News from LabRulezLCMS Library - Week 44, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 2nd February 2026? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies </strong>and<strong> Waters Corporation, </strong>technical note by<strong> Shimadzu </strong>and poster by <strong>Thermo Fisher Scientific / MSACL!</strong></p><h3><strong>1. Agilent Technologies: Quantitative Separation of THC Isomers and Metabolites from Whole Blood</strong></h3><p><strong>Using Agilent Captiva Enhanced Matrix Removal (EMR) cartridges and LC/MS/MS</strong></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_thc_isomers_captiva_emr_lctq_5994_8664en_agilent_5eb50dc6f9.pdf"><strong>Full PDF for download</strong></a></li></ul><p>THC isomers (Δ8- and Δ9-THC, in particular) are psychoactive compounds of increasing interest in forensic toxicology, where accurate identification and quantification of these individual isomers and their respective metabolites are essential for legal and clinical assessments. However, an analytical challenge derives from their structural or empirical similarity and the presence of potential isobaric interferences.&nbsp;</p><p>Isobaric compounds are molecules that are empirically identical, share the same nominal mass, but differ in structure. In the context of THC analysis, CBD and exo-THC are notable isobaric interferences. These compounds can coelute or produce overlapping mass spectral signals, complicating the interpretation of results. CBD, a nonpsychoactive cannabinoid, shares an identical molecular weight and similar fragmentation pattern with THC isomers, making it difficult to distinguish using conventional mass spectrometry alone. Exo-THC, another structural analog, further adds to the complexity for the same reasons.&nbsp;</p><p>Without adequate chromatographic separation, these isobaric interferences can lead to false positives or inaccurate quantitation. This is particularly problematic in forensic settings, where precise identification of psychoactive substances is critical. Therefore, a robust analytical method that can resolve these compounds and potential interferents is&nbsp;desirable.&nbsp;</p><p>This study introduces a workflow that combines enhanced matrix removal (EMR) with LC/MS/MS to achieve baseline separation of THC isomers and their metabolites from the isobaric interferences that were examined within the scope of this application note. The method enables confident separation, identification, and quantification in a single 15-minute analysis.</p><h4><strong>Experimental</strong></h4><h5><strong>Chromatographic separation and LC/MS/MS detection&nbsp;</strong></h5><p>This procedure can be accomplished using different instrument configurations. Chromatographic separation was verified using both an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1260+Infinity+II+LC"><strong>Agilent 1260 Infinity II LC</strong></a> and an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+Infinity+II+LC"><strong>Agilent&nbsp;1290 Infinity II LC</strong></a>. Analyte detection and quantitation were performed via both an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6475"><strong>Agilent 6475 triple quadrupole LC/MS</strong></a> and an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Ultivo"><strong>Agilent&nbsp;Ultivo triple quadrupole LC/MS</strong></a>. Method&nbsp;parameters are detailed in Tables 1 and 2. Detailed MRM transition settings are outlined in Appendix A.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This study presents an effective, integrated workflow for the separation and quantification of THC isomers and metabolites in whole blood. Agilent&nbsp;Captiva EMR–Lipid cartridges removed sufficient matrix interferences to enable clean extraction and high analyte recovery. Chromatographic separation using an Agilent InfinityLab Poroshell 120 PFP column provided reliable resolution of isobaric compounds, including CBD and exo-THC. Coupled with Agilent LC/MS/MS systems featuring Agilent Jet Stream ionization technology, the method delivered consistent sensitivity and selectivity across a complex panel of analytes. Together, this methodology offers the basis of a streamlined workflow for the separation of Δ8-, Δ9-, and Δ10-THC isomers and their respective hydroxy and carboxy metabolites and potential interferents from whole blood.</p><h3><strong>2. Shimadzu: Optimization of Supercritical Fluid Extraction Parameters for Vitamins D2, D3, and K1 from Pharmaceutical Preparations</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c190_e333_6198eb84b9.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Vitamins are organic compounds, essential in small amount, crucial for the normal functioning of the human body, facilitating numerous enzymatic and metabolic functions[1]. Since the human organism cannot produce vitamins, the diet represents the main route of ingestion of these compounds. As consumer awareness grows, reliable information about the vitamin content in foods is becoming a critical issue. However, considering that vitamins could be losses during food processing and storage, the readyto-use multi-vitamin pharmaceutical preparations are becoming widely employed among consumers. These facts, together with the introduction of labelling regulations, introduced the need for ensure the quality control of these types of formulation.