Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 26th July 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!
<blockquote>
<h4>👉 <a href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></h4>
</blockquote>
<blockquote>
👉 Need info about different analytical techniques? Peek into <a href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.
</blockquote>
This week we bring to you applications and other documents by LECO, Agilent Technologies, Metrohm Shimadzu!
<h4>1. LECO: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PEGBTX_GINGER_OIL_HYDROGEN_CARRIER_GAS_203_821_694_1685d36546.pdf">Ginger Oil Analysis and Grade Differentiation with Pegasus BTX Using Hydrogen Carrier Gas</a></h4>
<ul>
<li>application note</li>
</ul>
Key Words: Fast GC, Hydrogen, TOFMS, Flavor and Fragrance, Essential oil, Ginger oil, Quality control
Introduction: Ginger essential oil (ginger EO) derives from the rhizome of the plant and has been valued for centuries Zingiber officinale for its aromatic, medicinal, and culinary properties. With a rich history dating back to ancient China and India, ginger oil has been treasured for its versatile applications and therapeutic benefits. Ginger EO is renowned for its warming, spicy aroma and is commonly used in aromatherapy to alleviate nausea, improve digestion, and relieve muscle pain. In culinary applications, it adds depth and complexity to dishes, especially in Asian and Indian cuisines. Additionally, ginger oil is valued in skincare for its anti-inflammatory and antioxidant properties, promoting healthy skin and hair.
The chemical composition of ginger oil is complex, comprising various bioactive compounds such as gingerol, shogaol, and zingiberene. Gas Chromatography-Mass Spectrometry (GC-MS) analysis is commonly employed to assess the quality and purity of ginger oil, ensuring it meets industry standards and regulatory requirements. Differentiating essential oil grades is crucial for the perfumery, flavor, and food industries due to several reasons related to quality, consistency, safety, and overall product effectiveness. As an example, high quality EOs are often pure, unadulterated, and extracted using meticulous methods to preserve their natural properties, whil the low-quality ones may be diluted, adulterated, or extracted using less refined methods, potentially compromising their scent and taste profiles and therapeutic qualities.
In this context, perfumery industries often need to be able to assess EO quality parameters in a fast and reliable manner. This application note describes the conversion of a Helium-based method to a fast and reliable Hydrogen-based one using LECO&#39;s novel BTX GC-TOFMS instrument. This mass spectrometer offers a wide dynamic range and sensitivity at Pegasus low femtogram levels, allowing for the simultaneous detection of both abundant and trace components without losing any detail. Additionally, ChromaTOF Sync software was used to distinguish between different grades of ginger EO and identify ® markers for each of them.
Conclusions: This application note demonstrates how the BTX GC-TOFMS is an excellent solution for the rapid analysis of EOs Pegasus using H carrier gas. The results indicate that neither the chromatographic performance nor the mass spectral quality are 2 compromised by using H . A % reduction in runtime was achieved, leading to improved daily throughput. Additionally, 2 60 the Sync software tool effectively clustered the samples based on their origin and quality, enabling the ChromaTOF discovery of characteristic features that differentiate them. The output information received from Sync ChromaTOF allows for more informed usage of raw materials in creating new fragrances and enhances confidence in analyzing routine samples.
<h4>2. Metrohm: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_ra_009_download_d7cc0b953a.pdf">Comparison of SPELEC RAMAN and standard Raman microscopes</a></h4>
<ul>
<li>application note</li>
</ul>
Larger laser spot size can provide representative results with a single measurement
Standard Raman microscopes are traditionally used to perform Raman measurements or Raman spectroelectrochemical experiments when they are coupled with electrochemical equipment. Raman spectra collected with confocal microscopes allows the characterization of very small areas. However, these instruments can exhibit several limitations. SPELEC RAMAN, a new generation of spectroscopic and spectroelectrochemical instruments, offers powerful and interesting features to overcome these issues. In this Application Note, a detailed comparison is made between the main features of a standard Raman instrument and the SPELEC RAMAN by analyzing the results obtained with both instruments.
CONCLUSION
SPELEC RAMAN exhibits a number of competitive advantages over standard Raman microscopes. For instance, the spot size of SPELEC RAMAN allows the characterization of a large area in a single experiment, obtaining representative results with only one measurement. The versatility of the Raman probe is demonstrated since it can be used with different cells. The portability as well as the simplicity of SPELEC RAMAN facilitate the performance of optical experiments. It also ensures the synchronization of electrochemical and optical signals in case Raman spectroelectrochemical measurements are carried out. In addition, DropView SPELEC software allows realtime acquisition of the data and the performance of operando measurements. The easy data treatment and analysis of the results is done using one-click tools.
<h4>3. Shimadzu: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/c103_e421_5c783b2e76.pdf">FTIR Talk Letter (vol. 42)</a></h4>
<ul>
<li>other</li>
</ul>
Table of content
<ul>
<li>Development of Dual Functional Catalytic Materials for CO2 Capture and Selective Hydrogenation and Mechanistic Elucidation of High CO Selectivity Using FTIR Spectroscopy | 02 </li>
<li>Configuration of the AIRsight Infrared Raman Microscope | 06</li>
<li>Notes on Infrared Spectral Analysis – Aliphatic Saturated Hydrocarbons (Paraffins) | 10</li>
<li>Fourier Transform Infrared Spectrophotometers &quot;IRSpirit-X Series&quot; | 16</li>
</ul>
<h4>4. Agilent Technologies: <a href="https://gcms.cz/labrulez-bucket-strapi-h3hsga3/an_impurity_analysis_hydrogen_8890_gc_tcd_fid_5994_7590en_agilent_85e4bf7514.pdf">Helium, Argon, Nitrogen, and Hydrocarbon Impurity Analysis in Hydrogen Using an Agilent 8890 GC and TCD/FID System</a></h4>
<ul>
<li>Application Note - Energy &amp; Chemicals</li>
</ul>
Abstract
In this application note, the analysis of helium (He), nitrogen (N₂ ), argon (Ar), and hydrocarbon (HC) impurities in hydrogen (H₂ ) was demonstrated on an Agilent 8890 gas chromatography (GC) system using gas sampling valve injection, capillary column separation, and flame ionization/thermal conductivity detectors (FID/TCD). The system repeatability, sensitivity, and linearity were evaluated. The excellent test results demonstrated that the 8890 GC can provide accurate and precise analysis of the target analytes. In addition, this system can be applied to the quality control of fuel cell vehicles that used hydrogen, according to different regulations such as ISO 14687-2019 and GB/T 37244-2018.
Conclusion
In this application note, an Agilent 8890 GC configured with two gas valves, two types of detectors (FID/TCD), and three capillary PLOT columns, was applied to He, Ar, N₂, and HC impurity analysis in hydrogen. The system performance was evaluated using certified gas standards. The comprehensive assessment covered RT and response repeatability, linearity, quantitation accuracy, and method LODs. The area precision of all test compounds was better than 3.0% at the low concentration level. The LODs for He, Ar, N₂, and methane were 2.6, 0.6, 0.8, and 0.019 ppm, which were far below their quality limits in the ISO 14687-2019 and GB/T 37244-2018 standards. The quantitation accuracy was 92 to 116% across the calibration range. These excellent results demonstrate that the 8890 GC, together with the selected Agilent GC columns, can provide accurate, precise, and sensitive analysis of target components. The test system can reliably be used for the quality control of He, Ar, N₂, CH₄, and other HCs in FCV-grade hydrogen, according to ISO 14687-2019 and GB/T 37244-2018 requirements.

