Analysis of Fentanyl and Fentanyl Analogs Using Atmospheric Pressure Chemical Ionization Gas Chromatography–Mass Spectrometry (APCI-GC-MS)

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 10th February 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applications and other documents by Shimadzu, Agilent Technologies and Thermo Fisher Scientific!<h4>1. Agilent Technologies: Analysis of Aldehydes, Benzene, and Limonene in Recycled Polyethylene&nbsp;Terephthalate&nbsp;</h4>Using an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=Agilent+7697">Agilent 7697</a> headspace sampler and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?instrumentationItems=3-14&amp;manufacturerItems=1&amp;search=8890+5977">8890/5977C GC/MSD</a><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_aldehyde_benzene_limonene_pet_7697_headspace_8890_5994_8063en_agilent_1_af1ee904b7.pdf">Full PDF for download</a></li></ul>PET is commonly used in the food and beverage industry, as it is easy to recycle. The quantity of food containers and beverage bottles made from recycled PET materials is on the rise.&nbsp;Contaminants in recycled PET, including acetaldehyde, benzene, and limonene, can migrate from the packaging into the contents, potentially affecting the safety and quality of the products stored inside.1 Monitoring these contaminants is crucial for ensuring the quality of recycled PET products, as they can affect the physical, chemical, and sensory properties of recycled PET, potentially leading to product defects or health concerns.&nbsp;This application note demonstrates the use of a 7697 headspace sampler and 8890/5977C GC/MSD for the analysis of acetaldehyde, benzene, and d-limonene in recycled PET materials. With the developed method, acetaldehyde, benzene, and d-limonene in three recycled PET samples were successfully quantified.&nbsp;<h4>Conclusion</h4>This application note describes the quantitative analysis of acetaldehyde, benzene, and d-limonene using an Agilent 8890/5977C GC/MSD with an Agilent 7697 headspace sampler. This method offers the advantages of full automation, rapid analysis, and minimum sample preparation. With this automated workflow solution, excellent sensitivity was demonstrated with an LOD of 0.034 ng/µL for acetaldehyde, 0.002 ng/µL for benzene, and 0.006 ng/µL for d-limonene. Good linearity was demonstrated, with R2 above 0.999 for all three compounds over wide concentration ranges. Three recycled PET samples were analyzed, with a detection of acetaldehyde from 474 to 975 μg/kg, benzene from 5.5 to 18.6 μg/kg, and d-limonene from 0.42 to 3.21 μg/kg.&nbsp;<h4>2. Shimadzu: GC/MS Analysis of Fluorophosphates as Decomposition Products in Lithium Battery Electrolyte</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_05_sca_280_105_en_d3dcd7b97d.pdf">Full PDF for download</a></li></ul>User Benefits:<ul><li>A routine and fast GC/MS method for detection of LIB decomposition products.</li><li>Monitoring of the LIB electrolyte after manufacturing, storage and transport.</li><li>Fluorophosphates can be considered as markers for a started electrolyte decomposition.</li></ul>The electrolyte solution is a crucial part of a typical Lithium-ion battery, consisting Li salt (f.e. LiPF6), organic carbonates and additives to ensure a stable transport of Li ions during charging and discharging processes. A significant part of battery aging can be considered as a result of the decomposition of the electrolyte. At the end of this chemical and electrochemical processes oligomeric organic compounds 1) and organophosphates 2,3) could be detected. Especially fluor containing organophosphates are of interest due to their potential neurotoxicity 4,5,6).While the electrochemical aging takes place in a battery itself, the chemical aging starts already during manufacturing, storage and transport of the electrolyte. Typical factors that influence this are: exposure to air and moisture, too high temperature at manufacturing/storage, long term storage in general. Wrong materials in the production pipeline like glass are problematic as well due to a catalytic reaction of the fluoric acid traces with SiO2 as follows:&nbsp;SiO2 + 6HF → H2[SiF6] +2H2OThis application examples of analysis of the electrolyte solution for qualitative determination of fluorophosphates as a possibility for an earlystage quality control.<h5>Experimental</h5>25 µl LIB electrolyte consisting Ethyl methyl carbonate and Ethylene carbonate 1:1 with 1M LiPF6 has been diluted with 1 mL dichloromethane and centrifuged for 5 min at 8500 rpm to remove the solid LiPF6. The centrifuged solution was transferred into a 2 mL GC glass vial and measured by <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-QP2020+NX">GCMS-QP2020 NX</a>.<h5>Conclusion</h5>LiPF6 based LIB electrolyte degrade during chemical and electrochemical processes. With GC/MS based analysis method a clear assignment of tree fluorinated alkyl phosphates has been successfully accomplished in a long-term stored electrolyte showing the suitability of GCMS-QP 2020 NX to offer a reliable and simple way of analysis even at early stages of electrolyte decomposition.<h4>3. Thermo Fisher Scientific: Enhanced calibration precision: Leveraging RSE and WLS for optimal function optimization</h4><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/TN_003551_Enhanced_calibration_precision_Leveraging_RSE_and_WLS_for_optimal_function_optimization_184ab5a2c1.pdf">Full PDF for download</a></li></ul>This technical note outlines the advantages of employing relative standard error (RSE), weighted least squares (WLS) approximations, and inverse calibrations in enhancing the accuracy and precision of calibration in chromatographic analysis. It discusses the shortcomings of conventional metrics and introduces a more dependable and straightforward method for evaluating and optimizing calibration processes.<h5>Software</h5>Data evaluation was performed using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=2&amp;search=chromeleon">Thermo Scientific™ Chromeleon™</a> Chromatography Data System (CDS) version 7.3.2. The software's RSE definition (Equation 4) includes weighting factors, expanding its use to calibration functions that must pass through the origin.5<h5>Results and Discussion</h5>We included a gas chromatographic (GC) example to demonstrate the universal applicability of RSE in evaluating chromatographic calibration experiments. Figure 7 shows the separation of ethanol, which takes about 40 seconds after a headspace injection. The calibrated concentration range spans from 100 mg/L to 5,000 mg/L, the broadest range in our examples.&nbsp;We subjected the original method to RSE evaluation using OLS that constrained the calibration function to pass through the origin (Figure 7A). The RSE obtained was 7.6%, which is well within the EPA guideline of less than 20%. However, the relative amount deviation plot in Figure 7A showed increasing deviation at lower standard concentrations.&nbsp;The original calibration data set was re-analyzed using WLS with a quadratic fit and 1/Amount² weighting to enhance precision. This adjustment reduced the RSE to approximately 0.7%. It produced a relative amount deviation plot in Figure 7B that displayed minor deviations and a random scatter around the target value of 0% across the calibrated range. This demonstrates the improved accuracy and reliability of the optimized calibration method.<h5>Conclusion</h5>This technical note explores the advantages of using RSE, WLS approximations, and inverted calibrations to enhance calibration quality in chromatography. By optimizing calibration curves through quadratic fitting, offset adjustments, and suitable weighting factors (such as 1/Amount²), the calibration process can be significantly improved, resulting in lower RSEs and better overall calibration quality. Incorporating RSE as an evaluation tool offers a deeper understanding of calibration reliability.

