducing dependence on proprietary software. GcDUO combines the strengths of <strong>PARAFAC</strong> and <strong>PARAFAC2</strong> chemometric algorithms to perform automated peak detection, deconvolution, compound annotation, and quantification across large batches of samples.</p><p>The workflow begins with raw GC×GC-MS data imported from CDF files and converted into a four-dimensional matrix. Regions of interest (ROIs) are automatically selected using a watershed algorithm, allowing relevant chromatographic features to be isolated from the background. PARAFAC decomposition is then applied to separate overlapping compounds into their individual first-dimension retention times, second-dimension retention times, and mass spectra. Compound identification is performed using spectral similarity calculations, retention index information, and comparison against reference libraries, creating a consensus-based annotation strategy that improves confidence in identifications.</p><p>To further improve quantitative performance, GcDUO incorporates a constrained PARAFAC2 approach that can model chromatographic peak shifts between samples while preserving accurate peak integration. The framework was evaluated using benchmark GC×GC datasets containing fragrances, allergens, food-related compounds, and breath-analysis samples. Validation studies showed strong detection and annotation performance, including successful identification of most compounds in independent datasets such as FruityBeer and BreathMix. Quantitative comparisons with the widely used <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/41"><strong>ChromaTOF software</strong></a> demonstrated highly comparable retention times and peak areas for a range of volatile compounds, indicating that GcDUO can deliver results similar to established commercial platforms.</p><p>The authors conclude that GcDUO provides a powerful open-source alternative for GC×GC-MS data processing. The framework supports automated deconvolution, annotation, and quantification without requiring strict trilinearity assumptions often associated with traditional chemometric approaches. Although computational cost and user expertise remain important considerations, GcDUO offers performance comparable to gold-standard commercial software while expanding access to advanced GC×GC-MS data analysis for metabolomics, environmental, food, fragrance, and other analytical applications. The software is freely available through GitHub, supporting broader adoption and further development by the scientific community.</p><h3><strong>3. Shimadzu: Discrimination of Coffee Bean Species Based on Aroma Compounds</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_01123_en_c8ac025ba9.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>Qualitative analysis of aroma compounds can be easily performed using the Smart Aroma Database.</li><li>Intuitive statistical analysis and exploration of characteristic compounds are possible using eMSTAT Solution.</li><li>The AOC -6000 multifunctional autosampler system enables the analysis of aroma compounds without sample pretreatment.</li></ul><p>Common coffee bean types are broadly classified into two types: Coffea arabica (Arabica) and Coffea canephora (Robusta). Among them, Arabica is superior in flavor and is highly favored as a specialty beverage. However, in recent years, there have been multiple reports of products sold claiming to be 100% Arabica while being adulterated with Robusta<sup>1)</sup>. A reported method for discriminating between the two is the analysis of lipophilic extracts of coffee beans using a benchtop NMR spectrometer<sup>1)</sup>. This method uses 16-O-Methylcafestol, which is present in Robusta but almost undetectable in Arabica, as a marker. However, it requires complicated pretreatment such as extraction and concentration.&nbsp;</p><p>Therefore, in this Application News, we investigated a method to discriminate between Arabica and Robusta more easily and rapidly using GC-MS/MS and the statistical analysis software eMSTAT Solution.</p><h5><strong>Sample and Analytical Methods&nbsp;</strong></h5><p>Commercially available coffee beans roasted at the same roastery were used as samples. Four brands of Arabica (Kilimanjaro, Brazil Bourbon, Mandheling G1, Brazil No.2 #18) and two brands of Robusta (Vietnam Robusta, Java Robusta) were prepared (Table 1). Each brand was individually crushed with a mill, and 1 g was weighed and sealed in a screw vial.</p><p>Volatile compounds were concentrated and introduced into the GC-MS using the HS-SPME method and then analyzed under the conditions registered in the GC-MS(/MS) Smart Aroma Database (Table 2). The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMSTQ8040+NX"><strong>GCMS-TQTM8040 NX</strong></a> and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=AOC-6000"><strong>AOC-6000 multifunctional autosampler</strong></a> system were used as the analytical instruments (Fig. 1). To verify whether rapid analysis is possible, a temperature ramp of 10˚C/min was adopted, and a low-polarity column was used to obtain stable retention times for each compound. Data acquisition was performed in Scan mode or MRM mode, and each sample was analyzed three times.