News from LabRulezGCMS Library - Week 31, 2024

In the 2 weeks from August 12, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.
<blockquote>
<h4><a href="https://gcms.labrulez.com/webinars">👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</a></h4>
</blockquote>
<blockquote>
👉 Search and filter in the largest global database with over 3 500 GC, LC, MS and spectroscopy webinars.
</blockquote>
<h5>1. Agilent Technologies: Get the Most Out of Your MS: Novel Column Chemistry Raises the Bar on Sensitivity and Data Accuracy</h5>
<ul>
<li>Tu, 13.8.2024 17:00 CEST</li>
<li><a href="https://gcms.labrulez.com//webinar/3908">Registration</a></li>
</ul>
We’ll examine how column attributes like bleed, thermal stability, and inertness can translate into practical data quality improvements.
<h5>2. Phenomenex: Advancing Food Testing Using New and Unique GC Column Selectivities</h5>
<ul>
<li>Tu, 13.8.2024 19:00 CEST</li>
<li><a href="https://gcms.labrulez.com//webinar/4161">Registration</a></li>
</ul>
Learn about important applications in food testing and current trends. Recieve an overview of available new column selectivity, and relevant applications.
<h5>3. Shimadzu Corporation: Elevating Pharma 4.0: Harnessing CaliberLIMS For Digital Excellence</h5>
<ul>
<li>We, 14.8.2024 08:30 CEST</li>
<li><a href="https://gcms.labrulez.com//webinar/4163">Registration</a></li>
</ul>
CaliberLIMS is a robust, scalable, and reliable platform designed to meet the demands of modern laboratories aiming for Pharma 4.0.
<h5>4. Agilent Technologies: End Consumables Counting Chaos: Track and Trend for Timely GC Maintenance</h5>
<ul>
<li>Th, 15.8.2024 17:00 CEST</li>
<li><a href="https://gcms.labrulez.com//webinar/4209">Registration</a></li>
</ul>
Attend this GC Live session to learn how the latest GC instruments can track historical maintenance events and display trend plots for easy interpretation.
<h5>5. Agilent Technologies: UV-VIS-NIR in Battery Development</h5>
<ul>
<li>Th, 15.8.2024 20:00 CEST</li>
<li><a href="https://gcms.cz/webinar/3909">Registration</a></li>
</ul>
Agilent&#39;s portfolio of instruments offers the high performance and flexible accessories needed for pioneering new applications.
<h5>6. Agilent Technologies/Markes International: Environmental Air Monitoring: Methodologies, Regulations, and Market Trends</h5>
<ul>
<li>Tu, 20.8.2024 10:30 CEST</li>
<li><a href="https://gcms.labrulez.com/webinar/4187">Registration</a></li>
</ul>
An in-depth webinar on environmental air quality monitoring application solutions, organized by Agilent Technologies in collaboration with Markes International.

Webinars LabRulezGCMS Week 33-34/2024

A comparison of sensory evaluation and an electronic nose assay in the assessment of aroma in dry hopped beers

