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

News from LabRulezGCMS Library - Week 30, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 22th July 2024? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!
<blockquote>
<h4>👉 <a href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></h4>
</blockquote>
<blockquote>
👉 Need info about different analytical techniques? Peek into <a href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.
</blockquote>
This week we bring to you poster presentations from <a href="https://lcms.labrulez.com/events/568">ASMS 2024</a> by Agilent Technologies, Shimadzu, Thermo Fisher Scientific, and Waters Corporation!
<blockquote>
💡 Almost 1000 ASMS posters and presentations <a href="https://lcms.labrulez.com/library?mainauthorItems=284">available in the LabRulezLCMS library</a> (unique search and filtering)
</blockquote>
<h4>1. Waters Corporation: <a href="https://lcms.cz/labrulez-bucket-strapi-h3hsga3/2023_asms_king_liver_178c54e990.pdf">HIGH THROUGHPUT PLASMA PROFILING OF HUMAN LIVER DISEASE SAMPLES USING RAPID CHROMATOGRAPHY AND A MULTI- REFLECTING TIME-OF-FLIGHT MASS SPECTROMETER</a></h4>
<ul>
<li>poster - ASMS 2024</li>
</ul>
Introduction: Metabolomics is a valuable research strategy in the determination FIG. 5 FIG. 1 FIG. 7 FIG. 3 of disease progression, disease stratification, the identification of biological markers for early diagnosis and for the development of new therapeutics. Acute-on-chronic liver failure (ACLF) is a condition characterized by systemic inflammation, multiple organ failure, and high short-term mortality1. ACLF develops from the acute decompensation of cirrhosis and currently there is no biomarker identified for the early diagnosis of this disease. Therefore, fully understanding the role metabolites and lipids play in the progression of ACLF and its underlining mechanisms could greatly help determine new diagnostic markers driving development of new therapeutics. Investigating biomarkers for large scale studies requires robust, high-throughput analytical methods.
Rapid microbore metabolic profiling (RAMMP) methods and conventional high-resolution mass spectrometry have previously been shown to considerably reduce analysis time2-3. Here we compare these methods with a vacuum jacketed column technology (VJC)4-5 and ultra high-resolution mass spectrometry6 for the analysis of plasma from liver disease patients by reversed- phase (RP) for lipid and hydrophilic interaction chromatography (HILIC) for small molecules.
Conclusion:
<ul>
<li>Conventional LC-MS methods used for large cohort studies suffer from batch response variation. The rapid chromatographic methods reduce this impact and demonstrated reproducible response across the entire batch of 168 injections per polarity (Fig. 2).</li>
<li>The SELECT SERIES MRT mass spectrometer generated highly accurate mass measurements (&lt;1 ppm), improving annotation confidence for both lipids and small molecules, including essential amino acids and carnitines from the HILIC analysis (Fig. 3).</li>
<li>PCA of the RAMMP data showed good analytical reproducibility from the clustered QC samples and group separation with some overlap between the different disease groups (Fig. 4).</li>
<li>Group comparisons were performed by OPLS-DA where statistically significant features were highlighted for database annotation (Fig. 5).</li>
<li>A number of lipids classes, particularly lysophosphatidylcholines (LPC), phosphatidylcholines (PC) and sphingomyelins (SM), showed dysregulation in the diseased samples when compared to healthy controls and were annotated through Lipostar2 with mass accuracies between 0.1-0.3 ppm (Fig. 6).</li>