</p><h4><strong>2. Experimental</strong></h4><h5><strong>2.3 Instrumentation</strong></h5><p>The supercritical fluid extraction (SFE) was carried out by using a SFE pretreatment system (<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+UC"><strong>Shimadzu Nexera UC</strong></a>) equipped with: a CBM-40 controller, an SFE-30A module, an LC-30ADSF CO2 pump, an LC-40D XR modifier pump, an LC-40D make-up pump, an SFC-30A back pressure regulator, a DGU-40 on-line degasser, an FRC-40 fraction collector. A combination of static and dynamic extraction was employed (Figure 2).</p><h4><strong>Conclusion&nbsp;</strong></h4><p>Considering the obtained results, the vitamins extraction revealed as strictly matrix dependent, according to the formulation excipients. Therefore, detailed study needs to be performed to better understand the vitamin formulation.</p><h3><strong>3. Thermo Fisher Scientific / MSACL: Simultaneous quantitation and discovery (SQUAD) of fecal bile acids and their conjugates in children with autism spectrum disorder (ASD)</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_squad_fecal_bile_acids_children_asd_po_en_af787058d3.pdf"><strong>Full PDF for download</strong></a></li></ul><p>This study presents a <strong>Simultaneous Quantitation and Discovery (SQUAD)</strong> metabolomics workflow applied to the analysis of <strong>fecal bile acids and their microbial conjugates</strong> in children with <strong>Autism Spectrum Disorder (ASD)</strong> undergoing <strong>microbiota transfer therapy (MTT)</strong>. Bile acids play a key role in lipid metabolism and gut–brain signaling, and alterations in gut microbiota composition in ASD have been linked to disrupted bile acid metabolism. The SQUAD approach was designed to address the need for both <strong>targeted quantification</strong> of known bile acids and <strong>untargeted discovery</strong> of novel metabolic features within a single LC–MS injection.</p><p>The workflow integrates <strong>reversed-phase liquid chromatography</strong> with advanced mass spectrometry using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/748"><strong>Thermo Scientific Orbitrap Ascend Tribrid mass spectrometer</strong></a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/744"><strong>Thermo Scientific Vanquish Horizon UHPLC system</strong></a>. Quantitative analysis was performed using <strong>parallel reaction monitoring (PRM)</strong> in the <strong>linear ion trap</strong>, while <strong>high-resolution MS¹ scanning in the Orbitrap</strong> enabled confident metabolite annotation. The Tribrid architecture—combining a quadrupole, linear ion trap, and Orbitrap—allowed high selectivity and sensitivity, including MSⁿ capabilities for resolving <strong>co-eluting structural isomers</strong> such as leucine- and isoleucine-conjugated bile acids.</p><p>Using calibrated bile acid standards, the method achieved <strong>absolute quantitation across six orders of magnitude</strong>, with limits of quantitation below <strong>1.8 femtomoles on column</strong>. The SQUAD workflow was applied to fecal samples collected before and after MTT, revealing <strong>distinct shifts in bile acid and lipid-related metabolite profiles</strong> following treatment. Multivariate analysis, including <strong>principal component analysis (PCA)</strong>, demonstrated clear separation between pre- and post-treatment samples in the MTT group, while no comparable changes were observed in placebo controls.</p><p>Overall, the results demonstrate that SQUAD metabolomics enables <strong>high-throughput, highly sensitive, and information-rich analysis</strong> by combining quantitative rigor with deep metabolic coverage in a single experiment. This integrated LC–MS workflow provides valuable insight into the biochemical effects of microbiome modulation in ASD and highlights the power of <strong>Orbitrap Tribrid–based metabolomics</strong> for studying complex host–microbiome interactions in clinical research.</p><h3><strong>4. Waters Corporation: Analysis of Organic Carbonates in Lithium- Ion Battery Electrolyte by High-Performance Liquid Chromatography (HPLC) with Mass Detection (MS)</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009211_en_46cbebda90.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>Benefits&nbsp;</strong></h5><ul><li>Sensitive method for low-level detection and quantification of carbonate solvents (0.05–1 ppm) and carbonate-based aging products (0.00075–0.0025 ppm) in lithium-ion battery electrolyte solutions using the ACQUITY QDa II Mass Detector with SIR acquisition mode.</li><li>Robust chromatographic separation using the XSelect Premier HSS PFP Column under 7 minutes analysis time, operated under reversed-phase conditions.</li></ul><p>The electrolyte is one of the main components in the lithium-ion battery.<sup>1,2</sup> It is a conductive solution that transports lithium ions from the cathode to the anode during the charging process. During discharge, the lithium ions flow from the anode to the cathode. The electrolyte solution is composed of lithium salt dissolved in a mixture of organic solvents.<sup>1,2</sup> The organic solvents are typically a mixture of cyclic and linear carbonates, including EC, PC, DMC, EMC, and DEC.<sup>2</sup> Lithium hexafluorophosphate (LiPF<sub>₆</sub>) is commonly used as the conducting lithium salt,<sup>2</sup> providing the necessary ionic conductivity for efficient battery operation.&nbsp;</p><p>The LiPF6 salt in carbonate-based systems can exhibit chemical and thermal instability, which can impact the performance of the lithium-ion batteries.