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 5th August 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!
<blockquote>
<h4>👉 <a href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></h4>
</blockquote>
<blockquote>
👉 Need info about different analytical techniques? Peek into <a href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.
</blockquote>
This week we bring to you applications and other documents by LECO, Agilent Technologies, Waters Corporation, and Shimadzu!
<h4>1. LECO: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Essential_Oil_Fragrance_Samples_BT_G_Cx_GC_Paradigm_Shift_SA_CK_ANALYTIKA_SA_24_LPSS_318_8458df1480.pdf">Non-Target Characterization of Complex Essential Oil and Fragrance Samples with GCxGC-MS/FID for Reliable Identification and Relative Quantitation in a Single Injection</a></h4>
<ul>
<li>poster / Analytica</li>
</ul>
Introduction: Essential oils are extracts from plant materials that capture the plant&#39;s scent and flavors. They have a broad range of applications, as they can be both a finished product and an ingredient or intermediate in the creation of other products. Due to this versatility, the analysis of essential oils is an important area of research with a variety of analytical objectives. 
Because flavors and fragrances are composed of tens or hundreds of ingredients, characterization of these individual species can be challenging. It is not practical to use numerous standards for the identification and quantification of all the individual species. Instead, it is common to use a workflow where MS provides identification and FID provides relative area % quantification, often with separate injections for each.
Additionally, two one-dimensional chromatographic separations with different stationary phases are also often required to isolate the individual compounds due to the complexity of these samples. Here, we demonstrate a possible improvement to this workflow by using a GCxGC-TOFMS/FID instrument that provides reliable identification and relative quantitation in a single injection. GCxGC provides enhanced chromatographic separation of individual analytes, thus removing the requirement for two separate 1D analyses. Coupling this with dual MS and FID detection enables both identification via the FID in one single injection.
Conclusion: Harnessing the power of a TOFMS coupled with a GCxGC platform and an FID allowed us to not only determine the presence and amounts of targeted analytes, but also discover non-target analytes.
This platform, based on GCxGC-TOFMS/FID, can improve workflows in your industry.
<h4>2. Shimadzu: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00788_en_8355bce383.pdf">Comprehensive Characterization of Diesel Fuel on GC×GC Utilizing Impressive High-Speed Scan Technology of GCMS-QP2050</a></h4>
<ul>
<li>Application</li>
</ul>
User Benefits
<ul>
<li>Comprehensive characterization of complex matrices such as diesel fuel is possible with 2D gas chromatography.</li>
<li>The impressive high-speed scan technology of GCMS-QP2050 allows for effective peak separation.</li>
<li>Intuitive comprehension of compounds distribution can be achieved with displaying the data in a two-dimensional image.</li>
</ul>
Introduction: Kerosene, diesel, and other petroleum products are mixtures containing over 100 different hydrocarbons. The properties of petroleum products, such as ignitability and viscosity, depend on their composition and greatly affect physical properties like combustion. Comprehensive two-dimensional gas chromatography (GC×GC) offers high separation performance by utilizing two different columns, which provides more reliable compositional information for complex mixtures compared to one-dimensional chromatography. In this application, qualitative analysis of diesel fuel using a GC×GC system with GCMS-QP2050 that is capable of high-speed scanning (30,000 u/sec) was conducted. No less than 30,000 u/sec scanning speed improved the separation of peaks that are too close to each other and enabled accurate identification of compounds.
Conclusion: Diesel, a complex mixture of hydrocarbons, was measured using GC×GC-MS. Each component on the two-dimensional image showed characteristic distribution based on its molecular structure, allowing for intuitively understanding of the composition of diesel. Additionally, GC×GC-MS demonstrated Excellentseparation performance for components, enabling more reliable identification of components of diesel compared to 1D GC-MS. The high-speed scan of GCMS-QP2050 (30,000 u/sec) contributesto more precise qualification analysis.
<h4>3. Shimadzu: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_05_sca_280_108_en_d87677c8a2.pdf">Analysis of Trialkyl Phosphates as Markers for Lithium Battery Aging</a></h4>
<ul>
<li>Application</li>
</ul>
User Benefits
<ul>
<li>Lithium Batteries(LIB) decomposition and aging can be evaluated by monitoring Trialkyl Phosphates.</li>
<li>A routine and fast GCMS method for the detection of Trialkyl Phosphates was developed.</li>
<li>Trialkyl Phosphates can be detected with high sensitivity and selectivity in commercial liquid electrolytes</li>
</ul>
Introduction: The electrolyte solution is a crucial part of a typical Lithium-ion battery, consisting of Li salts (e.g. LiPF6), and organic carbonates. Decomposition and formation of phosphorous-based and other organic products starts already at the production stage of the electrolyte. The formation of such molecules does not affect the electrolyte/battery quality negatively, as long as the quantity is low enough. On the contrary, several decomposition products have a positive effect on the formation of the so-called SEI surface (Solid Electrolyte Interface) on the LIB anodes, which is crucial for the battery functionality. Nevertheless, this is a continuous chemical process and the increasing amount of some of the decomposition products is a clear indicator of the progressive aging of the battery/electrolyte. This application is demonstrating the GCMS analysis of Trialkyl Phosphates as reaction products of carbonates and LiPF6 salt. The choice of this compounds as markers for electrochemical battery aging is due to the fact, that their formation is very slow and depends only on a few external parameters, allowing to investigate the electrochemical aging (charge/discharge) by a simple comparison of before/after analyte content.
Conclusion: The presented application demonstrated the suitability of GCMS to investigate the aging of the LIBs using phosphatebased degradation products. This investigation is based on SCAN measurements. Here, a SCAN/SIM mode would be beneficial offering the possibility to detect the main compounds (carbonated, additives) and the degradation products in one measurement. A further improvement would be a dedicated SIM method for the mentioned phosphates with the highest selectivity and sensitivity.
<h4>4. Agilent Technologies: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_dithiocarbamate_pesticide_tea_gc_5994_7663en_agilent_78da56d0be.pdf">Analysis of Dithiocarbamate Pesticides in Tea Using GC/MS/MS</a></h4>
<ul>
<li>Application Note -Food Testing and Agriculture</li>
</ul>
Abstract: Dithiocarbamate pesticides are commonly used to control fungal diseases in ornamental plants and crops, and for control of tea gray blight. The residue definition for dithiocarbamate pesticides is expressed as total dithiocarbamate, determined as mg CS₂/kg. Methods for analysis of CS₂ use extraction of the sample into an acidified stannous chloride solution with isooctane, where the dithiocarbamate residues are converted to CS₂, which is captured in isooctane and analyzed by GC/MS. This application note describes the analysis of dithiocarbamate residues in tea using an Agilent GC/MS/MS in both SIM and MRM modes. A limit of quantification of 10 ppb was achieved in tea samples. Linearity was established in matrix-matched standards with R2 &gt; 0.999 for the range from 5 to 100 ppb, with average recoveries &gt; 85% at the 10 ppb level of fortification.
Conclusion: Analysis of dithiocarbamate pesticides as CS₂, using isooctane as a sample preparation solvent, can lead to the combination of a relatively high boiling solvent with low boiling analytes. Hot spitless injections result in poor peak shapes for CS₂; better peak shapes can be obtained with cold injection in split mode. Further improvement in peak shapes can be achieved by using a multibaffled liner. Matrixmatched calibration standards ranging from 5 to 100 ppb were used to assess calibration performance, with linearity established at R² &gt; 0.999 in both SIM and MS/MS modes. The method was validated following the criteria specified in SANTE 11312/2021v2, with the ability to detect CS₂ peaks down to 5 ppb using Agilent 7000D, 7000E, and 7010C GC/MS/MS instruments. Implementing a backflush method in the GC/MS analysis of tea samples can significantly improve the separation of target analytes from complex matrix components, enhancing sensitivity and throughput. Repeatability tests showed RSDs consistently below 4.2% for injections at 10 ppb concentration, indicating high precision and repeatability 
<h4>5. Waters Corporation: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008300_en_1dd7d73213.pdf">Converting Target Analysis of Organochlorine Pesticides in Environmental Matrices from Electron Ionization GC-HRMS Using Helium Carrier Gas to Atmospheric Pressure Ionization GC-MS/MS Using Nitrogen Carrier Gas</a></h4>
<ul>
<li>Application Note</li>
</ul>
Abstract: Organochlorine pesticides (OCPs) are among the high production volume chemicals produced in the past that had wide application and exhibit significant persistence in the environment. DDT, for example, has a half-life in sediment of up to 15 years meaning that it may not be 90% degraded for 45 to 60 years.¹ Furthermore, they are associated with a number of negative health effects when bioaccumulated in humans and animals. These are among the reasons that nine of the initial 12 compounds addressed by the 2004 Stockholm Convention on Persistent Organic Pollutants (POPs) belong to this compound class.² 
Due to the complexity of matrices, such as sediment and biota, encountered when monitoring the fate, transportand occurrence of these compounds, it is necessary to employ techniques with high sensitivity, specificity, and robustness for these studies. In the past this has required the use of complex sample extraction and clean-up combined with electron ionization (EI) and high resolution mass spectrometry (HRMS) using magnetic sector instrumentation. However, in recent years the performance of Gas Chromatography Atmospheric Pressure Ionization Tandem Quadrupole Mass Spectrometry (GC-APCI-MS/MS) has demonstrated equal or better performance than the classic technique.³ In this work the Atmospheric Pressure Gas Chromatography (APGC™) ionization source on a Xevo™ TQ-XS Tandem Quadrupole System was used with both helium (He) and nitrogen (N₂) carrier gas to analyze sediment and biota extracts for the presence of 39 OCPs. Performance characteristics and sample quantification results for APGC-MS/MS were compared with results for the same aliquots run using GC-EI-HRMS.
Conclusion: The GC-EI-HRMS reference method separations and runtime were matched on the APGC-MS/MS system with only minor modification to the He carrier gas flowrate. Scaling of the column dimensions for use with N₂ carrier gas effectively reproduced the reference method separations and total runtime which allows the use of the same acquisition and processing files across both configurations. The comparison between the APGC He and N₂ carrier gas data shows that sensitivity is also maintained within a factor of two times between the two carrier gases. Analysis of extracted samples of biota and sediment indicate good agreement between the APGC N₂ carrier gas method and the EI HRMS reference method values. These results demonstrate the feasibility of modernizing the traditional reference method with a technique that is more easily integrated into most labs and more accessible for most operators.