<li>For the HILIC small molecule analysis, differences in amino acid response were detected in comparisons between diseased and healthy controls.</li>
<li>The SELECT SERIES MRT MS achieved mass resolution of 170-200K FWHM at 30 Hz compatible with RAMMP (a) and VJC (b) methodologies for example lipids, PC36:1 (0.18 ppm) and SM42:3, O2 (0.16 ppm), with the VJC providing better peak shape and resolution of adjacent peaks (Fig. 7)</li>
<li>Comparison of the RAMMP and VJC negative lipid analysis showed very similar distribution of disease and healthy control groups demonstrating minimal impact on the overall statistics (Fig. 8).</li>
<li>Both RAMMP and VJC methodologies combined with the SELECT SERIES MRT provided highly accurate reproducible metabolic profiling for a biomarker study, with the VJC providing improved peak fidelity complemented by the fast scanning high resolution capabilities of the SELECT SERIES MRT.</li>
<li>This work demonstrated an accurate, reproducible and high throughput metabolomic method for the rapid screening of a large number of biological samples for biomarker discovery.</li>
</ul>
<h4>2. Thermo Fisher Scientific: <a href="https://lcms.cz/labrulez-bucket-strapi-h3hsga3/po_143_characterization_structure_adenopeptin_lc_hram_ms_po143_asms2024_en_7ae893f36c.pdf">In-depth characterization and structure elucidation of non-ribosomal peptides related to adenopeptin using LC-HRAM-MSⁿ</a></h4>
<ul>
<li>Poster - ASMS 2024</li>
</ul>
<h5>Abstract</h5>
Purpose: Characterization of adenopeptin and related peptaibol analogs in a crude fermentation broth extract using LC-HRAM-MSn to identify adenopeptin congeners and elucidate their structures. Methods: Adenopeptin and its analogs were separated using reversed phase chromatography and analyzed using multi-stage fragmentation on a Thermo Scientific Orbitrap IQ-X Tribrid mass spectrometer. 
Results: Several analogs of adenopeptin differing by one or more methyl groups could be detected and the site of their modification could be narrowed to specific amino acid residues based on their fragmentation patterns.
<h5>Conclusions</h5>
The LC/MS analysis of the crude adenopeptin extract revealed the presence of eight analogs above 0.5% relative MS-abundance, mainly resulting from ”demethylations”, i.e., substitution of Aib for Iva residues. Their modification sites could be determined based on shifts in the fragmentation pattern relative to adenopeptin. Additionally, a potentially crucial substitution of pipecolic acid with proline could be detected and verified based on MS3 spectral evidence for compound 4.
<h4>3. Thermo Fisher Scientific: <a href="https://lcms.cz/labrulez-bucket-strapi-h3hsga3/po_146_evaluation_automated_low_flow_lc_ms_setup_po146_asms2024_en_1d935eb142.pdf">Evaluation of an Automated “Quick” Optimization Routine to Streamline Low-Flow LC-MS Setup</a></h4>
<ul>
<li>Poster - ASMS 2024</li>
</ul>
<h5>Abstract</h5>
Purpose: When setting up low flow LC-MS experiments, a user regularly positions an emitter at an arbitrary fixed distance from the inlet based on visual alignment. A prototype ion source featuring an emitter mounted on a 3D motorized stage was used to evaluate a “quick” optimization strategy used to define the active position for subsequent LC-MS measurements.
Methods: The basis of the quick optimization routine was established using m/z- and position-dependent intensity distributions. The routine was evaluated against two methods to manually set the emitter position.
Results: All optimization strategies yielded a statistically equivalent number of protein and peptide identifications. However, the quick optimization routine yielded superior peak area reproducibility that translated into significantly better emitter-to-emitter consistency.