</p><h4><strong>Exploration of Characteristic Aroma Compounds for Arabica and Robusta&nbsp;</strong></h4><p>Next, we investigated which compounds contribute to the discrimination between Arabica and Robusta. The PCA score plot (Fig. 4) reflects the differences in the tendencies of each group, with Arabica distributed on the left side and Robusta on the right side, clearly separated along the first principal component (PC1) axis. Referring to the corresponding loading plot, compounds located on the left side of the origin tend to have higher area values in Arabica, which is also positioned on the left in the score plot. On the other hand, compounds on the right side tend to show higher values in Robusta, which is located on the right in the score plot. In other words, the difference in the balance of these compoundsisthe main factorseparating the two groups. First, Arabica was commonly rich in compounds such as 5-Methyl furfural, Acetoin, and Furaneol acetate. MS chromatograms analyzed using LabSolutions Insight GCMS are shown in Fig. 7. In eMSTAT Solution, not only score plots and loading plots but also box plots can be easily drawn, making it possible to easily visualize and compare the distribution tendencies of each compound. From the box plots of the above compounds (Fig. 8), it was visually confirmed that all of them are contained in abundance in Arabica. These compounds are sometimes described as having a roasted or creamy quality, and it can be inferred that this result supports the characteristics of Arabica, which issuperior in aroma and acidity.&nbsp;</p><p>On the other hand, a compound found in abundance in Robusta was p-Vinylguaiacol. This compound is known to cause an offflavor similar to a medicinal odor in sake, and its content was low in Arabica. From this, it was suggested that p-Vinylguaiacol may be one of the compounds contributing to the bitterness and offtastes characteristic of Robusta.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>In this Application News, we investigated the discrimination of coffee bean types based on aroma compounds using the triple quadrupole gas chromatograph mass spectrometer <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMSTQ8040+NX"><strong>GCMSTQ8040 NX</strong></a> and the GC-MS(/MS) <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Smart+Aroma+Database"><strong>Smart Aroma Database</strong></a> for aroma analysis.&nbsp;</p><p>Four types of Arabica and two types of Robusta were analyzed as samples. Analysis using Scan data confirmed a tendency for the two types to separate. Subsequently, data was acquired in MRM mode, which offers higher sensitivity and selectivity, and detailed analysis was performed using the statistical analysis software eMSTAT Solution. As a result, the two groups were clearly separated in PCA and cluster analysis, demonstrating the effectiveness of discrimination by this method. Additionally, a discrimination model was developed and validated, confirming that highly accurate discrimination is possible.&nbsp;</p><p>From the above results, we conclude that the discrimination of coffee beans by aroma compound analysisis highly feasible using this method. Furthermore, this method enables a comprehensive workflow, from discrimination to the identification of characteristic compoundsfor each type.</p><h3><strong>4. Waters Corporation: Improvements to the Analysis of PBDEs in Environmental Matrices: Transitioning from EI Magnetic Sector to GC-APCI TQ MS/MS</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009372_7abfa9f0e9.pdf"><strong>Full PDF for download</strong></a></li></ul><p>This poster evaluates the transition of polybrominated diphenyl ether (PBDE) analysis in environmental samples from traditional electron ionization high-resolution magnetic sector GC-MS to a modern <strong>GC-APCI triple quadrupole MS/MS (GC-APCI TQ MS/MS)</strong> workflow. PBDE flame retardants are highly regulated due to their environmental persistence and potential health risks, making accurate and reliable analytical methods essential. The study investigated whether a GC-APCI MS/MS approach could match or exceed the performance of established GC-HRMS methods while offering greater flexibility and modernization opportunities.</p><p>The method was developed on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/554"><strong>Waters Xevo TQ Absolute mass spectrometer</strong> </a>equipped with APCI ionization and an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890"><strong>Agilent 8890 GC</strong></a>. A key innovation was the use of <strong>nitrogen as the carrier gas instead of helium</strong>, helping laboratories reduce dependence on helium supplies and mitigate increasing helium costs. By applying nitrogen flow ramping, the authors maintained chromatographic resolution and runtime comparable to the reference helium-based method without requiring changes in column dimensions. The approach also reduced the risk of thermal degradation of highly brominated compounds such as BDE 209 and achieved faster elution while preserving peak shape and separation quality.</p><p>For quantitative analysis, up to six MRM transitions per analyte were monitored, taking advantage of the characteristic isotope patterns of brominated compounds. The use of multiple transitions improved selectivity and sensitivity, while Waters waters_connect software enabled summation of MRM signals to enhance signal-to-noise ratios near detection limits. Excellent calibration performance was achieved across more than three orders of magnitude, with correlation coefficients above 0.999 for all analytes. Internal standards and recovery standards demonstrated strong reproducibility, and quality control samples showed precision typically below 15% RSD and acceptable accuracy across low, medium, and high concentration levels.</p><p>The authors conclude that an all-nitrogen GC-APCI TQ MS/MS configuration can successfully meet the performance criteria established for PBDE analysis by reference EI GC-HRMS methods. The workflow maintains critical chromatographic separations, delivers accurate quantitative results, and offers a platform that could potentially combine PBDE determination with other halogenated flame retardants in a single analytical method. These findings demonstrate that GC-APCI TQ MS/MS represents a robust and practical modernization strategy for environmental PBDE analysis.</p></div></div></div></div></div></div></section></div></div></div></div></div></div></section>