News from LabRulezGCMS Library - Week 7, 2025

This study investigates the thermal stability of polar compounds in crude oils using ultra-high-resolution FT–MS with electrospray ionization (ESI). By monitoring the MS profiles of 14 key compounds subjected to micropyrolysis at temperatures up to 500 °C, we aim to better understand their thermal behavior.A new "MS ratio" is introduced, based on ion abundance changes during thermal modification, and is compared to established GC–MS diagnostic ratios. The results demonstrate a correlation between the proposed MS ratio and classical thermal evolution indicators, providing a new approach for assessing crude oil maturity.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.energyfuels.4c03496">Exploratory Analysis of Crude Oil Thermal Evolution by Ultra-High-Resolution Mass Spectrometry</a></h4>Arquimedes M. S. Coutinho, Marília Gabriela A. Pereira, Pedro G. C. Lucena, Jhonnatas de C. Carregosa, Wenes R. da Silva, Danielle M. M. Franco, Gesiane da S. Lima, Boniek G. Vaz, Alberto Wisniewski and Jandyson M. SantosEnergy Fuels 2024, 38, 22, 21932–21940<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acs.energyfuels.4c03496">https://doi.org/10.1021/acs.energyfuels.4c03496</a><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/">CC-BY 4.0</a></h6></blockquote>The chemical characterization of oils can be performed on the basis of the identification of biomarkers, which are compounds that allow inferences to be made concerning the geochemical features of oils, such as the type of original organic matter, the degree of thermal evolution, and the environmental origin. <a href="javascript:void(0);" aria-label="reference 3">(3)</a> Gas chromatography coupled with mass spectrometry (GC–MS) is the most common analytical technique used to identify biomarkers, enabling the calculation of diagnostic ratios to infer the degree of thermal evolution of the oil. <a href="javascript:void(0);" aria-label="reference 2 and 3">(2,3)</a> Additionally, the use of gas chromatography with flame ionization detection (GC–FID) is notable for its versatility and excellent response to hydrocarbons. Another valuable technique is comprehensive two-dimensional gas chromatography (GC × GC), which serves as an important tool for addressing coelution problems, a phenomenon commonly observed in the chromatographic analysis of oils. <a href="javascript:void(0);" aria-label="reference 4 and 5">(4,5)</a> The thermal evolution of an oil is a geochemical parameter that is related to its thermodynamic stability and depends upon the thermal stages in which it was formed as well as the temperature levels of its formation process. <a href="javascript:void(0);" aria-label="reference 2">(2)</a> The biomarker ratios most commonly used to evaluate thermal evolution are Ts/Tm, Ts/(Ts + Tm), and C32S/(S + R). <a href="javascript:void(0);" aria-label="reference 2 and 6 to 8">(2,6−8)</a> The compound 18α-22,28,30-trisnorneohopane (Ts) is more stable than 17α-22,29,30-trisnorhopane (Tm) at high temperatures; therefore, the Ts/Tm and Ts/(Ts + Tm) ratios increase with increasing degree of thermal evolution. <a href="javascript:void(0);" aria-label="reference 2 and 9">(2,9)</a> The same behavior occurs for the C32S/(S + R) ratio based on the ratio between the 17α(H),21β(H)-homohopane C32H56 isomers, involving conversion of the 22R isomer in the mixture of R and S isomers. <a href="javascript:void(0);" aria-label="reference 2 and 7">(2,7)</a>The thermal behavior of oils can be evaluated by pyrolysis, where thermal decomposition reactions of the material occur in an inert environment, with the resulting compounds being characterized and related to the original molecule. <a href="javascript:void(0);" aria-label="reference 10">(10)</a>Gas chromatography–mass spectrometry (GC–MS) is widely recognized as a fundamental technique for the analysis of hydrocarbon biomarkers of petroleum. Its significance is particularly evident in the separation of isomeric biomarkers, such as the previously mentioned Ts and Tm, allowing the determination of diagnostic ratios with high potential for inferring petroleum geochemical information. <a href="javascript:void(0);" aria-label="reference 11 and 12">(11,12)</a> Alternatively, ultra-high-resolution Fourier transform mass spectrometry (FT–MS) allows analysis to be performed by direct infusion of a simple oil solution into an electrospray ionization (ESI) source coupled to a mass analyzer, such as ion cyclotron resonance (ICR MS) or Orbitrap (Orbitrap MS) devices, enabling the detection and identification of thousands of components, in a single analysis and within only a few minutes. <a href="javascript:void(0);" aria-label="reference 3, 10 and 13 to 15">(3,10,13−15)</a>The main aim of this study was to evaluate the presence of typical compounds of the polar fraction of crude oils and to correlate them with data from micropyrolysis (Py) experiments, enabling the identification of potential biomarkers for use in geochemical thermal evolution diagnostics. The alternative analytical tool developed here is simpler and faster when compared to the classical biomarker ratios determined using GC–MS.<h3>Experimental</h3><h4>Analytical Micropyrolysis (Py)</h4>The 14 standard compounds described in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.energyfuels.4c03496/suppl_file/ef4c03496_si_001.pdf">Figure S1</a> of the Supporting Information were submitted to Py, according to the methodology of Maciel et al. <a href="javascript:void(0);" aria-label="reference 16">(16)</a> A 10 mg portion of each compound was inserted into a reactor tube with glass wool as an adsorbent material. The reactor tube was purged for 30 s with a 2 mL min–1 flow of N2, followed by heating to 500 °C in a Ni–Cr wire oven, resulting in a total reaction time of 3 min. The solvent used for final elution of the reactor tube contents was a methanol/toluene (1:1, v/v) mixture with a final volume of 1 mL. The solution obtained was analyzed by ESI(±) FT–MS.<h4>Ultra-High-Resolution Fourier Transform Mass Spectrometry (FT–MS)</h4>The FT–MS analyses were performed using an Orbitrap mass spectrometer (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=2&amp;search=Exactive+Plus">Exactive Plus, Thermo Scientific, U.S.A</a>.). The standard compounds, their Py products, and the crude oils were prepared by dissolution to a final concentration of 1 mg mL–1 in a mixture of toluene/methanol (1:1, v/v). Formic acid was added in a proportion of 0.1% and ammonium hydroxide in a proportion of 0.4% as ionization promoters for ESI(+) and ESI(−) analyses, respectively. The samples were introduced by a direct infusion. The operating conditions were a flow rate of 5 μL min–1, capillary voltage at –3.2 kV in ESI(−) mode and +4.0 kV in ESI(+) mode, capillary temperature of 280 °C, and N2 as sheath, auxiliary, and spare gases at 5, 5, and 2 (arbitrary units), respectively.The acquisition and interpretation of mass spectra were performed using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=2&amp;search=Xcalibur+2.0">Xcalibur 2.0 software</a> (Thermo Scientific, U.S.A.), in the m/z range of 100–1000, which in a total of 100 μscans were accumulated to obtain the final average mass spectrum. The software determined the exact mass, inferring molecular formulas, indicating the assignment error for each molecular formula, providing double bond equivalent (DBE) values, and the total abundance of ions that were used in the MS ratio proposed. Confirmation of peak attribution considered agreement between the experimental and theoretical m/z values together with the isotopic pattern.Sequential mass spectrometry analyses (MS/MS) were performed by FT-ICR MS (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=10&amp;search=solariX+9.4+T">solariX 9.4 T</a>, Bruker Daltonics, Germany), using ESI(−) ionization mode and a collision energy of 25 eV, for specific ions from the Py product of the 2,6-dimethyl-4-pyridinol standard compound. The ESI conditions of the FT ICR–MS/MS analysis were analogous to those described above for the Orbitrap FT–MS analyses.