<h4>4. Shimadzu: <a href="https://lcms.cz/labrulez-bucket-strapi-h3hsga3/ASMS_poster_PESI_v_DMS_170524_fed75d0c1e.pdf">DPiMS-MS (PESI) combined with vacuum differential mobility spectrometry for rapid forensic analysis.</a></h4>
<ul>
<li>Poster - ASMS 2024</li>
</ul>
Introduction
<ul>
<li>Ambient ionisation (AI) mass spectrometry techniques facilitate rapid turn-around of samples, often in a walk-up format with limited sample preparation, with obvious benefits for forensic applications.</li>
<li>The absence of a chromatographic separation enables sub-minute data acquisition. However, this comes with the cost of greater chance of problems with chemical noise and/or interference between isomeric/isobaric compounds.</li>
<li>One way to remove chemical noise and to separate interfering compounds is to add an ion mobility separation to the method.</li>
<li>Here we implement a novel low pressure differential mobility on a DPiMS-8060 (PESI) system and demonstrate performance for steroids and small molecule drugs in saliva.</li>
</ul>
Conclusion
<ul>
<li>These results demonstrate the potential of vDMS to enhance AIMS by removing chemical noise and separating isobaric species.</li>
<li>DPiMS-vDMS-8060 (PESI) retains the high acquisition speed of PESI while adding an additional dimension of separation.</li>
<li>The additional selectivity may lower the LOQ and reduce false positives.</li>
<li>vDMS-MS methods can be applied in a wide range of complex matrices (e.g. urine, plasma).</li>
</ul>
<h4>5. Shimadzu: <a href="https://lcms.cz/labrulez-bucket-strapi-h3hsga3/MP_045_Targeted_quantitative_screening_pesticides_using_high_resolution_DIA_spectral_library_matching_238a221a67.pdf">Targeted quantitative screening pesticides in food matrices using high resolution DIA spectral library matching.</a></h4>
<ul>
<li>Poster - ASMS 2024</li>
</ul>
Overview
<ul>
<li>A single, generic untargeted data independent acquisition (DIA) method was developed for the analysis of extended panels of pesticides in food matrices.</li>
<li>The high-resolution LC-MS/MS method was designed for multi-residue screening and quantitation of pesticides to meet the European Union SANTE 11312/2021 v2 guidelines capable of working with extended target pesticide panels.</li>
<li>The MS and DIA-MS/MS method was applied to quantify a routine panel of pesticides but also included an additional target panel of fungicides for qualitative screening.</li>
</ul>
Conclusions
<ul>
<li>Using a single generic LC-MS and DIA-MS/MS method targeted quantitation using ion ratio confirmation (to meet the EU SANTE guidelines) and extended search capabilities with library identification were supported.</li>
<li>The method results in the quantitation of &gt;250 pesticides at or below the default MRL concentration (10 µg/kg).</li>
</ul>
<h4>6. Shimadzu: <a href="https://lcms.cz/labrulez-bucket-strapi-h3hsga3/MP_045_Targeted_quantitative_screening_pesticides_using_high_resolution_DIA_spectral_library_matching_238a221a67.pdf">Identification of positional isomers of linoleic acid containing phospholipids involved in pancreatic ductal adenocarcinoma.</a></h4>
<ul>
<li>Poster - ASMS 2024</li>
</ul>
Overview
<ul>
<li>To enhance lipid identification, Oxygen Attachment Dissociation (OAD) MS/MS has been applied to provide double bond specific dissociation, enabling C=C position assignments.</li>
<li>High resolution OAD MS/MS was applied in positive and negative ion mode to provide further confidence in lipid identification in a pancreatic adenocarcinoma biomarker study</li>
</ul>
Conclusions
<ul>
<li>OAD-MS/MS is a high specificity fragmentation technique to enable C=C positional assignments in lipids. Analysis is easy to perform alongside CID-MS/MS and spectra are easy to interpret.</li>
<li>OAD-MS/MS has been applied to structurally characterize lipids found to be potential markers of PDAC in a previous study using high resolution metabolomics analysis by LC-CID-MS/MS and DPiMSᵗᵐ.</li>
<li>The use of this new technology aims to enhance pancreatic cancer research by providing more comprehensive identification needed to understand the biological roles of the lipids identified as potential markers of PDAC.</li>
</ul>