News from LabRulezGCMS Library - Week 32, 2024

In the research article recently published in ACS Analytical Chemistry journal the researchers Weier Hao and Daniel B. Cardin from Entech Instruments Inc., describe a Full Evaporative Vacuum Extraction (FEVE) method for efficient analysis of a wide range of semivolatile organic compounds (SVOCs) in water.
This study introduces a Full Evaporative Vacuum Extraction (FEVE) method for analyzing (<a href="https://gcms.labrulez.com/library?search=SVOCs">semivolatile organic compounds SVOCs</a>) in drinking and surface water using sorbent pens. The method involves a two-stage process to capture both lighter and heavier SVOCs, followed by desorption into a GC-MS with optimized parameters for enhanced sensitivity. The sorbent pens can be stored for up to 10 days with minimal loss in analyte recovery. Testing 10 water samples, the method detected 69 analytes, none of which exceeded California Proposition 65 safety limits.
<blockquote>
<h4>The original article</h4>
</blockquote>
<blockquote>
<h5><a href="https://pubs.acs.org/doi/10.1021/acs.analchem.2c03414">Full Evaporative Vacuum Extraction─A Quantitative and Green Approach for Analysis of Semivolatile Organic Compounds in Drinking Water and Surface Water Using GC–MS</a></h5>
Weier Hao, Daniel B. Cardin
Analytical Chemistry 2023 95 (8), 2959-3967
DOI: 10.1021/acs.analchem.2c03414
<h6>licensed under <a href="https://creativecommons.org/licenses/by/4.0/">CC-BY 4.0</a></h6>
</blockquote>
<h5>Selected sections from the article follow.</h5>
<h3>Abstract</h3>
Full evaporative vacuum extraction (FEVE) was developed in this work for analysis of a broad range of semivolatile organic compounds (SVOCs) in drinking water and surface water. Sorbent pens are used in a two-stage process that first evaporates the sample matrix through sorbent beds under vacuum to recover the lighter SVOCs, followed by the application of a higher temperature and stronger vacuum to the sample vial to recover the remaining heavier SVOCs once the matrix has evaporated. After extraction, the sorbent pens are desorbed into a GC–MS using a uniquely designed “splitless” delivery system to maximize sensitivity. Critical extraction and desorption parameters that affect the method performance were optimized. After FEVE, the sorbent pens can be stored for 7–10 days at room temperature while maintaining a less than 15% loss in analyte recovery. As a proof of concept, 10 drinking water and surface water samples were analyzed using this method. 69 analytes were detected in these water samples, with the highest concentration of 1986 ng/L for bromacil. Heptachlor epoxide, chlorpyrifos, metolachlor, butachlor, and 2,3′,4′,5-tetrachlorobiphenyl were detected in four samples. None of the analytes were above the health and safety thresholds set by California Proposition 65.
<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Analytical_Chemistry_2023_95_8_2959_3967_cover_image_95d3812bb7.jpg" alt="Anal. Chem. 2023, 95 (8), 3959-3967: graphical abstract."/>
<h3>Experimental Section</h3>
<h4>Design of FEVE</h4>
The <a href="https://gcms.labrulez.com/library?instrumentationItems=8&amp;manufacturerItems=42&amp;search=FEVE">FEVE sorbent pen</a> (FSP) has a special design that extends into the neck of 2 mL FEVE sample vials to ensure recovery of heavy SVOCs. To capture a broad range of SVOCs, the sorbent bed consists of two sorbents in series: first, PDMS-coated glass beads and then 35/60 mesh Tenax TA. This FSP design is shown in <a href="https://pubs.acs.org/doi/10.1021/acs.analchem.2c03414#fig1">Figure 1</a>. PDMS-coated glass beads were chosen as a first bed to minimize the desorption heat needed to recover the heavier and the more thermally labile compounds, thereby optimizing their recoveries. For analysis of more volatile compounds, a stronger third sorbent like Carboxen or Carbosieve can be added in the FSP to capture these lighter compounds. However, for the suite of SVOCs in this study, a third sorbent was not necessary.
<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Analytical_Chemistry_Anal_Chem_2023_95_8_2959_3967_Figure_1_Photograph_a_and_cross_section_b_of_an_FSP_showing_the_internal_sorbent_beds_PDMS_coated_glass_beads_red_and_Tenax_white_b3702abd97.jpg" alt="Anal. Chem. 2023, 95 (8), 2959-3967: Figure 1. Photograph (a) and cross-section (b) of an FSP showing the internal sorbent beds: PDMS-coated glass beads (red) and Tenax (white). The FSPs are stored in a sleeve when not in use (c)."/>
As shown in <a href="https://pubs.acs.org/doi/10.1021/acs.analchem.2c03414#fig2">Figure 2</a>, a 2 mL sample vial with 1 mL of the water sample was attached to an FEVE vacuum sleeve, and then, an FSP was inserted. A silicone O-ring was placed between the top of the sample vial and the bottom of the vacuum sleeve to create a leak-tight seal. The FEVE assemblies were placed into the extraction module shown in <a href="https://pubs.acs.org/doi/10.1021/acs.analchem.2c03414#fig3">Figure 3</a>. A top plate was used to compress the two upper vacuum sleeve O-rings against the vacuum manifold to ensure a leak-tight seal. The multi-position design of the manifold allows for up to 30 samples to be extracted simultaneously.
<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Analytical_Chemistry_Anal_Chem_2023_95_8_2959_3967_Figure_2_Components_comprising_the_FEVE_sample_assembly_including_2_m_L_sample_vial_with_1_m_L_of_the_water_sample_a_FEVE_vacuum_aa27c782ef.jpg" alt="Anal. Chem. 2023, 95 (8), 2959-3967: Figure 2. Components comprising the FEVE sample assembly, including 2 mL sample vial with 1 mL of the water sample (a), FEVE vacuum sleeve with a vial nut and silicone O-rings (b), and FSP (c). Photograph (d) and cross-section of the completed assembly showing the entrance of the FSP extending into the vial to ensure recovery of heavy SVOCs (e)."/>
<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Analytical_Chemistry_Anal_Chem_2023_95_8_2959_3967_Figure_3_Front_cross_section_view_of_the_FEVE_module_during_extraction_of_multiple_water_samples_a_Top_down_view_of_the_FEVE_top_plate_f257be0976.jpg" alt=" Anal. Chem. 2023, 95 (8), 2959-3967: Figure 3. Front cross-section view of the FEVE module during extraction of multiple water samples (a). Top-down view of the FEVE top plate, FSP cooling fan, vacuum output, and 30 FEVE sample assemblies in place (b)."/>
The FEVE process consists of four major steps: vacuum verification, matrix evaporation, high-vacuum dehydration, and high-temperature diffusive desorption. During vacuum verification, the FEVE instrument is pumped down through the low-vac valve to reach a target vacuum pressure. Then, the valve is turned off, and the rate of pressure increase is used to determine whether the system is leak-tight. After the vacuum verification standard is met, the matrix evaporation starts. The low-vac valve is left on to help slowly remove the water matrix under vacuum. When the pressure of the instrument drops below 10 Torr, the process advances to high-vacuum dehydration, where the high-vac valve is turned on to provide a stronger vacuum, pulling the remaining volatile matrix in the vial through the FSP sorbents to the pump. When the pressure drops to 1 Torr, the sample vials are heated at 200 °C for 7.5 min. This step helps transfer the heavier SVOCs from the vials to the sorbents. An FSP cooling fan is turned on at this stage to keep the FSP sorbent cool to maximize its adsorption capacity. After the vial heater is cooled down, the FSPs are ready for <a href="https://gcms.labrulez.com/library?instrumentationItems=8&amp;manufacturerItems=42&amp;search=TD%E2%80%93GC%E2%80%93MS">TD–GC–MS</a> analysis. The entire FEVE process takes 4–6 h, depending on the number of samples extracted simultaneously. Extraction of 30 samples in 6 h equates to an average time of 12 min per sample. As this is approximately half the time of a standard GC cycle, one FEVE system can provide maximum throughput for two GC–MS systems.
<h4>TD and GC–MS</h4>
After completion of the FEVE extraction process, the FSPs were loaded into a 30-position sorbent pen sample tray. The sample handling was performed using an SPR40 sample preparation rail (Entech Instruments) with full automation. The 5800-SPDU Sorbent Pen Desorption Unit (Entech Instruments) was used as the TD system to deliver the analytes to the GC–MS. A <a href="https://gcms.labrulez.com/library?instrumentationItems=3&amp;mainauthorItems=10&amp;search=5977c">7890B/5977C GC–MS (Agilent Technologies, Santa Clara, CA)</a> was used for optimization of the extraction and desorption parameters. A <a href="https://gcms.labrulez.com/library?instrumentationItems=3&amp;mainauthorItems=3&amp;search=ISQ+7000">Trace 1310/ISQ 7000 GC–MS (Thermo Fisher Scientific, Waltham, MA)</a> with an advanced electron impact ion source operating in the selected ion monitoring mode was utilized to further optimize the detection limits of the method, evaluate the method, and analyze the water samples. A UAC-1MS precolumn (5 m × 0.53 mm × 0.15 μm, methylpolysiloxane; Quadrex Corp, Bethany, CT) was used to collect the SVOCs during sample desorption while using a 7–8 mL/min flow rate, with excess flow eliminated through a split tee positioned at the junction between the precolumn and the analytical column. The analytical column used for GC separation was an Agilent HP-5MS (30 m × 0.25 mm × 0.5 μm, 5%-phenyl-methylpolysiloxane). The carrier gas was helium, at a flow rate of 1.2 mL/min.
<a href="https://pubs.acs.org/doi/10.1021/acs.analchem.2c03414#fig4">Figure 4</a> shows the configuration of the 5800-SPDU, the precolumn (column 1), the analytical column (column 2), and the flow and split control. This design of the instrument enables sorbent pen pre-purging and pre-heating, desorption, GC delivery, split control, and residual backflushing during the analysis of each sample. After an FSP is inserted into the desorption unit, valves 2 and 4 are turned on during preheating, thereby bypassing the FSP. Once the desorption starts, valves 1 and 4 are turned on, enabling desorption flow through the FSP to deliver SVOCs to column 1. During desorption, compounds more volatile than the lightest analyte of interest are split out through valve 4. After desorption, valves 1 and 3 are tuned on, allowing the analytes to proceed splitlessly to column 2. By using a thicker film on column 2 than that on column 1, the analytes dynamically refocus on column 2, resulting in narrower chromatographic peaks. In practice, column 2 with a film thickness of 0.25 or 0.5 μm is recommended, while column 1 is 0.15 μm. The length of column 1 can be greater than 5 m if longer desorption time is needed. During transfer of the analytes in the two columns, the desorption unit is baked at 260 °C to eliminate potential carryover in the FSP. After the heaviest analyte of interest is eluted out from column 1 and starts separating on column 2, valves 2 and 3 are turned on to backflush unwanted heavy compounds out through the entrance of column 1. Finally, the desorption unit cools down and returns to the idle status where valves 2 and 4 are on and ready for the next sample. The valve controls and flow directions of each stage are shown in <a href="https://pubs.acs.org/doi/suppl/10.1021/acs.analchem.2c03414/suppl_file/ac2c03414_si_001.pdf">Figure S2</a> in the Supporting Information. The GC oven temperature was held at 40 °C for 3 min during sample desorption, ramped at 12 °C/min to 160 °C, then ramped at 8 °C/min to 320 °C, and held for 1 min until the end of the run. Data acquisition and analysis were performed using Agilent <a href="https://gcms.labrulez.com/library?instrumentationItems=22&amp;manufacturerItems=1&amp;search=MassHunter+Workstation">MassHunter Workstation</a>, Thermo <a href="https://gcms.labrulez.com/library?instrumentationItems=22&amp;manufacturerItems=2&amp;search=Chromeleon">Chromeleon</a>, Entech SPRINT software, and Microsoft Excel.
<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Analytical_Chemistry_Anal_Chem_2023_95_8_2959_3967_Figure_4_Configuration_of_the_5800_SPDU_two_column_design_and_split_control_of_the_TD_GC_MS_system_Column_1_Quadrex_UAC_1_MS_55fcff8331.jpg" alt="Anal. Chem. 2023, 95 (8), 2959-3967: Figure 4. Configuration of the 5800-SPDU, two column design, and split control of the TD–GC–MS system. Column 1: Quadrex UAC-1MS (5 m × 0.53 mm × 0.15 μm). Column 2: Agilent HP-5MS (30 m × 0.25 mm × 0.5 μm)."/>
<h3>Conclusions</h3>
In this work, FEVE, a quantitative and green approach, was designed, developed, evaluated, and applied to analysis of 123 SVOCs in drinking water and surface water samples. This method enables quantification of a broad range of semivolatile compounds simultaneously, meanwhile providing a high level of sensitivity, accuracy, and precision. The extraction and analysis process is highly automated, enabling a simple and efficient workflow for analytical laboratories, and completely eliminates the use of solvents during sampling, analysis, and cleanup. Besides drinking water and surface water, FEVE also has the potential to be applied to other matrices. For example, for analysis of more complex environmental, biological, and foodstuff samples, after a simple pre-extraction to remove suspendid solids in the samples, a mixture of water and extract can be analyzed using FEVE. A 6 mL version of the FEVE technology will also be available to analyze up to 5 mL of the sample, which can further lower the detection limits.