<h4>Analysis by GC-MS</h4>Crude oil samples (5 g) were fractionated into saturate, aromatic, resin, and asphaltene (SARA) compounds, according to the conditions of Santos et al. <a href="javascript:void(0);" aria-label="reference 17">(17)</a> Briefly, n-heptane (in the proportion of 30 mL/g of crude oil) was added to the crude oil sample, and the mixture was refluxed for 1 h. Subsequently, the mixture was cooled and stored in the dark overnight, resulting in precipitation of the asphaltenes. The maltene fractions soluble in n-heptane were separated using open-column chromatography (3 × 40 cm) after previously being adsorbed on activated neutral alumina (80–200 mesh, Brockmann I, Sigma-Aldrich, Steinheim, Germany). Cyclohexane was used to elute the saturated fraction, which was analyzed by GC–MS, using a gas chromatography/triple quadrupole mass spectrometry system (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=TQ8040">GCMS-TQ8040</a>, Shimadzu, Japan).GC–MS was operated in electron ionization (EI) mode, following the conditions of Carregosa et al. <a href="javascript:void(0);" aria-label="reference 18">(18)</a> Briefly, the chromatographic separation was performed with a SH-RTX5SilMS capillary column [crossbond 1,4-bis(dimethylsiloxy)phenylene dimethylpolysiloxane, 30 m × 0.25 mm inner diameter, 0.25 μm film thickness, Restek, U.S.A.]. A 1 μL volume of the solution was injected in the splitless mode. The injector temperature was 300 °C. The oven temperature was programmed from 70 to 325 °C, at 3 °C min–1, resulting in a total chromatographic run time of 85 min. Helium (99.995% purity) was used as the carrier gas at a constant flow rate of 1 mL min–1. The mass spectrometer ion source and interface temperatures were 280 and 290 °C, respectively. The collision gas was Ar (99% purity), and the collision energy was set at 12 eV.Multiple reaction monitoring (MRM) GC–MS analysis was performed to identify terpane and sterane compounds that could be employed as thermal evolution biomarkers. The m/z transitions monitored were m/z 370 &gt; 191, to calculate Ts/Tm and Ts/(Ts + Tm) ratios, and m/z 412 &gt; 191, to calculate C32S/(S + R) ratios.<h3>Results and Discussion</h3><h4>&nbsp;ESI(−) FT–MS of the Crude Oils</h4>The six crude oils analyzed by ESI(−) FT–MS presented a complex chemical mixture, with a wide range of polar compounds, as also described by Santos et al. <a href="javascript:void(0);" aria-label="reference 17">(17)</a> A representative MS spectrum is shown for the AL crude oil (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.energyfuels.4c03496#fig4" data-tab="pane-pcw-Figures" id="">Figure 4</a>a), with expansion to visualize the deprotonated ions of 2,6DPO (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.energyfuels.4c03496#fig4" data-tab="pane-pcw-Figures" id="">Figure 4</a>b) and 1DP (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.energyfuels.4c03496#fig4" data-tab="pane-pcw-Figures" id="">Figure 4</a>c), to highlight that only the standard compound and its 1DP product from Py were naturally present in the chemical composition of the oil.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Energy_Fuels_2024_38_22_21932_21940_Exploratory_Analysis_of_Crude_Oil_Thermal_Evolution_by_Ultra_High_Resolution_Mass_Spectrometry_Figure_4_832bae4e51.jpeg" alt="Energy Fuels 2024, 38, 22, 21932–21940 - Exploratory Analysis of Crude Oil Thermal Evolution by Ultra-High-Resolution Mass Spectrometry - Figure 4. ESI(−) FT–MS spectrum of (a) AL, with expansions at (b) m/z 121–123, highlighting 2,6DPO, and (c) m/z 241, highlighting 1DP." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Energy_Fuels_2024_38_22_21932_21940_Exploratory_Analysis_of_Crude_Oil_Thermal_Evolution_by_Ultra_High_Resolution_Mass_Spectrometry_Figure_4_832bae4e51.jpeg 99w," sizes="100vw" width="1600" height="2528">The ESI(−) FT–MS data for all of the crude oils are shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.energyfuels.4c03496/suppl_file/ef4c03496_si_001.pdf">Figures S2</a>–<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acs.energyfuels.4c03496/suppl_file/ef4c03496_si_001.pdf">S6</a> of the Supporting Information for the CA, PI, SE, O3, and O16 samples, respectively. The presence of ions corresponding to 2,6DPO and its 1DP product from Py was found for all of the crude oils analyzed. The m/z, molecular formula, DBE, and structures are summarized in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.energyfuels.4c03496#tbl2" data-id="tbl2">Table 2</a>.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Energy_Fuels_2024_38_22_21932_21940_Exploratory_Analysis_of_Crude_Oil_Thermal_Evolution_by_Ultra_High_Resolution_Mass_Spectrometry_Table_2_6367dc796b.jpg" alt="Energy Fuels 2024, 38, 22, 21932–21940 - Exploratory Analysis of Crude Oil Thermal Evolution by Ultra-High-Resolution Mass Spectrometry - Table 2. ESI(−) FT–MS Data for the Six Crude Oils Related to the 2,6DPO and 1DP Compounds" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Energy_Fuels_2024_38_22_21932_21940_Exploratory_Analysis_of_Crude_Oil_Thermal_Evolution_by_Ultra_High_Resolution_Mass_Spectrometry_Table_2_6367dc796b.jpg 176w," sizes="100vw" width="814" height="722">Both compounds were naturally present in all of the crude oils but in different abundances, reinforcing that a relation between the abundances of the ions could be explored in the geochemical context of thermal evolution.<h3>Conclusion</h3>The thermal behaviors of 14 typical petroleum compounds were evaluated on the basis of ESI(±) FT–MS analyses, to identify a potential geochemical biomarker of thermal evolution among the polar compounds present in the oils. It was found that pyrolysis of 2,6-dimethyl-pyridin-4-ol (2,6DPO) led to the formation of product ions, which were also observed in the FT–MS analyses of the crude oils. MS/MS analysis identified the main thermal product as 2,2-[(ethene-1,2-diyl)]bis(6-methylpyridin-4-ol), denoted 1DP. These ions were used in a proposed indicator, denoted the MS ratio, which could be used to evaluate the degree of thermal evolution of oils based on FT–MS analysis. The resulting MS ratio values were directly correlated with the values of classical diagnostic ratios [Ts/Tm, Ts/(Ts + Tm), and C32S/(S + R)], obtained by GC–MS, and showed the same order of thermal evolution for the six crude oils evaluated. Therefore, the MS ratio is a tool that can be used to infer the thermal evolution of oils, focusing on the polar compounds, as an alternative to the traditional methods based on GC–MS, with the advantages of simpler direct analysis and faster data acquisition. Furthermore, the MS ratio offers potential advancements in geochemical research by enhancing the tracking of polar molecules, which are often neglected in traditional biomarker analysis. This method has practical implications for geochemical studies, enabling rapid and accurate evaluations of oil maturity degrees.