<h4>7. Agilent Technologies: <a href="https://lcms.cz/labrulez-bucket-strapi-h3hsga3/po_2dlc_6545xt_monitoring_oxidation_mabs_asms_2024_wp030_en_agilent_77f2bb18d5.pdf">Monitoring oxidation in recombinant monoclonal antibodies at subunit level through two-dimensional liquid chromatography coupled with mass spectrometry</a></h4>
<ul>
<li>Poster - ASMS 2024</li>
</ul>
Introduction: Oxidation, induced by reactive oxygen species, is a prevalent chemical modification in monoclonal antibodies (mAbs), affecting amino acid residues such as cysteine (C), methionine (M), tryptophan (W), tyrosine (Y), lysine (K), and others (Gupta et al., 2022). Each residue&#39;s oxidation uniquely influences the protein&#39;s structure and function. Methionine is highly prone to oxidation in mAbs, typically resulting in the formation of a methionine sulfoxide product with increased polarity. These methionine residues are found in both the antigen-binding (Fab) and effector activity (Fc) domains of a mAb, with those situated on the surface being particularly susceptible to oxidation (Hageman et al., 2019). The increasing popularity of two-dimensional liquid chromatography (2D-LC) has led to a significant rise in the integration of two complementary chromatographic techniques, coupled with mass spectrometry (MS), aiming to provide comprehensive insights into mAb post-translational modifications (PTMs) (Sarin et al., 2022). The proposed 2D WCX-RP-MS workflow enables the analysis of mAbs at the subunit level, providing an automated analytical platform for characterizing and identifying oxidized regions within both the Fc and Fab domains.
Conclusions: The oxidized peaks not resolved by 1D methods are successfully resolved by the D2 RPC column with additional HC-LC information. It should be highlighted that the proposed method completely uses MS compatible buffers and is a faster method to identify mAb modification and their correlation in different mAb fragments compared to the tedious bottomup approach. A general mAb bottom-up analysis takes up to 24-48 hours with the risk of sample loss, degradation, and induced modifications. In the present study, sample preparation took only 4-10 hours (depending on oxidation incubation), and sample analysis took only 3 hours. Hence, 7-13 hours is enough for the subunit analysis with a low risk of sample loss and degradation. The present study focuses on oxidation as the chemical modification of interest, but the workflow can be extended to other critical charge modifications easily resolved by the WCX column.
<h4>8. Agilent Technologies: <a href="https://lcms.cz/labrulez-bucket-strapi-h3hsga3/po_2dlc_6545xt_monitoring_oxidation_mabs_asms_2024_wp030_en_agilent_77f2bb18d5.pdf">Flash Characterization of mAbs Using a Combination of Reagents via Automated On-Line Microdroplet Reaction</a></h4>
<ul>
<li>Poster - ASMS 2024</li>
</ul>
Introduction: Recently, an unmodified Agilent Jet Stream ESI source (AJS) was used to demonstrate “Flash Characterization” of mAbs by microdroplet facilitated reductions or enzyme digestions with good reproducibility and high yield 1. These results motivated us to evaluate treatments that combined enzymatic digestion, reduction, and/or deglycosylation of mAb in a single microdroplet experiment. New optimization parameters for the Agilent Injection Program on Agilent 1290 Infinity II LC were presented. Microdroplet experiments, including GlycINATOR ® deglycosylation, the combination of IdeS cleavage and DTT reduction and IdeS cleavage and GlycINATOR ® deglycosylation were examined for reproducibility, intact mAb remaining after treatments and simplified subunit characterization. GlycINATOR is an endoglycosidase that cleaves N-linked glycans and leaves the core GlcNAc residue with or without a fucose on the asparagine. Additional antibodies of Herceptin and sigmamab are also studied with the combination treatment in the microdroplet reaction.
Conclusions: 
<ul>
<li>Flash Characterization of mAbs with an automatic injector, combination treatments, and microdroplet reaction in the AJS source demonstrates simplification, reproducibility, and cost reduction of protein characterization. </li>
<li>Combination treatments are viable with microdroplet reactions to accelerate the reduction, cleavage, and deglycosylation of native IgG1 significantly.</li>
</ul>

News from LabRulezLCMS Library - Week 30, 2024

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