<sup>2-4</sup> Electrolyte solutions can also degrade, forming aging products including DMDOHC and DEDOHC.<sup>2</sup> Various techniques are employed to investigate quality and properties of the electrolytes. Techniques such as scanning calorimetry (DSC) and thermogravimetric analysis (TGA) offer a comprehensive analysis of an electrolyte’s thermal properties, while rheology measures viscosity of the conductivity solutions.<sup>1</sup> Additionally, chromatographic methods are used to measure the quantity of carbonate solvents in electrolyte solutions.<sup>2-4</sup> Gas chromatography mass spectrometry (GC/MS) and liquid chromatography mass spectrometry (LC/MS) are common techniques used to investigate carbonate-based electrolytes.<sup>3</sup>&nbsp;</p><p>In this application note, an HPLC method with mass detection was developed for the analysis of five common carbonate solvents and two carbonate-based aging products (Table 1). The method employed an ACQUITY QDa II Mass Detector coupled with an Arc Premier System. Method performance characteristics including limit of detection (LOD), limit of quantification (LOQ), linearity and system suitability were demonstrated. Additionally, the developed method was applied for the analysis of LiPF<sub>6</sub><sup>-</sup>based electrolyte solution.</p><h4><strong>Experimental</strong></h4><h5><strong>Method Conditions&nbsp;</strong></h5><ul><li><strong>System: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/306"><strong>Arc Premier System</strong></a>, Column Manager with active pre-heating, PDA and the ACQUITY QDa II Mass Detector&nbsp;</li><li><strong>Column: </strong>XSelect Premier HSS PFP Column, 2.5 µm, 4.6 mm x 100 mm (Waters, p/n: 186010051)</li><li><strong>MS system: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1543"><strong>ACQUITY QDa II Mass Detector</strong></a></li></ul><h5><strong>Data Management&nbsp;</strong></h5><ul><li><strong>Chromatography data software (CDS): </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/627"><strong>Empower™ 3.6.1</strong></a></li></ul><h4><strong>Results and Discussion&nbsp;</strong></h4><p>Chromatographic columns with a wide range of selectivity were explored during this study to ensure separation between carbonate solvents and carbonate-based aging products. The selected columns (XSelect Premier CSH™ C18, XSelect Premier CSH Phenyl Hexyl, XSelect Premier HSS T3, XSelect Premier HSS PFP) were tested with acetonitrile and methanol solvents. The study showed that XSelect Premier HSS PFP Column with methanol provided the best retentivity and separation for all analytes (Figure 1). The method successfully separated carbonate solutions and carbonate-based aging products in less than a 7-minute gradient time. The MS total ion chromatogram (TIC) data was collected across the mass range of 35–300 Da using electrospray ionization in positive (ESI+) mode (Figure 1A). The mass spectral data facilitated quick and accurate identification of the components. The carbonate solvents formed [M + H]+ molecular ions, while the selected aging products formed sodium adducts, [M + Na]+. These ions were measured using a selected ion recording (SIR) acquisition mode, which determines intensity for a single ion of interest (Figure 1B).</p><h4><strong>Conclusion&nbsp;</strong></h4><p>A sensitive and reliable HPLC-MS method using the Arc Premier System coupled with the ACQUITY QDa II Mass Detector was developed for the analysis of carbonate solvents and carbonate-based aging products in lithium-ion battery electrolyte. This reversed-phase LC method successfully separated all five carbonate solvents (EC, PC, DMC, EMC, DEC) and two aging products (DMDOHC/DEDOHC) on an XSelect Premier HSS PFP Column. Low-level quantification limits were achieved using SIR acquisition mode ranging from 0.05 to 1 ppm and 0.00075–0.0025 ppm for carbonate solvents and aging products, respectively. The method was demonstrated to be applicable for the analysis of lithium-ion battery electrolyte.</p>

News from LabRulezLCMS Library - Week 06, 2026

News from LabRulezLCMS Library - Week 09, 2026

News from LabRulezLCMS Library - Week 20, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 13th July 2026? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you posters by <strong>Agilent Technologies / ASMS,&nbsp;</strong> <strong>MDCW / William &amp; Mary, </strong>and<strong> Thermo Fisher Scientific</strong> <strong>/ ASMS </strong>and technical note by <strong>Shimadzu!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Comprehensive PFAS Analysis in Textiles Using Triple Quadrupole GC/MS and LC/MS Workflows</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_pfas_textiles_gc_tq_lc_tq_wp_414_asms_2026_en_agilent_a1d50ab96c.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>Per- and polyfluoroalkyl substances (PFAS) are widely used in textiles to provide water-, stain-, and oil-repellent functionality. Increasing evidence of environmental and human-health risks has led to heightened global regulatory pressure, including REACH/POPs restrictions, and strengthened requirements from industry frameworks such as ZDHC, OEKO-TEX®, AFIRM, and Bluesign. These initiatives demand highly sensitive, reliable, and standardized analytical workflows capable of quantifying both volatile and non-volatile PFAS in diverse textile matrices. This study demonstrates end-to-end PFAS solutions aligned with EN 17681-1:2025, comprising heat- and ultrasound-assisted (HUA) extraction followed by GC/TQ and LC/TQ determination of volatile and non-volatile PFAS, respectively. The workflow enables robust quantification of a comprehensive PFAS panel in T-shirts, waterproof shorts, and socks.