News from LabRulezGCMS Library - Week 25, 2026

<p><strong>This study presents an optimized dispersive liquid–liquid microextraction (DLLME) method coupled with GC-FID for the determination of eight priority polycyclic aromatic hydrocarbons in surface waters. Experimental design approaches, including fractional factorial and Box–Behnken designs, were used to optimize extraction conditions and maximize analytical performance.</strong></p><p>The validated method achieved rapid chromatographic separation, low detection limits, good precision, and high enrichment factors while maintaining favorable green analytical characteristics. Successful application to wastewater, lake, river, and drain water samples demonstrates its suitability for routine environmental monitoring of PAHs.</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.6c01489"><strong>Experimental Design-Based Dispersive Liquid–Liquid Microextraction with GC-FID for Determination of Polycyclic Aromatic Hydrocarbons in Surface Water</strong></a></h4><p>Chen Minghong, Song Peiyu, Tien Ping Lee, Garret Chan Zhe Ming, Philip J. Marriott, and Yong Foo Wong*</p><p>ACS Omega 2026, 11, 21, 31418–31431</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsomega.6c01489">https://doi.org/10.1021/acsomega.6c01489</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><div><p>Polycyclic aromatic hydrocarbons (PAHs) are organic pollutants containing two or more fused benzene rings and are widely associated with carcinogenic, teratogenic, and mutagenic properties. <a href="javascript:void(0);">(1)</a> These hydrophobic substances can bioaccumulate with long environmental half-lives and are classified as high priority ecotoxicants of the first danger class. <a href="javascript:void(0);">(1,2)</a> Anthropogenic activities (e.g., fossil fuel combustion, industrial processes, biomass burning, and others) are predominantly recognized as the primary sources of PAHs in most environmental compartments. <a href="javascript:void(0);">(3−6)</a> In the present work, the hydrophobic nature of PAHs facilitates adsorption onto suspended particulate matter and organic material in aquatic systems, followed by deposition into underlying sediments. <a href="javascript:void(0);">(7)</a> These persistent organic pollutants have been reported in surface waters as well as estuarine and coastal environments and can potentially disrupt ecosystem functioning. <a href="javascript:void(0);">(7,8)</a></p><p>From a public health perspective, PAHs exposure via upon ingestion, has been linked to a spectrum of adverse health effects such as cancer and reduced fertility. <a href="javascript:void(0);">(2,9)</a> Sixteen unsubstituted PAHs have been designated as priority pollutants by the United States Environmental Protection Agency (USEPA). <a href="javascript:void(0);">(10)</a> The International Agency for Research on Cancer (IARC) has classified benzo(a)pyrene (BaP) in Group 1 (carcinogen to humans) and other PAHs in Group 2A (possible human carcinogens). <a href="javascript:void(0);">(10,11)</a> The maximum permissible concentrations of benzo(a)pyrene (0.00001 mg/L) in water intended for drinking water is regulated by the European Union (EU). The EU limits the total content of polyaromatic compounds in drinking water to &lt;0.1 μg/L. <a href="javascript:void(0);">(12)</a> In heavily polluted waterways, PAH concentrations have been reported to reach 10 μg/mL. <a href="javascript:void(0);">(13)</a> Epidemiological evidence also suggests a positive relationship between increased cancer incidence in human populations that are having high exposure to organic ecotoxins. <a href="javascript:void(0);">(14)</a> For these reasons, quantitative assessments of PAH occurrence and distribution in surface waters remain important and fertile research topics. <a href="javascript:void(0);">(15,16)</a></p><p>PAHs in water and environmental matrices are routinely analyzed using either gas chromatography (GC) and/or liquid chromatography (LC) with various detection modalities. <a href="javascript:void(0);">(17,18)</a> The coupling of chromatography to mass spectrometry has been the preferred technique, owing to the distinct selectivity and sensitivity, particularly when operated in selected ion monitoring (SIM) or multiple reaction monitoring (SRM) modes. <a href="javascript:void(0);">(19)</a> Additionally, LC coupled with fluorescence detection is also extensively utilized for PAH analysis. <a href="javascript:void(0);">(20,21)</a> As PAHs typically occur at trace to ultratrace levels in complex real-world matrices, sample pretreatment and/or preconcentration is generally required prior to instrumental analysis. <a href="javascript:void(0);">(22,23)</a> Conventional approaches such as liquid–liquid