Full Evaporative Vacuum Extraction─A Quantitative and Green Approach for Analysis of Semivolatile Organic Compounds in Drinking Water and Surface Water Using GC–MS

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

News from LabRulezGCMS Library - Week 33, 2024

In the 2 weeks from August 19, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.
<blockquote>
<h4><a href="https://gcms.labrulez.com/webinars">👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</a></h4>
</blockquote>
<blockquote>
👉 Search and filter in the largest global database with over 3 500 GC, LC, MS and spectroscopy webinars.
</blockquote>
<h5>1. Agilent Technologies/Markes International: Environmental Air Monitoring: Methodologies, Regulations, and Market Trends</h5>
<ul>
<li>Tu, 20.8.2024 10:30 CEST</li>
<li><a href="https://gcms.labrulez.com/webinar/4187">Registration</a></li>
</ul>
An in-depth webinar on environmental air quality monitoring application solutions, organized by Agilent Technologies in collaboration with Markes International.
<h5>2. Wasson-ECE Instrumentation: Single Cylinder Sample Heater (New Product)</h5>
<ul>
<li>Tu, 27.8.2024 21:30 CEST</li>
<li><a href="https://gcms.labrulez.com/webinar/4216">Registration</a></li>
</ul>
Please join us for an introduction to Wasson&#39;s new Single Cylinder Heater/Auto Sampler.
<h5>3. Thermo Fisher Scientific: Improved EA-IRMS NCS workflow for archaeology and ecology applications</h5>
<ul>
<li>We, 28.8.2024 16:00 CEST</li>
<li><a href="https://gcms.labrulez.com/webinar/4210">Registration</a></li>
</ul>
This presentation will describe how we have optimized our Thermo Scientific EA IsoLink System with the new High Performance Kit for sulfur analysis to allow for high precision and accuracy NCS analysis.
<h5>4. LECO: Non-targeted screening in forensics, a discussion of method development and screening of forensic samples using GCXGC-TOFMS</h5>
<ul>
<li>Th, 29.8.2024 14:00 CEST</li>
<li><a href="https://gcms.labrulez.com/webinar/4212">Registration</a></li>
</ul>
Non-targeted screening in forensics, a discussion of method development and screening of forensic samples using GCXGC-TOFMS.