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumentation&nbsp;</strong></h5><p>A dual-platform analytical approach combining GC/TQ and LC/TQ systems was used to quantify over 100 PFAS across 14 chemical classes (Figure 1). More than 30 volatile PFAS were analyzed using an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890"><strong>Agilent 8890 GC</strong></a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7010D"><strong>7010D TQ</strong></a> and a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=DB-624"><strong>DB-624 column</strong></a>. Over 70 non-volatile PFAS were determined using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6475"><strong>Agilent 6475 LC/TQ</strong></a> paired with a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+infinity+III"><strong>1290 Infinity III UHPLC </strong></a>and a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=ZORBAX+RRHD+Eclipse+Plus+C18"><strong>ZORBAX RRHD Eclipse Plus C18</strong></a> column.</p><h4><strong>Conclusions</strong></h4><ul><li>A dual-platform approach deploys Agilent 8890 GC coupled with 7010D TQ and Agilent 1290 Infinity III LC with 6475A TQ system for volatile and non-volatile PFAS in textiles.&nbsp;</li><li>Fast and simplified workflow: Utilizes a streamlined protocol based on EN 17681-1:2025. The method enhances lab productivity by eliminating tedious evaporation and reconstitution steps.&nbsp;</li><li>Regulatory compliance: Effectively addresses increasing textile industry focus on PFAS monitoring and supports compliance with various regulatory standards and limit requirements for PFAS detection in textiles.</li></ul><h3><strong>2. MDCW / William &amp; Mary: The Effect Of Using Low-Bleed Columns In The First Dimension For Comprehensive Two-Dimensional Gas Chromatographic Analyses</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Webb_MDCW_Poster_2026_1_5657991949.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>In gas chromatography, the presence of column bleed impacts peak data quality. As siloxanebased stationary phase components fragment, they release bleed artifacts into the mass spectrometer (MS), producing interference and decreasing signal-to-noise ratios (S/N) of analytes. <sup>1</sup> When using comprehensive twodimensional gas chromatography (GC×GC), a secondary column with an orthogonal stationary phase is used in providing improved separation between column bleed and analytes. However, it also introduces more stationary phase that can be degraded to produce more bleed artifacts.</p><p>The goal of this research was to define how replacing the primary column in a GC×GC-MS system impacts the resulting S/N and analyte identification quality, in order to clarify how column bleed impacts analytes that appear to be chromatographically resolved from column artifacts in GC×GC output. This will demonstrate the advantage that low-bleed columns can provide for future analyses.</p><h5><strong>Methods</strong></h5><p>Samples analyzed were the Century Mix2 , containing approximately 100 different analytes within different classes (i.e. Century Mix2) and a 52- component Indoor Air Standard. Both were assessed using a 5% phenyl/95% dimethylsiloxane standard column in the first dimension and a (50%-phenyl)-methylpolysiloxane standard column in the second dimension. Samples were then reanalyzed with a low-bleed column replacement in the first dimension.</p><p>Analysis of the samples was performed using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/37"><strong>Pegasus BT4D GC×GCTOFMS</strong></a> with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/44"><strong>quad-jet dual-stage cryogenic modulator</strong></a><strong> </strong>(LECO Corporation). <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/41"><strong>ChromaTOF software</strong></a><strong> </strong>(LECO Corporation) was used to analyze the chromatographic data.</p><h4><strong>Conclusions</strong></h4><p>This work demonstrated that samples run with the low-bleed first dimension column showed a reduction in the presence of column bleed components identified and maintained or improved the quantitative signal-to-noise ratios of components compared to the samples run on standard first dimension columns. This showed that that low concentration analytes were more reliably detected in the absence of column bleed, even when contour plots showed physically resolved components. In the future, this can be applied to improve the resolution of complex samples and increase analyte signal.</p><h3><strong>3. Shimadzu: Dimethyl carbonate as a green organic modifier in supercritical fluid extraction of pesticide residue analysis in apple samples</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c190_e347_869b9e2ade.pdf"><strong>Full PDF for download</strong></a></li></ul><p>According to the Green Analytical Chemistry (GAC) principles[1], a highly promising strategy to minimize the side effects of analytical methods involves replacing potentially toxic solvents and/or obtained by non-renewable sources with more environmentally friendly alternatives. In this frame, dimethyl carbonate (DMC) is an environmentally friendly, non-corrosive, safe handling, and biodegradable chemical, extensively used in several application fields, such as pharmaceuticals, coatings, and lithium-ion battery electrolytes [2]. Additionally, instead of the historical use of toxic and corrosive phosgene as a carbonate source, simple and direct synthesis routes from carbon dioxide (CO2) have been proposed [3]. Thus, also falling within the “carbon capture and utilization” processes, ensuring the reduction of atmospheric CO2 concentration and its conversion into useful chemical products.