extraction and solid-phase extraction are widely used but are often solvent-intensive and laborious and generate substantial hazardous waste. More recently, microextraction techniques (e.g., dispersive microsolid phase extraction, dispersive liquid–liquid microextraction (DLLME), solid phase microextraction, etc.) have emerged as attractive alternatives, providing advantages such as speed and simplicity and requiring substantially lower volumes of hazardous solvents. <a href="javascript:void(0);">(24−26)</a></p><p>DLLME has shown good efficiency for extracting and preconcentrating hydrophobic PAHs from aqueous matrixes. <a href="javascript:void(0);">(24,27)</a> Briefly, DLLME involves rapid injection of a small volume of an extraction solvent (immiscible with water) and dispersive solvent into the aqueous sample. <a href="javascript:void(0);">(24)</a> Target analytes partition into the microdroplets and are subsequently recovered in a minimal volume of the organic phase after centrifugation. The large interfacial contact area between the two phases enhances mass transfer, leading to fast attainment of extraction equilibrium with high enrichment factors. <a href="javascript:void(0);">(28,29)</a> DLLME has been applied to a wide range of matrices, including environmental samples, <a href="javascript:void(0);">(25,30)</a> milk and dairy products, <a href="javascript:void(0);">(31)</a> honey, <a href="javascript:void(0);">(32)</a> and others. <a href="javascript:void(0);">(33)</a> Optimization of DLLME conditions for targeted solutes is often performed using a one-factor-at-a-time approach, which is time-consuming, labor-intensive, and may inadequately take into account interaction between or among variables. <a href="javascript:void(0);">(34)</a> In contrast, multivariate experimental design methodologies accommodate simultaneous variation of multiple extraction variables, facilitating identification of interaction effects and development of statistically robust models. <a href="javascript:void(0);">(35−37)</a></p><p>Over the past decade, multivariate design of experiments (DOE) has become an important optimization strategy for process development. Compared with traditional one-factor-at-a-time approaches, DOE can reduce time, effort, and resource consumption while extracting meaningful information from a relatively small number of experimental analyses. <a href="javascript:void(0);">(37−40)</a> Among the DOE frameworks, the Box-Behnken design (BBD), an economical variant of response surface methodology, has been widely used for process optimization, offering high statistical efficiency and good predictive performance when tuning experimental variables in analytical and industrial applications. <a href="javascript:void(0);">(35,39,41−45)</a> This study evaluates the applicability of using RSM to optimize DLLME conditions for selective extraction and preconcentration of acenaphthene, fluorene, anthracene, phenanthrene, fluoranthene, pyrene, benzo(a)anthracene, and benzo(a)pyrene. A fractional factorial design (FrFD) was initially used to screen and identify statistically significant DLLME variables. The selected factors were then optimized using the BBD to construct quadratic models and generate response surface plots for determining optimal extraction conditions. The optimized DLLME-GC-FID method was validated, and AGREEprep and AGREE were used to quantify ‘greenness’ metric scores. Analytical practicability of the validated method was demonstrated by determining the targeted PAHs in several surface water samples.</p><h4><strong>2. Experimental Section</strong></h4><h5><strong>2.4. GC-FID Analysis</strong></h5><p>All experiments were performed using an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890B"><strong>Agilent 7890B GC system</strong></a> equipped with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7693A"><strong>G4513A autosampler</strong></a> and a split–splitless inlet (Agilent Technologies; Santa Clara, CA, USA). Chromatographic separation was effected by using a <strong>DB-5HT column</strong> (Agilent Technologies, Santa Clara, CA, USA; 30 m × 0.25 mm I.D. × 0.25 μm film thickness). Injection mode and oven temperature programming were optimized to achieve baseline separation of all target PAHs. Helium (99.999%) was used as the carrier gas at a constant flow rate of 1 mL/min. Splitless mode with a splitless time of 2.1 min was used, with a 1 μL injection volume. The injector temperature was maintained at 300 °C. The oven temperature program was 70 °C (hold for 3.3 min) and ramped to 300 °C (hold 5 min) at a rate of 25 °C/min. The FID temperature was set to 300 °C.