Exploratory Analysis of Crude Oil Thermal Evolution by Ultra-High-Resolution Mass Spectrometry

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 17th February 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies&nbsp; and Shimadzu and product spotlight by Thermo Fisher Scientific!<h4>1. Agilent Technologies: Extractable Pollutants from Microplastics to Vegetables: Incorporation to the Food Chain</h4>Using static headspace GC/MS with the Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890%2F5977B">8890 GC and 5977B GC/MSD</a><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_extractable_pollutants_from_microplastics_to_vegetables_5994_7882en_agilent_5b4df39dff.pdf">Full PDF for download</a></li></ul>Most studies of organic pollutants in vegetables focus on persistent organic pollutants (POPs)10,11, which are extracted from samples and usually monitored by liquid chromatography (LC).12 However, the accumulation of MP-associated pollutants in vegetables has hardly been evaluated.This application note presents:<ol><li>A developed and validated approach to the targeted and untargeted analyses of MP-associated pollutants found in vegetables</li><li>Quantitation of MP pollutants</li><li>Assessment of the influence of vegetable type (edible- versus nonedible-roots) on the intake of MP-associated pollutants</li><li>The accumulation and environmental migration pathways of the MP pollutants</li></ol>In this application note, an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=SHS-GC%2FMS">SHS-GC/MS</a> method involving a static headspace coupled to an 8890 GC and 5977B GC/MSD was used for the evaluation of volatile extractables from plastic residues present in vegetable matrices. This technique is well suited to extract volatile compounds from different samples due to its simplicity, automation, speed, low cost, and minimal sample preparation requirements.13–15 Additionally, the application of MS in combination with a spectral deconvolution and retention indices (RIs) enabled advanced detection and identification of volatile MPassociated pollutants in vegetable matrices.&nbsp;<h4>Conclusion</h4>A straightforward, reliable, and robust SHS-GC/MS methodology using an Agilent 8890 GC and an Agilent 5977B GC/MSD was developed to identify and quantify plasticassociated pollutants in vegetable samples. The method represents a preliminary approach to assess the impact of agricultural MP contamination on food. The obtained data add new information to the mobility of MP leachates from agricultural soils to vegetables. The application of chemometrics to the dataset acquired from the SHS-GC/MS analysis has demonstrated that the accumulation of these organic pollutants was higher in edibleroot than nonedible-root vegetables. The main contributors to this differentiation were 2,4-di-tert-butylphenol, cumene, 2-tert-butyl-4 methylphenol, and 2,4-dimethylphenol, which are chemicals associated with plastic contamination. Specifically, cumene may be related to polystyrene (PS) pollution.A total of 92 putative compounds were accurately identified using spectral deconvolution retention indices (RIs). In the samples, plastic-associated compounds were quantified. Their contents varied from 0.14 to 28,800 ng/g for 2,4-di-tert-butylphenol and p,α-dimethylstyrene, respectively. The presence of phenylacetaldehyde in all the samples, as well as styrene, cumene, and p,α-dimethylstyrene in some of them, indicated PS contamination. Other compounds found in the studied vegetables, such as xylene isomers and ethylbenzene, highlighted potential contamination of other polymeric materials like polyvinyl chloride (PVC) or polyethylene terephthalate (PET).<h4>2. Shimadzu: Analysis of Essential Oil Using GC-MS/FID Detector Splitting System</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00819_en_c5c92dcd13.pdf">Full PDF for download</a></li></ul><h5>User Benefits</h5><ul><li>The detector splitting system allows for simultaneous acquisition of MS and FID data in a single measurement.</li><li>Even complex samples can undergo simplified statistical analysis using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=eMSTAT+Solution">eMSTAT SolutionTM</a>.</li><li>The combination of the compact <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GC-2050">BrevisTM GC-2050</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-QP2050">GCMS-QP2050</a> enables space-saving in the laboratory.</li></ul>In this application, five types of Hinoki oils, including Hinoki oil made by our company and Hinoki oils from different regions, were analyzed using the detector splitting system between MS and FID. The results from MS were compared using eMSTAT Solution to analyze the composition of the components. Additionally, the quantification of δ Cadinene, an important aromatic component that is a sesquiterpene was conducted using FID, which showed high calibration linearity over a wide concentration range. Furthermore, with a compact width of approximately 63 cm, the device configuration of Brevis GC-2050 + GCMS-QP2050 not only contributes to space-saving in the lab but also demonstrates high analytical performance.<h5>Essential Oil Analysis Using GC-MS/FID</h5>In quality control (QC) of fragrances like Hinoki oil, where a wide concentration range is typically expected, GC-FID, which provides detector response over a broad range, is commonly used. By comparing the chromatogram shapes of product samples obtained during the production process with approved reference samples, the component profile is confirmed. However, in the case of Hinoki oil containing numerous components, qualitative analysis of each peak becomes challenging with an FID detector. Therefore, by using the detectorsplitting system between MS and FID, it is possible to obtain data from both MS and FID simultaneously in a single measurement. This allows for the usual confirmation of chromatogram shapes with FID and enables qualitative analysis with MS when unknown components are detected.<h5>System Configuration and Analysis Conditions</h5>The system configuration and analysis conditions are shown in Table 1 and 2, respectively In this analysis, SMI (Smart Micro Inert) FLOW DEVICE 2-Way Splitter for detector splitting was used (Fig. 1). The SMI FLOW DEVICE is a capillary flow device for analysis with features such as low leakage, low dead volume, low heat capacity, and inertness. This allows for the analysis of highly adsorptive components. We adjusted the inner diameter of the resistors used for MS/FID detector Splitting, as well as the pressure of the AUX-APC (Digital Flow Controller), to set the split ratio at approximately 1:3 for MS:FID. By using eMSTAT Solution for analysis, we visually grasped the differences in component characteristics of each Hinoki oil and identified the compounds contributing to those differences.<h4>Conclusion</h4>Five different types of Hinoki oils were analyzed using a detector splitting system with MS and FID. When conducting multivariate analysis with the results from MS using eMSTAT Solution, it was possible to visually capture the differences in component characteristics. It was revealed that (-)-Borneol is a characteristic component of Shimadzu oil. Additionally, accurate quantification of δ-Cadinene, which varies significantly in concentration among samples, was achieved using FID.<h4>3. Thermo Fisher Scientific: Fully automated method implementation for compliant analysis of polychlorinated dibenzodioxins/furans by GC-MS/MS</h4><ul><li>Other</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/sl_003541_gc_ms_eworkflow_dioxin_sl003541_na_en_9f48797bef.pdf">Full PDF for download</a></li></ul>Performance-based methodology for dioxin analysis is applied within the EU to ensure accurate reporting of dioxin levels within food and feed. Results are evaluated according to strict quality control and reporting criteria. For analytical testing laboratories, this often means a significant time investment for adoption and implementation of the methodology for dioxin analysis, as well as a requirement for highly skilled operators. Even for laboratories experienced with GC-MS-based test procedures, the addition of dioxin testing to the overall portfolio is demanding. To simplify this process, a dedicated eWorkflow™ template is available within the Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=2&amp;search=chromeleon">Chromeleon™</a> Chromatography Data System. This eWorkflow template is available for the Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=2&amp;search=TSQ+9610">TSQ™ 9610 </a>triple quadrupole GC-MS/MS system and is free to download from the Thermo Scientific™ AppsLab™ Library of Analytical Applications (Dioxin eWorkflow).&nbsp;Processing methods within the Dioxin eWorkflow template use isotopic dilution for quantitation, allowing users to perform data acquisition and real-time quantitation within the same software. Spiking levels of both syringe and internal standard can be defined per injection, permitting samples spiked with different levels of internal or syringe standard concentration to be analyzed in a single sequence. This can be seen in Figure 3 where internal standard concentration level within the sequence is defined at different levels for calibration standards (i.e., PCDD/F CS1), check standards (LOQ, LOQ/2, LOQ/4), and blank/sample injections (Sample).The Dioxin eWorkflow template allows analytical testing laboratories to easily implement compliant analytical methodology for dioxin analysis. It delivers validated data acquisition/processing methods and reporting templates for dioxin analysis, helping remove time-consuming steps around method development and data processing.Included within the Dioxin eWorkflow template:<ul><li>Injection sequence templates with pre-optimized analytical parameters for method injection and data acquisition.</li><li>Incorporation of isotopic dilution quantitation, removing the need for additional software or script writing to perform data calculations.</li><li>Interactive tables and charts to facilitate quick data evaluation for compliance purposes.</li><li>Fully customizable data evaluation and report layout templates based on the analyst’s needs.</li></ul>