&nbsp;</p><p>Firstly introduced in the second edition of the GlaxoSmithKline’s solvent selection guide, DMC has been included among the “few issues” solvents, along with water [4]. Thereafter, it has attracted widespread attention as a valuable chemical and/or solvent, and substantial research efforts have been made in the scientific community. Its potential as a green alternative to conventional solvents in both reversed-phase liquid chromatography [5–7] and supercritical fluid chromatography [8] has been explored. The extraction capabilities of DMC toward different target molecules have been also investigated. In 2022, Alfieri et al. optimized an ultrasoundassisted extraction of two lignans from Linum species [9]. The extraction performances of a panel of green solvents and two natural deep eutectic solvents (in combination with water in a solvent/water ratio of 80:20) were tested versus methanol and chloroform (used for comparison with published studies). The results showed that, in terms of purity and recovery, DMC was the optimal media for the 6-methoxypodophyllotoxin extraction. DMC has been also employed in an in-syringe extraction coupled to solid phase extraction to assess nicotine in environmental water and sportspersons’ urine samples [10]. Extracts enriched in oleanolic acid were obtained by solid-liquid extraction of grape pomace using DMC compared to other tested solvents (ethyl acetate, acetone, n-butanol) [11]. In addition to the highest obtained recovery value, the lowest co-extraction of other matrix components was also achieved.&nbsp;</p><p>Supercritical fluid extraction (SFE) represents a reliable alternative to conventional solvent-based extraction methods. Several advantages are provided when CO2 is employed as supercritical fluid due to its non-toxicity, non-flammability, abundancy, renewability (as a by-product of industrial processes, as fermentation or combustion), recyclability, and cost-effectiveness. Supercritical CO2 has a polarity similar to that of n-hexane; thus, the addition of a co-solvent is necessary for the extraction of polar molecules [12, 13].&nbsp;</p><p>This work aims to expand the use of DMC that, to the best of the author’s knowledge, is here firstly proposed as an organic modifier in SFE. The extraction efficiency and selectivity of DMC toward conventional solvents, such as acetonitrile (ACN) and bio-ethanol (EtOH) obtained from edible renewable feedstocks, has been evaluated for multi-residue analysis of pesticides (64 pesticides, representing diverse chemical classes, polarities, and molecular weights) in apple samples. Considering the sustainable and nontoxic nature of CO2 and DMC, the use of DMC in SFE represents a win-win combination. Thus, improving the overall sustainability and automation of the extraction process closely align with the GAC principles. Furthermore, in this research, always following the GAC principles, a low-pressure gas chromatography-tandem mass spectrometry (LP-GC-QqQMS) method was employed, allowing a greater sample loadability and a higher optimal linear velocity allowed by the vacuum conditions of the system, effectively reducing the analysis time at about 10 minutes [14, 15].</p><h4><strong>2. Materials and methods</strong></h4><h5><strong>2-3. Instrumentation</strong></h5><h5><strong>Low‑pressure gas chromatography triple quadrupole mass spectrometry&nbsp;</strong></h5><p>The LP-GC-QqQMS analyses were performed using a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GC-2010"><strong>GC-2010 Plus system</strong></a> (Shimadzu Corporation, Kyoto, Japan) coupled with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=8040"><strong>triple quadrupole mass spectrometer (TQ8040</strong></a>, Shimadzu). Injection was performed using an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=AOC-20i"><strong>AOC-20i autosampler</strong></a><strong> </strong>and<strong> </strong>a split/splitless injector (injection temperature 280 °C) equipped with a focus liner (volume: 810 μL). The injection was performed in splitless mode (3 μL) using the high-pressure injection mode function (290 kPa for 0.5 min).&nbsp;</p><p>To avoid that sub-ambient pressure conditions reach the injector, an uncoated column (0.48 m × 0.1 mm ID) was installed before the separation column, a non-polar Equity-5 [poly(5% diphenyl/95% dimethyl siloxane)] of the following dimension: 5 m × 0.53 mm ID × 0.53 μm df. Both the columns were provided by Merck KGaA. The oven was temperature programmed as follows: 40 °C (2 min) to 320 °C raised at 30 °C min−1. Helium was used as carrier gas with an average constant linear velocity of 100 cm s−1 (into the separation column).&nbsp;</p><p>Electron ionization was performed at 70 eV. The interface and ion source temperatures were 320 and 280 ˚C, respectively. The collision gas was argon at a pressure of 200 kPa. The targeted analyses were carried out in the multiple reaction monitoring (MRM) acquisition mode (acquisition frequency: 3.3 Hz). To ensure univocal identification, two different MRM transitions (quantifier and qualifier) were monitored for each compound (Table S1). The SCAN analysis was performed with an acquisition frequency of 3.3 Hz and a mass range of 50–600 m/z. The GCMS Solution v.4.45 software (Shimadzu) was used for data collection and processing.