</p><h4><strong>3. Results and Discussion</strong></h4><p>The initial GC-FID conditions were adopted from Hor et al. for the determination of BAP, BAA, BBF, and chrysene in tocotrienol concentrates. <a href="javascript:void(0);">(52)</a> Under those chromatographic conditions, baseline separation of all the targeted PAHs could not be achieved (Flt, Pyr, BaA, and BaP). Hence, GC conditions, particularly the oven temperature program, were briefly optimized to obtain baseline separation of all the targeted PAHs (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.6c01489#fig1">Figure 1</a>A).</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2026_11_21_31418_31431_Figure_1_Chromatograms_of_Ai_standard_mixture_265d7e1014.jpeg" alt="ACS Omega 2026, 11, 21, 31418–31431: Figure 1. Chromatograms of (Ai) standard mixture (100 μg/L) before DLLME; (Aii) standard mixture (100 μg/L) after DLLME; (B) lake water sample spiked with PAHs (10 μg/L); and (C) wastewater sample. 1, Ace; 2, Flu; 3, Ant; 4, Phe; 5, Flt; 6, Pyr; 7, BaA; 8, BaP." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2026_11_21_31418_31431_Figure_1_Chromatograms_of_Ai_standard_mixture_265d7e1014.jpeg 234w," sizes="100vw" width="2100" height="1402"></p><h5><strong>3.1. Evaluation of the Type of Extractants and Dispersants for DLLME</strong></h5><p>Extraction performance in DLLME is strongly influenced by the choice of extraction solvent (i.e., that which is sedimented), which controls the solutes’ partitioning behavior between the aqueous and organic phases. <a href="javascript:void(0);">(24)</a> Five extraction solvents of different polarity, namely, dichloromethane (DCM, dielectric constant (ε): 8.93 <a href="javascript:void(0);">(53)</a>), chloroform (ε: 4.81 <a href="javascript:void(0);">(54)</a>), carbon tetrachloride (ε: 2.24 <a href="javascript:void(0);">(55)</a>), chlorobenzene (ε: 5.62 <a href="javascript:void(0);">(56)</a>), and cyclohexane (ε: 2.02 <a href="javascript:void(0);">(57)</a>), were evaluated. Based on the overall response (i.e., peak areas), dichloromethane outperformed the other chlorinated solvents (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.6c01489#fig2">Figure 2</a>). This might be attributed to the stronger partitioning of PAHs into DCM, which exhibited the highest polarity among the tested extractants. <a href="javascript:void(0);">(58)</a> Therefore, DCM was selected as the extraction solvent. It is known that the dispersive solvent serves as a “bridge” between the aqueous sample and the water-immiscible extractant, and its selection is therefore crucial to DLLME performance. Five dispersive solvents (methanol, ε: 33; <a href="javascript:void(0);">(59)</a> ethanol, ε: 24.5; <a href="javascript:void(0);">(60)</a> isopropanol, ε: 20.1; <a href="javascript:void(0);">(61)</a> acetone, ε: 20.7; <a href="javascript:void(0);">(62)</a> acetonitrile, ε: 36 <a href="javascript:void(0);">(63)</a>) of different polarities were studied. Among these, ACN having the highest polarity provided the highest extraction response. This might be attributed to the reduced interfacial tension, which promotes formation of smaller microdroplets, and increases interfacial area for partitioning process, thereby improving extraction efficiency. <a href="javascript:void(0);">(64)</a> Thus, DCM and ACN were selected as the extractant and dispersant, respectively, for subsequent FrFD and BBD experiments.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2026_11_21_31418_31431_Figure_2_Effect_of_A_selection_of_extraction_solvent_B_selection_of_dispersive_solvent_5abd279b17.jpeg" alt="ACS Omega 2026, 11, 21, 31418–31431: Figure 2. Effect of (A) selection of extraction solvent; (B) selection of dispersive solvent." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2026_11_21_31418_31431_Figure_2_Effect_of_A_selection_of_extraction_solvent_B_selection_of_dispersive_solvent_5abd279b17.jpeg 135w," sizes="100vw" width="1000" height="1154"></p><h4><strong>4. Conclusion</strong></h4><p>An improved and environmentally friendly DLLME-GC-FID method was described for the quantitative analysis of PAHs in surface water. RSM was applied by first screening influential variables using a fractional factorial design, followed by the Box-Behnken design optimization of the DLLME parameters. In contrast to single-factor experimentation, the fitted model and 3D response surface plots showed factor interactions and their combined effects on extraction performance, facilitating near-optimal conditions to be identified with a limited number of experiments. Using the optimized conditions, low detection limits, good enrichment factors, acceptable reproducibility, and recoveries were achieved. The validated analytical features indicate that the proposed method is robust and cost-effective for the routine screening of PAHs in terrestrial water bodies.</p></div>