News from LabRulezGCMS Library - Week 8, 2025

In the week from February 17, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.<blockquote><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars">👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</a>👉 Search and filter in the largest global database with over 4 000 GC, LC, MS and spectroscopy webinars.</blockquote><h5 data-start="151" data-end="272">1. GERSTEL: Determination of PFAS in Various Sample Types, including Air, Water, and Food, Using GC-MS or LC-MS</h5><ul data-start="274" data-end="328"><li data-start="274" data-end="313">Tuesday, February 18, 2025, 20:00 CET</li><li data-start="314" data-end="328"><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4734">Registration</a></li></ul>Are you looking for PFAS in air, water, or food samples? Discover how to automate analytical methods for PFAS determination, including ASTM D8591-24, EPA methods 533, 537.1, and 1633, and FDA method C-010.03.<h5 data-start="540" data-end="632">2. GERSTEL: Precise Results Within Seconds – The Future of MOSH/MOAH Data Analysis</h5><ul data-start="634" data-end="690"><li data-start="634" data-end="675">Wednesday, February 19, 2025, 10:00 CET</li><li data-start="676" data-end="690"><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4641">Registration</a></li></ul>Discover the GERSTEL ChroMOH software, our powerful evaluation software for MOSH/MOAH data, in our informative webinar!<h5 data-start="813" data-end="928">3. New Food Magazine/Bruker: Enhancing Food Safety Labs with Rapid Detection of Salmonella, Listeria, and Moulds</h5><ul data-start="930" data-end="986"><li data-start="930" data-end="971">Wednesday, February 19, 2025, 16:00 CET</li><li data-start="972" data-end="986"><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4723">Registration</a></li></ul>This webinar focuses on advanced methodologies for detecting microorganisms, including rapid techniques such as MALDI-TOF MS and FTIR-spectroscopy.<h5 data-start="1137" data-end="1194">4. Agilent Technologies: Molecular Spectroscopy</h5><ul data-start="1196" data-end="1251"><li data-start="1196" data-end="1236">Thursday, February 20, 2025, 04:00 CET</li><li data-start="1237" data-end="1251"><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4673">Registration</a></li></ul>In this second session, we will talk about the analysis of microplastics in the environment and food.