</p><h4><strong>4. Conclusions&nbsp;</strong></h4><p>Under the optimized extraction conditions, the use of DMC as a co-solvent in SFE demonstrated promising performance in the analysis of pesticide residues in apple samples. The method achieved an average extraction yield of 85% across the 64 analyzed pesticides, spanning a broad range of chemical classes, polarities, and molecular weights. Notably, DMC provided cleaner extracts with significantly lower amounts of co-extracted matrix components compared to conventional solvents like ACN and EtOH. Despite the recovery for certain analytes being below 70%, the results remained within acceptable precision limits according to SANTE guidelines. Overall, DMC not only fulfills the analytical requirements for pesticide residue determination but also offers a greener, more sustainable alternative that supports enhanced instrument maintenance and aligns with the principles of GAC.</p><h3><strong>4. Thermo Fisher Scientific / ASMS: Improved detection capabilities for polychlorinated dibenzo-p-dioxins/furans (PCDD/Fs) using GC Orbitrap MS</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_004693_lsms_pcdd_fs_exploris_gc_efs_po004693_asms2026_na_en_68e4d9e8b3.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Polychlorinated dibenzo-p-dioxins/furans (PCDD/F) analysis requires ultra-high sensitivity and selectivity due to their toxicity at trace levels. Regulatory compliance requires laboratories to adhere to strict analytical criteria (Figure 1). Through the integration of NVAEI source (NVAEI) with HRAM Thermo Scientific Orbitrap mass spectrometer, the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2419"><strong>Orbitrap Exploris GC S </strong></a>delivers mass resolution and accuracy that far exceed those required while delivering enhanced sensitivity required for pg/g (part per trillion (ppt)) detection within food and feed matrices.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>Enhanced sensitivity of the NeverVent AEI ion source coupled to the Orbitrap Exploris GC S delivers accurate quantitation down to 2 fg/μL (10 fg on column) of TCDD while meeting analytical criteria required for Dioxin analysis compliance.&nbsp;</p><p>Response of 2 fg/μL (10 fg on column) of TCDD standard remained stable over a 185-injection sequence of food/feed extract, demonstrating robust performance of the NeverVent AEI at maintaining trace level sensitivity.&nbsp;</p><p>Good agreement in the analysis of food and feed extracts preformed by GC-HRMS magnetic sector demonstrates the Orbitrap Exploris GC S can deliver accurate quantitation at and below regulatory limits.</p></div></div></div></div></div></div></section></div></div></div></div></div></div></section>

News from LabRulezGCMS Library - Week 29, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 17th August 2026? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you posters by <strong>Agilent Technologies / ASMS, Thermo Fisher Scientific / ASMS </strong>and<strong> Shimadzu / ASMS </strong>and application note by<strong> Waters Corporation!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Quantitation of N-Nitroso Duloxetine N-Nitrosamine Drug Substance Related Impurities (NDSRI) in API and Formulation by 6475 LC/TQ</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_drug_impurities_lc_tq_tp_402_asms_2026_en_agilent_b933b9bddf.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Nitrosamine impurities are nitroso derivatives where the nitroso group is attached to an amine. The active pharmaceutical ingredient (API) derived from a class of nitrosamines are known as N-nitrosamine drugsubstance-related impurities (NDSRI). Nitrosamine impurities in APIs and drug products pose safety concerns, even in small quantities, and thus are a major concern for drug makers [1].&nbsp;</p><p>Analytical methods must be sufficiently sensitive to quantify the nitrosamine of interest at levels as low as 10% of the specification limit and, where feasible, down to ≤5% of the specification limit, for the determination of the limit of detection. LC/MS/MS is an inherently selective and highly sensitive analytical technique that is well suited for the identification and quantification of trace-level impurities at extremely low concentrations. Consequently, LC/MS/MS has been widely adopted within the pharmaceutical industry, particularly for nitrosamine analysis [2-3].&nbsp;</p><p>Therefore, manufacturers must develop and qualify a dedicated analytical method that is appropriate for the specific sample matrix and targeted NDSRIs. An LC/MS/MS method based on multiple reaction monitoring (MRM) was developed for the detection and quantification of the N-nitroso duloxetine NDSRI impurity over a concentration range of 0.5 to 40 ppb (absolute standard concentration), using an atmospheric pressure chemical ionization (APCI) source on an Agilent 6475A LC/TQ instrument.</p><h4><strong>Experimental</strong></h4><ul><li><strong>MS:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6475"><strong>6475 Triple Quadrupole LC/MS System</strong></a></li><li><strong>Column:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Poroshell+HPH+C18"><strong>Poroshell HPH C18</strong></a> (4.6*150mm, 2.7µm)</li></ul><h4><strong>Conclusions</strong></h4><ul><li>A highly sensitive and robust MRM LC/MS/MS method was developed for the quantitation of N-nitroso duloxetine in duloxetine hydrochloride API and finished formulation using the Agilent 6475A LC/TQ.