Experimental Design-Based Dispersive Liquid–Liquid Microextraction with GC-FID for Determination of Polycyclic Aromatic Hydrocarbons in Surface Water

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 3rd 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>and<strong> Shimadzu </strong>and presentation by<strong> MDCW / University of Alberta!</strong></p><h3><strong>1. Agilent Technologies: Analysis of Trace Impurities in Monocyclic Aromatic Solvents Following ASTM D7504</strong></h3><p><strong>Dual simultaneous analysis using the Agilent 8860B gas chromatograph</strong></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_trace_impurity_aromatic_solvents_analysis_astm_d7504_8860_gc_5994_9316en_agilent_c9fa6868e6.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>The production of high-purity monocyclic aromatic hydrocarbons, such as benzene, toluene, ethylbenzene, and xylenes (BTEX), is a cornerstone of the modern petrochemical industry. These compounds serve as essential feedstocks for the synthesis of plastics, resins, and textiles. Because even trace impurities can adversely affect downstream chemical reactions and product quality, rigorous analytical testing is required to ensure these intermediates meet strict commercial specifications.&nbsp;</p><p>ASTM D7504 is the industry-standard test method for determining the purity of, and trace impurities in, monocyclic aromatic hydrocarbons using gas chromatography (GC) with flame ionization detector (FID).1 This method is favored for its streamlined workflow; it utilizes effective carbon number (ECN) correction factors for area normalization. This eliminates the need for labor-intensive, multipoint calibrations for every individual impurity, allowing laboratories to calculate purity and quantify trace nonaromatics and aromatics with high precision.&nbsp;</p><p>The application scope of ASTM D7504 covers a wide array of aromatic liquids, including benzene, toluene, mixed xylenes, and styrene. To comply with the method's stringent performance requirements, the GC system must&nbsp;demonstrate:&nbsp;</p><ul><li><strong>High sensitivity: </strong>A limit of quantitation (LOQ) of at least 0.0006% by mass.</li><li><strong>Good resolution: </strong>Maintaining a valley-to-peak ratio of no more than 50% for critical separations (such as p-xylene and m-xylene).&nbsp;</li><li><strong>Strict precision: </strong>Highly reproducible peak areas to ensure accurate purity calculations.</li></ul><p>Implementing ASTM D7504 on a dual-channel GC/FID platform—where two independent analytical channels configured with identical injectors, columns, and detectors operate within a single GC oven—provides significant operational advantages:&nbsp;</p><ol><li>Enhanced laboratory throughput: By performing two injections simultaneously, the test lab can double its sample capacity per instrument, effectively reducing the cost-per-analysis and maximizing hardware ROI.&nbsp;</li><li>Method flexibility and redundancy: A dual-channel set up allows a lab to run different sample types (such as toluene on the front channel and xylene on the back) in a single oven cycle. Furthermore, it provides an immediate "back up" channel to maintain uptime during routine&nbsp;maintenance.&nbsp;</li></ol><p>For the system to be considered reliable, both channels should meet ASTM D7504 sensitivity, resolution, and precision requirements. In addition, both channels should yield consistent quantitative results for the same sample. The reproducibility limit (R) demonstrated in ASTM D7504 interlaboratory testing will be used to evaluate the result consistency between the two channels.</p><p>ASTM D7504 recommends helium and hydrogen as carrier gas. In China, major Chinese petrochemical companies often align their internal quality control standards directly with ASTM D7504 when testing for export of high-purity chemical intermediates. Because nitrogen is commonly used in China, they commonly adapt the ASTM D7504 method to use nitrogen carrier gas.&nbsp;</p><p>This application note demonstrates how dual-channel analysis on the Agilent 8860B GC, following ASTM D7504, delivers consistent and high-precision data using three types of carrier gas.</p><h4><strong>Experimental</strong></h4><p>An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8860B"><strong>Agilent 8860B GC</strong></a><strong> </strong>was configured with dual split/splitless inlets and dual flame ionization detectors (FIDs). The sample introduction was made by dual <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7693A"><strong>Agilent 7693A automatic liquid samplers (ALS)</strong></a> with high density turrets (16-vial). The analytical parameters and consumables are summarized in Tables 1 and 2. Data acquisition and analysis were conducted using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=OpenLab+CDS"><strong>Agilent OpenLab CDS version 2.8</strong></a></p><h4><strong>Conclusion&nbsp;</strong></h4><p>The Agilent 8860B gas chromatography system configured with two identical analytical channels are applied for impurity analysis in monocyclic aromatic solvents using three carrier gases. Each analytical channel was evaluated according to the ASTM D7504 method in terms of resolution, sensitivity, quantitation precision, and recovery with satisfactory results. The quantitation results between the two channels are consistent with each other.