Webinars LabRulezGCMS Week 34-35/2024

In the research article published in ACS Analytical Chemistry journal the researchers from the University of Natural Resources and Life Sciences, BOKU Vienna, and from Novartis Technical Operations Anti-Infectives, MS&amp;T Laboratories reported a new approach towards the quantification of N-acetylglucosamine in biotechnological cell samples using <a href="https://gcms.labrulez.com/library?instrumentationItems=4">GC–MS/MS</a> and <a href="https://gcms.labrulez.com/library?instrumentationItems=13">GC–TOFMS</a>.
N-Acetylglucosamine is a crucial component of bacterial and fungal cell walls and the extracellular matrix in animals, playing roles in cell surface structure and signaling pathways. Given the challenges in distinguishing its stereoisomers, which share identical masses and similar fragmentation patterns, efficient separation techniques are essential. A gas chromatography method using automated online derivatization was developed for precise quantification of these stereoisomers. This approach, combined with ¹³C-labeled internal standards and mass spectrometric analysis, allows accurate detection of low-abundance stereoisomers, as demonstrated in Penicillium chrysogenum cultivations with strong consistency across different mass spectrometric techniques.
<blockquote>
<h4>The original article</h4>
</blockquote>
<blockquote>
<h5><a href="https://pubs.acs.org/doi/10.1021/acs.analchem.9b04582">Selective and Accurate Quantification of N-Acetylglucosamine in Biotechnological Cell Samples via GC–MS/MS and GC–TOFMS</a></h5>
Teresa Mairinger, Michael Weiner, Stephan Hann, and Christina Troyer
Analytical Chemistry 2020 92 (7), 4875-4883
DOI: 10.1021/acs.analchem.9b04582
<h6>licensed under <a href="https://creativecommons.org/licenses/by/4.0/">CC-BY 4.0</a></h6>
</blockquote>
<h5>Selected sections from the article follow.</h5>
<h3>Abstract</h3>
N-Acetylglucosamine is a key component of bacterial and fungal cell walls and of the extracellular matrix of animal cells. It plays a variety of roles at the cell surface structure and is under discussion to be involved in signaling pathways. The presence of a number of N-acetylhexosamine stereoisomers in samples of biological or biotechnological origin demands for dedicated high efficiency separation methods, due to identical exact mass and similar fragmentation patterns of the stereoisomers. Gas chromatography offers high sample capacity, separation efficiency, and precision under repeatability conditions of measurement, which is a necessity for the analysis of low abundant stereoisomers in biological samples. Automated online derivatization facilitates to overcome the main obstacle for the use of gas chromatography in metabolomics, namely, the derivatization of polar metabolites prior to analysis. Using alkoximation and subsequent trimethylsilylation, carbohydrates and their derivatives are known to show several derivatives, since derivatization is incomplete as well as highly matrix dependent inherent to the high number of functional groups present in carbohydrates. A method based on efficient separation of ethoximated and trimethylsilylated N-acetylglucosamines was developed. Accurate absolute quantification is enabled using biologically derived ¹³C labeled internal standards eliminating systematic errors related to sample pretreatment and analysis. Due to the lack of certified reference materials, a methodological comparison between tandem and time-of-flight mass spectrometric instrumentation was performed for mass spectrometric assessment of trueness. Both methods showed limits of detection in the lower femtomol range. The methods were applied to biological samples of Penicillium chrysogenum cultivations with different matrices revealing excellent agreement of both mass spectrometric techniques.
<h3>Experimental Section</h3>
<h4>Automated Derivatization</h4>
The two-step derivatization of samples and standards with (1) ethylhydroxylamine or methylhydroxylamine hydrochloride and (2) MSTFA with 1% TMCS was performed automatically on a Gerstel <a href="https://gcms.labrulez.com/library?mainauthorItems=2&amp;search=MPS2+dual+rail+sample+preparation+robot">MPS2 dual rail sample preparation robot</a> (Gerstel GmbH, Muehlheim, Germany). The robot was equipped with two parallel rails, each carrying a robotic tower capable of performing independent liquid handling steps. One tower was equipped with a 10 μL syringe for sample injection; the second tower was equipped with a 100 μL syringe for the addition of the reagents. Both towers were also in use for transportation of the samples. Each rail was equipped with a heated agitator for derivatization. Underivatized dried samples were stored at 6 °C in a cooled stack until the onset of just-in-time derivatization. Reagents were stored at 6 °C in a Peltier cooled tray. Sample preparation as well as the injection were controlled by the <a href="https://gcms.labrulez.com/library?mainauthorItems=2&amp;search=Maestro">Maestro software</a> package 1.4.30.6. (Gerstel), which was linked with the <a href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=MassHunter">MassHunter</a> Acquisition software B07.06 (Agilent Technologies Inc.).
For derivatization and analysis, aliquots of 60 μL of standards, 50 μL of extracts, 80 μL of washing and quenching solutions, and 120 μL of the cultivation supernatant were used. The ratio of internal standard volume/sample volume was 0.2 for extracts, 0.15 for washing and quenching solutions, and 0.1 for supernatants.
20 μL of O-ethylhydroxylamine hydrochloride in pyridine (c(EtOX) = 20 mg mL−1) was added to the spiked samples and standards prior to drying in a vacuum centrifuge, in order to prevent the degradation of keto carbonyl group containing compounds. (23) The samples were evaporated to complete dryness at pressures of &lt;1 mbar to ensure efficient and quick drying at low temperatures. Dried samples were immediately crimped with magnetic caps to enable transportation on the robot and were placed in the drawer cooled stack (6 °C) of the MPS 2 autosampler until derivatization. If dried samples were not analyzed within 24 h, they were redried before analysis. In the first derivatization step, the samples were dissolved in 18 μL of water-free pyridine containing 19 mg mL–1 EtOx. The samples were incubated (25 °C, 120 min) under agitation (250 rpm) to convert ketone and aldehyde carbonyl groups into ethylhydroxylamino groups. Subsequently, 42 μL of MSTFA with 1% TMCS were added and the samples were heated and agitated (250 rpm) at 40 °C for 50 min to replace acidic protons by trimethylsilyl groups. Syringes were washed with pyridine before and after each liquid dosage. After a cool down to room temperature for 1.5 min in an open tray of the MPS2, samples were cooled in the cooled stack at 6 °C for 5 min and were then injected for GC–MS analysis. After injection, samples were placed back into the cooled tray at 6 °C. Derivatization was controlled by Maestro software package (Gerstel). Sequences were scheduled in a way that samples were derivatized during the GC runs of the preceding samples, hence enabling injection of the derivatized samples immediately after sample preparation was finished.
<h4>GC–MS/MS and GC–TOFMS Analysis</h4>
GC separation was carried out on <a href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=Agilent+7890B">Agilent 7890B</a> gas chromatographs coupled either with an Agilent Technologies <a href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7200B+Q-TOF">7200B</a> Q-TOF (GC–TOFMS) mass spectrometer or with an Agilent Technologies <a href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7010B+Triple+Quadrupole">7010B Triple Quadrupole</a> (GC–MS/MS) mass spectrometer (Agilent Technologies Inc.). Both GC–MS systems were equipped with (1) a nonpolar deactivated precolumn (3 m × 0.25 μm i.d., Phenomenex), which was connected to the analytical column via a backflush unit (purged ultimate union), and (2) a nonpolar deactivated postcolumn (3 m × 0.18 μm i.d., Phenomenex), which was connected with the analytical column via a second ultimate union T-piece serving as a restrictor column to the MS. The following analytical columns were tested: ZORBAX DB-5MS + 10 m Duragard capillary column (5% phenyl–95% dimethylpolysiloxane, 30 m × 250 μm × 0.25 μm) from Agilent Technologies Inc., and Optima 5 MS Accent (5% phenyl–95% dimethylpolysiloxane, 60 m × 250 μm × 0.25 μm) and Optima 1 MS Accent (100% dimethylpolysiloxane, 30 m × 250 μm × 0.25 μm), both from Macherey Nagel. The GC–QTOFMS instrument was equipped with an Agilent split/splitless injector, whereas the GC–MS/MS was equipped with an Agilent Multi Mode Inlet. Agilent Ultra Inert splitless liners with a single taper were used. Sample aliquots of 1 μL were injected in the splitless mode (220 °C, splitless time 2 min, septum purge flow 3 mL min–1). The following GC-temperature program was used: 70 °C (hold for 1 min), 30 °C min–1 to 240 °C, 2 °C min–1 to 260 °C, with 30 °C min–1 to 310 °C (hold for 3 min). The transfer line to the MS was kept at 280 °C. Helium 5.0 was used as carrier gas with a constant flow of 1.1 mL min–1 for the precolumn, 1.2 mL min–1 for the analytical column, and 1.4 mL min–1 for the post column. The electron ionization (EI) source of the instruments was operated with an electron energy of 70 eV and an emission current of 35 μA for the QTOF and 100 μA for the MS/MS at a temperature of 230 °C. For both instruments, the quadrupole was set at 150 °C. For chemical ionization (CI), an emission current of 10 μA was used, the ion source was operated at 150 °C, and a reagent gas flow of 20% CH4 (corresponding to 1 mL min–1) was employed. (24) The QTOF was operated in TOF-mode with a scan speed of 3.33 Hz and in 2 GHz Extended Dynamic Range mode. The mass accuracy was &lt;2 ppm for the calibration ions and resolution at approximately 8000 RFWHM at m/z 501.9706. Mass spectra were acquired in profile mode and were converted postacquisition to centroid. The GC–MS/MS system was operated with 3.5 Hz, and the resolution was set to widest (corresponding to a mass isolation window of 2.5 m/z) for both mass selective quadrupoles. For data evaluation, MassHunter Quantitative analysis B.08.00 (Agilent Technologies Inc.) was used.
<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Analytical_Chemistry_Anal_Chem_2020_92_7_4875_4883_Figure_1_Extracted_ion_chromatograms_GC_CI_TOF_of_the_three_biologically_relevant_N_acetylated_hexosamines_i_e_b8d10f631c.jpg" alt="Anal. Chem. 2020, 92, 7, 4875-4883: Figure 1. Extracted ion chromatograms (GC–CI-TOF) of the three biologically relevant N-acetylated hexosamines, i.e., N-acetylglucosamine (GlcNAc), N-acetylgalactosamine (GalNAc), andN-acetylmannosamine (ManNAc), using two different oximation reagents, namely, MOX and ETOX (dotted and dashed lines, respectively). For this purpose, the [M – CH₃]⁺ of the respective cis and trans 4TMS derivative was extracted. (a) Separation using a 60 m Optima 1 MS column is depicted. (b) Separation using a 60 m Optima 5 MS is shown."/>
<h3>Conclusions</h3>
A robust and highly selective GC based separation method with mass spectrometric detection for GlcNAc was validated and successfully employed for the analysis of biotechnologically relevant Penicillium chrysogenum samples. GlcNAc was detectable in all biological sample types. The presence of GlcNAc in the cultivation supernatant underlines the relevance of a separate sampling/preparation procedure for quenching supernatant, washing supernatant, cultivation supernatant, and cell-extract in combination with a robust quantification method for accurate intracellular balancing of GlcNAc in biological samples. In contrast to matrices like urine or blood plasma, the matrix of biotechnological samples can change vastly in the course of a batch or fed-batch experiment. This highly concentrated matrix clearly leads to a rapid degradation of the performance of the GC–MS system, more specifically S/N ratio and sensitivity. This heavy matrix, together with the strong matrix dependence of the derivatization efficiency, renders internal standardization with stable isotope labeling indispensable.
Nevertheless, the present method proved to be robust, since even after more than 50 injections, concentrations of less than 30 nmol L⁻¹ were still possible to be quantified. GC–MS instruments with automated liner exchange and ion source cleaning systems could restore the performance of the system within sequences.
A comparison of MS/MS and TOFMS shows comparable validation results with the exception of the linear range, which is more limited for TOFMS. However, TOFMS shows the advantage of changing data evaluation strategies retrospectively, such as the use of lower abundant isotopologues for peak integration in case of detector saturation. By this means, the full potential of TOFMS for accurate quantitation can be exploited.