&nbsp;</li><li>The optimized chromatographic conditions provided effective separation of the analyte from the API, placebo, and formulation matrices, ensuring reliable quantitation.&nbsp;</li><li>The calibration curve was linear over the concentration range of 0.5-40 ng/mL, with 1/x weighting. R and R2 values were observed for both to be greater than 0.99.&nbsp;</li><li>Recovery studies demonstrated efficient sample extraction, with recoveries ranging from 92-99% in API samples and 109-116% in pellet formulations at the LOQ, specification, and 200% specification levels.&nbsp;</li><li>The method also showed excellent reproducibility across all evaluated concentration levels, confirming its suitability for routine analysis.</li></ul><h3><strong>2. Shimadzu / ASMS: Non-Targeted Analysis of Per- and Polyfluoroalkyl Substances in Environmental Extracts by Microflow LC-QToF Coupled with Multi-spray ESI</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/TP_562_Non_Targeted_Analysis_of_Per_and_Polyfluoroalkyl_Substances_in_Environmental_Extracts_by_Microflow_LC_Q_To_F_Coupled_with_Multi_spray_ESI_c2a7e1d5bf.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Targeted screening methods are well established for monitoring Perand polyfluoroalkyl substances (PFAS) in environmental samples. However, PFAS comprise a large and evolving class of compounds, creating a need to screen existing, emerging, and transformation products across diverse matrices. Non-targeted Analysis (NTA) allows for the confirmation of suspected PFAS in the environment, but the sample characterization is often limited by analytical sensitivity. Microflow (0.5 – 40 µL/min) coupled with a multi-nozzle emitter enhances sensitivity by improving desolvation. When this is coupled to a high mass accuracy and resolution Quadrupole Time-ofFlight Mass Spectrometer (QToF), capable of data-dependent and independent MS/MS, PFAS characterization of unknown analytes is possible. In this study, various environmental extracts were processed and screened using NTA for PFAS compounds.</p><h4><strong>Methods</strong></h4><p>A <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+Mikros"><strong>Shimadzu Nexera Mikros LC</strong> </a>was used to introduce the sample to a Newomics DuoESI source with an M3 emitter on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=9050"><strong>LCMS-9050 QToF MS</strong></a> (Fig. 1). A direct injection on an octadecyl column without delay column was performed. Direct injection was chosen over trapand-elute configuration to minimize selectivity bias caused by the trap column.&nbsp;</p><h4><strong>Conclusion</strong></h4><p>With the increased sensitivity of microflow LC-QToF coupled with multi-spray ESI with DIA acquisition, Insight Explore aided in NTA PFAS analysis. When paired with Insight Discovery and Profiler, a streamlined batch data processing workflow with statistical analysis was shown to effectively handle complex environmental matrices and their analyses.</p><h3><strong>3. Thermo Fisher Scientific / ASMS: Robust and sensitive quantitation of 18 steroids in human serum using Thermo Scientific TSQ Certis Triple Quadrupole mass spectrometer</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_004707_lsms_18_steroids_tsq_certis_clinical_po004707_asms2026_na_en_244c52437b.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Accurate quantification of endogenous steroids in human serum is essential for biomonitoring physiological functions such as hormone regulation, reproduction, and immune response in clinical research laboratories. Liquid chromatography–tandem mass spectrometry (LC–MS/MS) is the gold standard for steroid analysis due to its superior sensitivity, selectivity, and multiplexing capability compared to immunoassays. However, steroid measurements remain challenging because of low endogenous concentrations and complex serum matrices. Here, we describe a robust and sensitive LC–MS/MS method for the simultaneous quantification of 18 steroids in human serum using the Thermo Scientific TSQ Certis triple quadrupole mass spectrometer (Figure 1). The method leverages advanced ion source design and fast acquisition to deliver enhanced sensitivity, stability and throughput suitable for high-volume laboratory workflows.</p><h4><strong>Materials and methods</strong></h4><h5><strong>Liquid chromatograph – mass spectrometry&nbsp;</strong></h5><p>Samples were analyzed on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/744"><strong>Thermo Scientific Vanquish Horizon UHPLC system</strong></a> coupled to the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2207"><strong>TSQ Certis MS</strong></a><strong> </strong>operated in selected reaction monitoring (SRM) mode. The mobile phase composition, analytical column details, LC gradient, and overlaid extracted ion chromatograms (EICs) are shown in Figure 3.&nbsp;</p><h5><strong>Data analysis&nbsp;</strong></h5><p>Data were acquired and processed using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/77"><strong>Thermo Scientific TraceFinder software</strong></a> (v 5.2).