&nbsp;</p><ul><li>Column resolution compounds pair demonstrated good separation with H/V no less than 5:1 for 300 ppm m-xylene and p-xylene solvent.&nbsp;</li><li>The LODs achieved for benzene on each analytical channel are less than 0.0001%, exceeding the 0.0002% LOD required by ASTM D7504.&nbsp;</li><li>The response and mass concentration precisions of most impurities in check standards are below 1%, meeting or exceeding the precision requirements in D7504.&nbsp;</li><li>Excellent recovery results, ranging from 93 to 105%, was achieved for added impurities, indicating good quantification accuracy based on the 8860B GC system.&nbsp;</li><li>The quantitation difference of all probe impurities between two channels is less than the reproducibility thresholds (R), demonstrating excellent across channel consistency</li></ul><p>Besides great instrument performance, the Agilent OpenLab CDS software can realize ECN based normalization for easy and fast quantitation and report generation. The 8860B dual channel GC system coupled with the OpenLab CDS software provides an accurate and reliable analysis of impurities in monocyclic aromatic solvents with satisfactory precision. Lab productivity can be improved significantly compared to the single channel analytical system.</p><h3><strong>2. MDCW / University of Alberta: Leveraging Local Libraries for Positively Parsimonious Peak Tables</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/O_6_Harynuk_f005bdafaf.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>James J. Harynuk’s presentation, <strong>“Leveraging Local Libraries for Positively Parsimonious Peak Tables,”</strong> explores how custom mass spectral libraries can simplify and improve compound identification in complex GC×GC-(HR)MS datasets. GC×GC-MS is widely applied in petroleum, environmental, food/flavour, and omics research, where samples can contain hundreds or thousands of peaks. While expanded separation space, cleaner spectra, retention patterns, and high-resolution accurate-mass data provide strong identification capabilities, converting large datasets into coherent peak tables with consistent compound assignments across multiple samples remains challenging.</p><p>The presentation demonstrates the approach using a field pea study investigating how nitrogen availability influences plant metabolism and volatile organic compounds. A conventional workflow based on peak finding and library searching can generate very large peak tables and inconsistent assignments. Incorporating retention indices (RI) and LECO’s Identification Grading System (IGS) substantially reduces the number of questionable peaks. In one example, a pea sample containing <strong>789 detected peaks was reduced to 146 retained peaks</strong> after RI filtering and IGS scoring, producing a much more manageable dataset. However, conventional libraries still struggle with isomers and with compounds that repeatedly occur in a laboratory’s samples but cannot yet be confidently identified—the presentation calls these <strong>“unknown knowns.”</strong></p><p>Harynuk therefore proposes building a <strong>custom local HRMS library</strong> containing not only standards and confidently identified compounds, but also reproducible unknown features. To qualify for inclusion, a peak should have a high-quality spectrum, S/N &gt;100, chromatographic purity, occurrence in multiple technical replicates, an assigned retention index, and a unique identifier. Crucially, the exact chemical identity does not need to be known: an unknown but reproducible feature can receive an internal identifier such as “JJH-001” and be updated later as more information becomes available. This allows laboratories to retain analytically meaningful recurring signals instead of discarding them simply because a definitive library identification is unavailable.</p><p>The results show that combining a custom library with local RI data and IGS filtering improves both the consistency and efficiency of peak-table generation. Compounds with IGS scores ≥3.0 were generally assigned the same identification across samples when the custom library was used, while reliance on NIST and IGS alone produced less consistent results. After correcting only a small number of problematic identifications per peak table, retention-index errors for custom-library entries dropped dramatically—in the evaluated samples, typically to around <strong>0.5–1.9 RI units</strong>. The key recommendation is therefore straightforward: <strong>build a custom MS library, include recurring “unknown knowns,” collect local retention-index data, and apply identification-quality filters</strong> to obtain cleaner and more consistent GC×GC-MS peak tables with substantially less manual effort.