Webinars LabRulezGCMS Week 8/2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 24th February 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies, Knauer&nbsp; and Shimadzu!<h4>1. Agilent Technologies: Analysis of 65 Volatile Organic Compounds in Ambient Air by Canister Sampling Using an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=8890%2F5977">8890/5977</a> GC/MSD</h4><h5>A method using both scan and SIM mode that fully meets the requirements in the HJ 759-2023 standard</h5><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_voc_air_gc_msd_5994_7723en_agilent_4b88e40417.pdf">Full PDF for download</a></li></ul>This application note introduces the use of a canister for gas sampling. Samples were introduced into an Agilent 8890 gas chromatograph (GC) with an Agilent 5977 single quadrupole mass selective detector (MSD) and the Markes Multi-Gas thermal desorption (TD), to analyze volatile organic compounds (VOCs) in the atmosphere or in semiconductor cleanrooms. The results of linearity, reproducibility, and detection limit fully met the requirements of the China method HJ759-2023. This method is widely used as a reference both in environmental laboratories and semiconductor cleanrooms. The linear correlation coefficient for all 65 compounds was greater than 0.991, with 86% of compounds having a value greater than 0.999. The results of reproducibility in scan mode varied between 0.3 to 6.8%, while results in SIM mode varied between 1.1 to 6.7%. The sampling volume was 300 mL, which resulted in detection limits of 0.013 to 0.113 nmol/mol for scan mode and 0.002 to 0.013 nmol/mol for SIM mode.&nbsp;<h4>Experimental</h4>This study was performed on an 8890 GC coupled to a 5977 single quadrupole GC/MSD with an electron ionization (EI) source. A Markes Multi-Gas thermal desorption sample introduction and preconcentration system was used and included three modules:<ul><li>CIA Advantage-xr (CIA): canister autosampler</li><li>Kori-xr: water removal module</li><li>Unity-xr: thermal desorption instrument</li></ul>First, three internal standards (ISTDs) were introduced into the Unity trap by CIA. Then, the sample was passed through a heated transfer line through the CIA Advantage into the Kori for water removal. Finally, the sample flowed into the focusing cold trap of the Unity for preconcentration. Eventually, the Unity trap was desorbed at high temperature, and the 65 VOCs and three ISTDs all entered the GC/MSD for analysis. Figure 1 shows the flow path of the combined system.&nbsp;<h4>Conclusion</h4>An Agilent 8890/5977 GC/MSD system, equipped with a Multi-Gas CIA Advantage-xr TD provides a robust analytical procedure for the analysis of 65 VOCs in ambient air. This system offers a highly efficient and highly sensitive solution for the simultaneous analysis of multiple VOCs in both atmospheric quality monitoring laboratories and semiconductor cleanrooms. Based on different application requirements, users can choose to collect data in scan or SIM mode, demonstrating the flexibility of Agilent instruments. Excellent analytical performance has been achieved based on this system both in scan and SIM mode, which fully meets the requirements detailed in method HJ 759-2023.<h4>2. Knauer: GPC vs. SPE and subsequent determination of polycyclic aromatic hydrocarbons using GC/MS</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/VEV_0081_Comparison_of_GPC_and_SPE_purification_methods_of_sludge_samples_FINAL_web_376100390f.pdf">Full PDF for download</a></li></ul>Polycyclic aromatic hydrocarbons (PAHs) are ubiquitous environmental pollutants generated primarily during the incomplete combustion of organic materials. The removal of PAHs from the atmosphere by dry and wet deposition processes are strongly influenced by their gas/particle partitioning. Atmospheric deposition is a major source for PAHs in soil [1] which can be determined by various extraction and purification processes, subsequently detected by a GC/MS using the reference method UNI EN 15527. Our main purpose is to demonstrate that the purification of environmental matrix with high organic component using the gel permeation chromatography purification (AZURA GPC Cleanup, FS conditioned resins CHEX/DCM), compared to a SPE purification, allows are well-defined separation time of the analytes and it can provide narrow bands without their physical chemical interaction with the column, resulting in less chance of loss of analytes [2]. This differs from other separation techniques which depend upon chemical or physical interactions to separate analytes [3].<h4>Conclusion</h4>The GPC cleanup procedure of mud sludge samples prior analysis of PAHs with GC/MS technique is a good alternative to SPE purification steps. Advantages like better S/N ratios and third mass identification are obvious. The automatization of the GPC Cleanup using AZURA GPC Cleanup system yields high efficiency of the application.<h4>3. Shimadzu: Material Analysis of Microplastics in River Water - FTIR and Pyrolysis-GC-MS Analysis</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00806_en_c2c7bba8be.pdf">Full PDF for download</a></li></ul><h5>User Benefits</h5><ul><li>Automated pretreatment of microplastics (MPs) reduces workload and enables highly reproducible pretreatment.</li><li>Material analysis of MPs processed by the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=MAP-100">MAP-100</a> device can be easily performed by <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=FTIR-ATR">FTIR+ATR.</a></li><li>Highly reproducible GC-MS analysis of MPs is possible by homogeneously pulverizing samples with Cryogenic Mill (IQ MILL-2070).</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=EGA%2FPY-3030D">Pyrolysis</a>-<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=GCMS-QP2020+NX">GC-MS</a> can measure the weight of multiple types of plastics even when they are mixed.</li></ul>Microplastics (MPs) are microscopic plastic particles measuring a few µm to 5 mm in size. They are feared to have an impact on ocean pollution and ecosystems. Against this backdrop, surveys and studies on MPs in surface waters such as oceans, rivers, lakes and marshes are being conducted worldwide. Fourier Transform Infrared Spectrophotometer (FTIR) is often used for material analysis of MPs. ASTM recently published the D8401-24 standard test method for the qualitative and quantitative determination of MPs in water that uses a pyrolysis gas chromatograph mass spectrometer (Py-GC-MS). In this application news, a sample taken from a river was pretreated and analyzed for MPs using FTIR and Py-GC-MS.<h4>Conclusion</h4>Samples collected from river water were automatically pretreated using MAP-100, and the MPs materials were then analyzed by FTIR and Py-GC-MS. PP, PE and EVA were detected in both instruments, indicating that PP and PE are the main components (Fig. 8). Using an FTIR, individual qualitative results can be obtained easily, and the number ratios and densities can be calculated. Py-GC-MS also provides a more accurate massto material ratio (%). The system supports screening methods that take advantage of the features of each instrument, from preparation to analysis of MPs.

News from LabRulezGCMS Library - Week 9, 2025

In the week from February 24, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.<blockquote><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars">👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</a>👉 Search and filter in the largest global database with over 4 000 GC, LC, MS and spectroscopy webinars.</blockquote><h5>1. Agilent Technologies: Detecting Microplastics in Cannabis: An Analysis Using LDIR Spectroscopy</h5><ul data-start="167" data-end="214"><li data-start="167" data-end="201">Tu, 25.2.2025</li><li data-start="202" data-end="214"><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/2772">Registration</a></li></ul>Detecting Microplastics in Cannabis: An Analysis Using LDIR Spectroscopy.<h5>2. Separation Science/Biotage: Automated Sample Preparation for Multi-Residue Pesticide Analysis by LC-MS and GC-MS</h5><ul data-start="395" data-end="443"><li data-start="395" data-end="430">We, 26.2.2025</li><li data-start="431" data-end="443"><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4724">Registration</a></li></ul>Learn how Biotage's automated preparation workflow can analyze the entire panel and produce results equivalent to manual preparation.<h5>3. LECO: Detailed Hydrocarbon Type Analysis of Aviation Fuels: Navigating the Challenges of Evolving Feed Stocks</h5><ul data-start="720" data-end="768"><li data-start="720" data-end="755">We, 26.2.2025</li><li data-start="756" data-end="768"><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4687">Registration</a></li></ul>This webinar will review both historical and contemporary analytical methods used for HTA, with a focus on the evolving challenges associated with achieving accurate identification and quantification with GCxGC<h5>4. Wiley: Advances in Spectral Identification: SmartSpectra, Classifications, &amp; More!</h5><ul data-start="720" data-end="768"><li data-start="720" data-end="755">We, 26.2.2025</li><li data-start="756" data-end="768"><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4789">Registration</a></li></ul>This webinar covers the latest advances in spectral analysis, including Wiley’s KnowItAll models, SmartSpectra, and functional group analysis tools.