Selective and Accurate Quantification of N-Acetylglucosamine in Biotechnological Cell Samples via GC–MS/MS and GC–TOFMS

In the week from August 26, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.<blockquote><h4><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars">👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</a></h4></blockquote><blockquote>👉 Search and filter in the largest global database with over 3 500 GC, LC, MS and spectroscopy webinars.</blockquote><h5>1. Wasson-ECE Instrumentation: Single Cylinder Sample Heater (New Product)</h5><ul><li>Tu, 27.8.2024 21:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4216">Registration</a></li></ul>Please join us for an introduction to Wasson's new Single Cylinder Heater/Auto Sampler.<h5>2. Thermo Fisher Scientific: Improved EA-IRMS NCS workflow for archaeology and ecology applications</h5><ul><li>We, 28.8.2024 16:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4210">Registration</a></li></ul>This presentation will describe how we have optimized our Thermo Scientific EA IsoLink System with the new High Performance Kit for sulfur analysis to allow for high precision and accuracy NCS analysis.<h5>3. LECO: Non-targeted screening in forensics, a discussion of method development and screening of forensic samples using GCXGC-TOFMS</h5><ul><li>Th, 29.8.2024 14:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4212">Registration</a></li></ul>Non-targeted screening in forensics, a discussion of method development and screening of forensic samples using GCXGC-TOFMS.