</p><h3><strong>3. Shimadzu: Simultaneous Analysis of Pesticide Residues in Food Using Triple Quadrupole GC-MS/MS with SPL Mode of a Multimode injection Unit (MMI)</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_01234_en_d8cff47c74.pdf"><strong>Full PDF for download</strong></a></li></ul><h4><strong>User benefits</strong></h4><ul><li>The MMI’s rapid heating and cooling technology significantly reduces waiting time during inlet maintenance, improving instrument uptime.&nbsp;</li><li>The Smart Pesticides Database enables automatic creation of analytical methods without the need for pesticide standards.&nbsp;</li><li>Peakintelligence for GCMS uses AI-based peak processing to deliver highly accurate analysis with no parameter settings required</li></ul><p>GC-MS/MS is an indispensable tool for the simultaneous analysis of pesticide residues in food. However, improving productivity in high-throughput workflows remains a persistent challenge. With the increasing use of simplified sample preparation methods such as QuEChERS, contamination of the inlet by matrix components is unavoidable, and frequent inlet maintenance, including liner replacement, is often required. Because this maintenance involves both cooling the inlet and waiting for temperature re-stabilization afterward, it can become a major source of instrument downtime.&nbsp;</p><p>The newly developed Multi-Mode Inlet (MMI) incorporates Shimadzu’s proprietary thermal insulation technology, providing excellent temperature stability together with rapid heating and cooling performance. While maintaining high data compatibility with conventional split/splitless inlets, the MMI significantly reduces the waiting time associated with inlet maintenance.</p><p>In this Application News, simultaneous multiresidue analysis in SPL mode is demonstrated for four food matrices with different characteristics - spinach, orange, avocado, and ginger - using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ+8040+RX"><strong>GCMS-TQ 8040 RX triple quadrupole</strong> </a>GC-MS/MS equipped with the MMI.</p><h4><strong>Data Analysis&nbsp;</strong></h4><p>LabSolutions Insight, a quantitative data processing software package designed for high-throughput sample analysis, was used for data analysis, with Peakintelligence for GCMS applied as the peak integration algorithm (Fig. 6). Peakintelligence is an AI-based waveform processing algorithm that uses machine learning to emulate the peak processing performed by experienced analysts. It requires no operator-defined parameter settings and provides peak integration performance comparable to that of skilled users.&nbsp;</p><p>For more information on improving the efficiency of pesticide data analysis using Peakintelligence for GCMS, please refer to Application News 01-00585-EN, “<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00585_en_7e311a3c77/an_01-00585-en.pdf"><strong>Time-Saving Data Processing for Pesticide Residues with Peakintelligence for GCMS</strong></a>.”</p><h4><strong>Conclusion&nbsp;</strong></h4><p>In this Application News, an example of simultaneous multiresidue pesticide analysis in food using a triple quadrupole GC-MS/MS equipped with a Multi-Mode Inlet (MMI) was presented. By adopting the MMI, instrument downtime associated with inlet maintenance can be significantly reduced while maintaining high quantitative performance. In addition, by combining automated method creation with the Smart Pesticides Database and efficient data analysis using the AIbased waveform processing algorithm Peakintelligence for GCMS, highly accurate results were obtained even for complex food matrices. This system optimizes the overall analytical workflow, from method development and maintenance to data analysis, and can make a substantial contribution to improving productivity in high-throughput pesticide residue analysis.</p></div></div></div></div></div></div></section></div></div></div></div></div></div></section>

News from LabRulezGCMS Library - Week 32, 2026

Article

Product

Events

Webinars

Application

Academy

Video

Poster

Scientists

Plastics

Environment

Food

Water

Health

Presentation

Scientific article

Interview

Toxicology

Popularization

Science and research

Software

Covid-19

Career

Laboratories

Various

Zaměření

Type of News

Focus

Everything from the world of analytical chemistry in one place. We connect people in solving their problems. At Labrulez you will find all the necessary information easily, quickly and clearly. Stop searching and start finding.

LabRulez

Agilent Innovation Tour 2026

LECO at IMSC 2026

Restek at IMSC 2026

From Spectra to Mechanism: Using DRIFTS to Understand CO₂ Catalysis

Safer Narcotics Identification in the Fentanyl Era: Lessons from Rhode Island State Police

Verifying Raw Materials with a Handheld Instrument