Webinars LabRulezGCMS Week 9/2025

Ionic liquid coating for stir bar sorptive extraction and its application for extraction and nontargeted screening analysis via TD-GC–Orbitrap-HRMS of pollutants in river water

In the week from March 3, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.<blockquote><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars">👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</a>👉 Search and filter in the largest global database with over 4 000 GC, LC, MS and spectroscopy webinars.</blockquote><h5>1. Agilent Technologies: Application of GC/MS for the Analysis of Poly-Aromatic Hydrocarbons (PAHs) and Pesticides in Drinking Water According to the Directive EU 2020/2184</h5><div><div><ul><li><div>We, 5.3.2025 14:00 CET</div></li><li><div><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4712">Registration</a></div></li></ul></div>The main analytical techniques for the analysis of PAHs and pesticides in GC/MS in drinking water, with particular attention to the Solid Phase Micro-Extraction (SPME) technique.</div>

Webinars LabRulezGCMS Week 10/2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 3rd March 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you poster by Agilent Technologies and application notes by Knauer, Shimadzu and Thermo Fisher Scientific!<h4>1. Agilent Technologies: GC/MS Approach for Analysis of Extractables and Leachables (E&amp;L) in Complex Matrices Using Spectral Deconvolution and Retention Indices</h4><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_7250_5977c_extractable_leachable_asms_2024_mp208_en_agilent_71b19d3b16.pdf">Full PDF for download</a></li></ul>Modern drug delivery systems are meant to protect a drug from environmental contamination, but they may also be a source of contamination. It is necessary to identify those compounds that can extract, leach, or migrate from the package or device. Extractables and leachables analysis presents a challenge for GC/MS because of the complexity of the various sample matrices and a diverse range of compounds to be identified. This study demonstrates how unit resolution GC/MS workflow is employed for identifying GC-amenable E&amp;L compounds by leveraging spectral deconvolution in combination with retention index-based time filtering. An addition of the accurate mass high-resolution GC/Q-TOF into the workflow provided extra confidence in compound identification, sensitivity and capability of structural elucidation.&nbsp;Operating in the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=OpenLab+ECM">OpenLab Electronic Content Management </a>(ECM) XT configuration enabled tools that help facilitate compliance with various national and EU electronic record regulations, including audit trails, and remote data storage.<h5>Experimental</h5>Rubber syringe gaskets were extracted using tetrahydrofuran (THF) solvent at room temperature for six months. An aliquot of the extracts was analyzed using both <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=GC%2FMSD">GC/MSD</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=GC%2Fq-TOF">GC/Q-TOF</a> systems. The acquisition software operated under a unified compliance environment. The instrumental parameters are shown in Table 1. The chromatographic deconvolution and library search were performed in the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=MassHunter">MassHunter</a> Unknowns Analysis 12.1. The NIST23 library was used to perform initial compound identification. Structural elucidation was performed using Molecular Structure Correlator (MSC) software 8.2.&nbsp;Retention time locking was used to achieve the same retention times between multiple GC/MSD and GC/Q-TOF systems allowing for using both retention index and retention time matching.<h5>Conclusions</h5><ul><li>The optimized GC/MSD and GC/Q-TOF approach for analysis of extractables and leachables allowed for identifying over 150 compounds in a complex E&amp;L extract&nbsp;</li><li>High-resolution GC/MS enabled identification of over 60 additional components with increased confidence and structure elucidation of the unknowns&nbsp;</li><li>The novel ultra low bleed Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=J%26W+DB-5Q">J&amp;W DB-5Q</a> GC column resulted in significant decrease in background, that could potentially yield higher number of identifications of late eluting compounds.</li></ul><h4>2. Knauer: GPC cleanup method for soil samples before PAHs analysis</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/VEV_0082_GPC_Cleanup_of_soil_samples_FINAL_web_5260b86091.pdf">Full PDF for download</a></li></ul>GPC (Gel Permeation Chromatography) is a size-exclusion clean-up procedure that readily separates high molecular weight interferents from sample extracts using organic solvents and a porous hydrophobic gel (primarily a crosslinked divinylbenzene-styrene copolymer) [1]. It is possible to distinguish between different types of Bio-Beads resin based on the type of cross-linkage. In this application Bio-Beads S-X3 with 200–400 mesh was used according to EPA method 3640 [1]. GPC clean-up can be used extensively in numerous environmental analysis especially for preparing sample extracts prior to semivolatile compounds determination, such as pesticide, and PAHs analysis by GC/MS or HPLC-UV-DAD. Sample cleanup is particularly important for analytical separations such as GC, HPLC, and electrophoresis because high-boiling materials can cause a variety of problems in analytical systems, like analyte adsorption in the injection port or in front of a GC or LC column [2]. GPC cleanup protects GC and HPLC columns, reduces analytical maintenance costs, improves accuracy, and allows lower detection limits.<h5>Materials and Methods</h5>Extraction of Polycyclic Aromatic Hydrocarbons was carried out using Accelerated Solvent Extraction (ASE), according to the 3545A EPA method [3]. Bio-Beads S-X are supplied dry and must be swollen prior to pack into a chromatographic column. A mixture of cyclohexane and dichloromethane (70:30, v:v) is suitable for clean-up of soil samples. As a general rule, the beads should be swollen in the same solvent chosen as mobile phase, so 10 g of Bio-Beads S-X3 were swelled with 50 mL of cyclohexane and dichloromethane mixture (70:30, v:v) overnight. After the beads were fully swollen, they were packed into a chromatographic column. Before sample cleanup, GPC column was equilibrated with the desired solvent mixture, flushing it almost three times the column volume at 1 mL/min. Cleanup method was performed with AZURA® GPC Cleanup System, which is operated with the Mobile Control Chrom® Software running on a tablet directly mounted on the system. The identification and quantification of PAHs was carried out by GC-MS/MS analysis. Calibration curves were constructed in the concentration range from 10 μg/L to 130 μg/L. To perform GC separation and MRM acquisition, optimization of the best chromatographic and detection conditions was necessary.<h5>Conclusion</h5>This application shows how to perform GPC cleanup with KNAUER AZURA® GPC Cleanup System for the analysis of PAHs in soil samples. This report is very detailed to ensure good performance in GPC cleanup for application in environmental area. We can conclude that AZURA GPC Cleanup System is an helpful tool for sample preparation before instrumental analysis because, unlike other techniques, is very useful for the removal of high boiling materials which would contaminate injection ports and column heads, prolonging column life, stabilizing the instrument, and reducing column reactivity. It could be considered an universal cleanup technique for a broad range of semivolatile organics and pesticides. Moreover, AZURA GPC Cleanup System allows the customer to process many extracted samples, with a reduction in time for the cleanup procedures.