Webinars LabRulezGCMS Week 35/2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 19th August 2024? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!
<blockquote>
<h4>👉 <a href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></h4>
</blockquote>
<blockquote>
👉 Need info about different analytical techniques? Peek into <a href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.
</blockquote>
This week we bring to you a posters from <a href="https://gcms.labrulez.com/events/568">ASMS 2024</a> by LECO, Agilent Technologies, Shimadzu, and Thermo Fisher Scientific!
<h4>1. LECO: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/NIST_LIBRARY_MATCH_QUALITY_HRT_MMS_CF_ASMS_24_LPSS_320_90d3c6e8c9.pdf">Evaluation of the NIST Library Matching Quality of Mass Spectra Generated by the GC-HR-TOFMS with Multi-Mode Ionization Source</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
Introduction: Comparison of electron ionization spectra against standardized libraries is a staple approach to compound identification in non-targeted GC-MS analysis. High-quality matches are central to the pace of, and confidence in, such analyses. Recent developments in gas chromatography high resolution mass spectrometry have progressed non-targeted analysis applications to a wide variety of studies. However, modern ion-optical design principles which allow gains in sensitivity and resolving power may inadvertently alter fragmentation patterns, which may in turn affect the reliability of automated comparisons against standard libraries. Thus, thorough evaluation and validation of the high-quality spectra matching to the standard libraries, like NIST, is necessary for comprehensive assessment of the promised benefits of new technologies.
Conclusions: This multi-mode ionization source, as assessed using these 207 diverse analytes, generates fragmentation patterns which align very well with the NIST spectral library. Across all analytes in standard solutions, the mean library match score was 935 and the standard deviation for this value was 24.2. Mean match scores were agreeable regardless of moieties present. Percent differences for MRPS #2 spiked into a Pu’er Tea and MRPS #8 spiked into a dietary supplement were - 3.75 % and -1.44 %, illustrating how the system can easily maintain spectral confidence even in complex matrices. Overall, this study suggests the electron ionization mode of this multimode ion source, in combination with its high-resolution time of flight mass analyzer, yields spectra in excellent agreement with the quadruple dominated NIST library.
<h4>2. Agilent Technologies: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_7000d_mrm_fast_analysis_enviro_compounds_asms_2024_thp360_en_agilent_d338929001.pdf">Fast Analysis of 140 Environmental Compounds by GC/MS/MS</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
Introduction: Pesticides, polycyclic aromatic hydrocarbons (PAHs), and polychlorinated biphenyls (PCBs) are persistent environmental pollutants with the potential for bioaccumulation.¹ Previously, these compound classes have been analyzed using gas chromatography with an electron capture detector (GC-ECD), but this requires full chromatographic separation of all analytes for confident chemical identification. With a triple quadrupole detector (QQQ), analysis time significantly drops due to mass identification eliminating the need to chromatographically separate all components. Further, multiple reaction monitoring (MRM) mode on the QQQ provides a higher confidence in peak identification than analysis by scan or selected ion monitoring (SIM) mode. Combining chromatographic separation and MS/MS analysis is especially useful for PAHs and PCBs where multiple analytes may have the same m/z value.
Conclusions: Transitioning methods from GC-ECD to GC/MS/MS is highly beneficial.
By running in MRM mode, we enable the following:
<ul>
<li>Significant time-savings</li>
<li>Increased confidence in hits</li>
<li>Sample quantification remains the same</li>
</ul>
<h4>3. Shimadzu: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Th_P364_Novel_High_Sensitivity_Detector_for_GCMS_adcdac36c4.pdf">Novel High Sensitivity Detector for GC/MS</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
Overview
<ul>
<li>We have developed a novel high sensitivity detector which has a simple structure to achieve high ion transmission and eliminate neutral molecules simultaneously.</li>
<li>Signal to noise ratio (S/N) was 1.5 times higher than that with a conventional detector.</li>
</ul>
Introduction: 
In GC/MS, numerous neutral molecules originated from carrier gas pass through quadrupole mass filter without being removed, and thereby they are finally transferred to ion detector. When they enter the detector, they may cause noise in the detecting signal. For this problem, some detector structures have already been proposed to remove these neutral molecules. However, they have complex structures and the room for improvement of ion transmission. In this study, we have developed the new high sensitivity detector which has a simple structure to achieve high ion transmission and to eliminate neutral molecules simultaneously.
Conclusions:
<ul>
<li>We have developed the new high sensitivity detector and achieved the high ion transmission and removal of neutral molecules simultaneously.</li>
<li>Signal intensity was increased by 1.2 times and noise was reduced by about 20%, S/N was 1.5 times higher than that with the conventional detector.</li>
<li>This noise reduction effect will be larger in the high flow analysis. In addition, this detector is promising to extend the lifetime of the detector due to less contamination from neutral particles in the conversion dynode and electron multiplier.</li>
</ul>
<h4>4. Thermo Fisher Scientific: <a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_142_utilizing_hydrogen_pesticides_food_gc_ms_po142_asms2024_en_7ed0951b93.pdf">Utilizing hydrogen carrier gas for sensitive analysis of pesticides in food using gas chromatography mass spectrometry</a></h4>
<ul>
<li>poster / <a href="https://gcms.labrulez.com/companies/296">ASMS 2024</a></li>
</ul>
<h5>Abstract</h5>
Purpose: To demonstrate the performance of the Thermo Scientifc HeSaverH2Safer kit for iConnect split-splitless (SSL) injection module for trace analysis of pesticides using H2 as a carrier gas as a safe and sustainable solution for laboratory operations 
Methods: In this study, hydrogen was used as a carrier gas for GC-MS/MS analysis of trace levels of pesticides in food. The GC was fitted with a new hydrogen safer split/splitless injector, with chromatographic separation performed on a TG-5 SIL MS (30 m × 0.25 mm, 0.25 μm) capillary GC column. The chromatographic conditions applied ensured critical pair separation was achieved. The GC-MS/MS system was equipped with an advanced electron ionization (AEI) source to increase sensitivity for analyte detection. Quantification and assessment of critical regulatory requirements, such as linearity and sensitivity, were performed in a single software.
<h5>Conclusions</h5>
<ul>
<li>The use of the HeSaver-H2Safer technology allows for a safe and compliant use of hydrogen as an alternative carrier gas in GC/GC-MS applications without the need to install a hydrogen sensor and removes any risk of unwanted reactions with the sample in the hot SSL injector.</li>
<li>When used with hydrogen, the limited carrier gas consumption offered by the HeSaverH2Safer mode permits a very controlled system demand for hydrogen, making this solution ideal for laboratories working with hydrogen generators.</li>
<li>Migrating the GC-MS/MS method from helium to hydrogen requires an adaptation of method parameters to address (i.e., retention time shift and different fragmentation patterns).</li>
<li>97% of pesticides in baby food and 98% in honey showed a linear response in the concentration range 0.005–0.500 mg/kg and the relative standard deviation for N=5 repeats of each sample type at 0.01 mg/kg was equal or lower than 10% for 98% of the evaluated compounds.</li>
</ul>

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News from LabRulezGCMS Library - Week 34, 2024

Selective and Accurate Quantification of N-Acetylglucosamine in Biotechnological Cell Samples via GC–MS/MS and GC–TOFMS

Webinars LabRulezGCMS Week 35/2024

News from LabRulezGCMS Library - Week 33, 2024

Full Evaporative Vacuum Extraction─A Quantitative and Green Approach for Analysis of Semivolatile Organic Compounds in Drinking Water and Surface Water Using GC–MS

Webinars LabRulezGCMS Week 34-35/2024

News from LabRulezGCMS Library - Week 32, 2024

A comparison of sensory evaluation and an electronic nose assay in the assessment of aroma in dry hopped beers

Webinars LabRulezGCMS Week 33-34/2024

News from LabRulezGCMS Library - Week 31, 2024

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