<h4>3. Shimadzu: Blood alcohol content (BAC) analysis using a liquid injection approach</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/AP_Blood_alcohol_content_via_liquid_injection_SCA_180_051_294d6843f8.pdf">Full PDF for download</a></li></ul><h5>User Benefits</h5><ul><li>Blood alcohol analysis using liquid injection is an alternative to the headspace</li><li>analysis of blood samples for clinical purposes</li><li>It provides reliable results for whole blood and plasma samples without adverse matrix effects&nbsp;</li></ul>Blood alcohol content (BAC) is relevant for legal regulations regarding driving limits, but also investigated for forensic and clinical purposes with respect to poisoning. Blood alcohol analysis does not only focus on ethanol, which is the classical drinking alcohol, but also investigates other alcoholic substances like methanol and isopropanol as well as metabolites like acetone. Ethanol is present in alcoholic beverages, but also used for antiseptics, various daily life products, and pharmaceuticals. Being a central nervous system depressant, consumption can cause severe intoxication with toxic levels at above 100 mg/dL blood [1]. Methanol intoxication could originate from the consumption of counterfeit alcohol, with as few as 30 mL pure methanol consumed being potentially lethal [2]. Isopropanol is widely used as solvent or antiseptic in households and sometimes used as cheap substitute for ethanol by alcohol abusers. It is metabolized by alcohol dehydrogenase to acetone, which alike isopropanol is a central nervous depressant [3].Blood alcohol analysis can be performed using gas chromatography (GC) with flame-ionization detection (FID). Due to the complexity of blood as matrix, headspace analysis is a widely used technique for simple sample transfer onto the GC column, which is especially valuable in forensics, where the matrix states investigated can drastically vary depending on the time the sample is taken. For clinical analysis, fresh blood is used, making the sample more uniform. In this approach, the analysis of BAC using a liquid injection technique as alternative to headspace sampling is presented.<h5>The Package</h5>The recommended analytical hardware and software configuration is listed below.<ul><li>Main Unit<ul><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=nEXIS+gc-2030+%28fid%29">Nexis GC-2030 with FID-2030</a>: Gas chromatograph with flame ionization detector</li></ul></li><li>Accessory<ul><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=AOC-30i+">AOC-30i </a>autosampler: Liquid autosampler with 30 vials capacity</li></ul></li><li>Main Consumables<ul><li>SH-BAC1 column (30 m x 0.32 mm x 1.8 µm;</li><li>P/N 221-76135-30)</li></ul></li><li>Software<ul><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=3&amp;search=LabSolutions+LCGC">LabSolutions LCGC</a></li></ul></li></ul><h4>Conclusion</h4>Liquid sample injection presents a reliable alternative to headspace injection when analyzing blood samples for clinical purposes. Ethanol and methanol can be determined from whole blood, isopropanol and acetone from plasma samples without adverse matrix effects. Both whole blood and plasma analysis can be done using the same analytical method and one data processing approach, facilitating data evaluation and routine work.<h4>4. Thermo Fisher Scientific: Trace analysis of volatile organic compounds in wastewater according to U.S. EPA Method 624.1&nbsp;</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/an_003068_gc_gc_ms_isq_7610_epa_624_1_an003068_na_en_2297d596f3.pdf">Full PDF for download</a></li></ul>It is crucial that analytical testing laboratories monitor wastewater for the presence of volatile organic compounds (VOCs). VOCs are human-made contaminants used and produced in the processing of paints, adhesives, petroleum products, pharmaceuticals, and refrigerants. If they are released into wastewater from industrial activities, they can have an adverse effect on the natural environment and, ultimately, the public.1 U.S. EPA Method 624.1 is an approved test method under the Clean Water Act2 for determination of purgeable organic pollutants in industrial discharges and other environmental samples. The accurate detection and quantitation of VOCs via this method help ensure wastewater is not contaminated. Due to technological advances in analytical instrumentation and techniques, U.S. EPA Method 624.1 allows the analyst to modify P&amp;T parameters and GC/MS conditions. This can result in reduced sample run time and increased laboratory throughput in a 12-hour period.&nbsp;To perform U.S. EPA Method 624.1, method acceptance criteria must be achieved. These criteria include creating a working calibration curve, method detection limits (MDLs), and Initial Demonstration of Capability (IDC) of accuracy and precision for target compounds. As the sample matrix is water, it is essential that moisture is reduced, limiting the impact on the analytical column as this could damage the column and affect the results.&nbsp;The following evaluation describes the use of the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=2&amp;search=ISQ+7610">ISQ 7610</a> GC-MS system coupled with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=2&amp;search=TRACE+1610">TRACE 1610 GC</a> equipped with the Thermo Scientific™ HeSaver-H2 Safer™ split/splitless injector and a Teledyne LABS Tekmar Lumin P&amp;T concentrator paired with the AQUATek LVA autosampler for U.S. EPA Method 624.1 for the analysis of wastewater.<h5>Experimental</h5><h5>GC-MS parameters&nbsp;</h5>A TRACE 1610 GC was coupled to the ISQ 7610 MS equipped with a Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=2&amp;search=NeverVent">NeverVent™ </a>vacuum probe interlock (VPI) and a Thermo Scientific™ ExtractaBrite™ ion source. A Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=2&amp;search=TraceGOLD">TraceGOLD™ TG-VMS</a>, 30 m × 0.25 mm, 1.4 µm film column (P/N 26080-3320) was used for compound separation. The HeSaver-H2 Safer injector was utilized which reduces the carrier gas consumption by decoupling the gas used for the chromatographic separation from the gas used to pressurize the inlet and maintain split and purge flows. The critical separations were maintained with a run time of under 13 minutes.&nbsp;For this analysis, the ISQ 7610 MS was operated in full scan mode, ensuring the sensitivity needed for required the method detection limits. Nevertheless, the instrument could operate in Selected Ion Monitoring (SIM) mode for increased selectivity, if needed. Extended method parameters for the ISQ 7610 MS are shown in Table 2.<h5>Conclusion</h5>The ISQ 7610 MS system with the VPI coupled with the Teledyne LABS Tekmar Lumin P&amp;T concentrator paired with the AQUATek LVA autosampler exceeds all the requirements outlined in U.S. EPA Method 624.1 for analysis of VOCs in wastewater:<ul><li>MDLs calculated from n=7 repeat injections of 0.5 ppb water standards showed no interference from unwanted water entering the system and resulted in values &lt;0.15 ppb for most compounds.</li><li>Precision and accuracy for n=7 20 ppb water standards showed excellent results with %RSD &lt;20% and mean recovery of 93% for the compounds.</li><li>System robustness was tested by continuously acquiring 209 injections of water samples over two days with no user intervention at all. The average %RSD of the calculated concentration was 6.5% over this robustness study.</li><li>Utilizing the HeSaver-H2 Safer technology reduced helium consumption for the method by 4 times, reducing laboratory overheads.&nbsp;</li></ul>Further information on VOC analysis using the ISQ 7610 system and the Tekmar Lumin P&amp;T paired with the AQUATek LVA can be found in the Thermo Fisher Scientific AppsLab library.3 &nbsp;

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