</p><h4><strong>Conclusions&nbsp;</strong></h4><p>A sensitive and robust LC–MS/MS method was developed for simultaneous quantification of 18 steroids in human serum using the Vanquish Horizon UHPLC and TSQ Certis MS with OptaMax Plus ion source. The method demonstrated excellent linearity, accuracy, and reproducibility across a wide dynamic range. Optimization of MS conditions, particularly vaporizer temperature, significantly improved sensitivity. Overall, the workflow delivers high sensitivity, selectivity, and long-term stability, providing a reliable solution for high-throughput steroid analysis in clinical and research settings.</p><h3><strong>4. Waters Corporation: Alkaline-hydrolysis Method for PFAS in Textiles and Textiles Products by Xevo™ TQ-S micro with ACQUITY™ UPLC™ H-Class Plus System</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009443_en_0ab4914d72.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><h5><strong>Benefits&nbsp;</strong></h5><ul><li>Alkaline hydrolysis method (EN 17681-1:2025) used for preparing textiles, coated textiles and textile products for PFAS analysis allowed the inclusion of side-chain fluorinated polymers&nbsp;</li><li>Extraction method provided significant advantages in handling complex textile matrices by creating clear extracts free from dispersions, settleable solids and particulates&nbsp;</li><li>Protected the high-value LC-MS/MS components from potential damage&nbsp;</li><li>The method improved analytical sensitivity, reproducibility and accuracy, enabled cost-effective and timeefficient PFAS analysis maintained high analytical quality even for challenging high-matrix samples</li></ul><p>Many PFAS are linked to health concerns because of their ability to interfere with the body’s hormone systems, acting as endocrine disruptors also, linked to other toxic effects. Since textiles come into direct and prolonged contact with the skin, there is an increased risk of human exposure—especially for babies and children.4 In addition, PFAS pose significant environmental concerns. These “forever chemicals” do not readily break down and can be released during manufacturing, washing and disposal, allowing them to enter water pathways and persist in the environment. As a result, testing for PFAS has become increasingly important in the textile industry to demonstrate supply chain transparency, build consumer trust and protect brand reputation.</p><p>Synthetic fluorinated chemicals are categorized into two main groups - non-polymeric PFAS and polymeric PFAS, known for their use as water and grease repellent, heat resistant finishes in textiles, upholstery, leather, apparel, carpet and other industrial applications such as packaging, firefighting foams, non-stick cookware, etc. (Figure 1). PFAS are fluorinated substances contain at least one fully fluorinated methyl or methylene carbon atom (without any H/Cl/Br/I atom attached to it), i.e. with a few noted exceptions, any chemical with at least a perfluorinated methyl group or a perfluorinated methylene group.2 PFAS are classified as long chain and short chain based on their perfluorinated carbon chain length. Short chain fluorinated polymers encompasses a diverse range of chemistries, categorized according to their generic chemical and repeating units structures. Few examples are: derivatives of fluorotelomers, perfluoropolyethers with varying carbon chain lengths and acrylates, epoxylates, urethane, silicones of repeated units based structures.3 Polyfluoroalkyl substances such as fluorotelomer alcohols (FTOHs) contain C–H bonds, rendering them more susceptible to degradation. The ethoxylates in fluorotelomers-methacrylate break down to FTOH whereas polymeric fluorinated urethanes, acrylates break down to PFCAs (non-polymeric and polymeric side chain fluorinated polymers). In contrast, perfluoroalkyl substances such as PFOS and PFOA are extremely persistent due to their fully fluorinated carbon chains.&nbsp;</p><p>In alkaline hydrolysis methods, methanolic aqueous sodium hydroxide is used to break down precursor PFAS such as FTOHs, branched side chain PFAS. This process releases terminal perfluorinated carboxylic acids (PFCAs), which can then be measured. However, the efficiency of hydrolysis varies among different PFAS compounds and the presence of interfering substances such as organic matter or other chemicals in the sample matrix can inhibit the cleavage and detection of these analytes.</p><h4><strong>Experimental</strong></h4><ul><li><strong>LC system:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/198"><strong>ACQUITY UPLC H-Class Plus System</strong></a> and SMFTN fitted with PFAS kit</li><li><strong>Column(s):</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1823"><strong>XBridge™ BEH™ C18 5 µm Column</strong></a>, 4.6 x 100 mm&nbsp;</li><li><strong>MS system: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/209"><strong>Xevo TQ-S micro Mass Spectrometer</strong></a></li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>By strictly following the critical steps of the alkaline hydrolysis method using methanolic aqueous sodium hydroxide (NaOH) both freely extractable PFAS and those previously bound within side-chain fluorinated polymers such as esters linked to fluorotelomer alcohols (n:2 FTOHs, where n = 4, 6, 8, 10, 12), can be effectively extracted. This approach also safeguards the LC-MS/MS instrumentation from blockages, damage, or contamination by preventing polymer accumulation and matrix interferences.&nbsp;</p><p>The analytical method using the ACQUITY UPLC H-Class Plus System and Xevo TQ-S micro LC-MS/MS System was found to be sensitive, reproducible and accurate, enabling cost-effective and time-efficient PFAS analysis in chemically processed textiles, coated textiles and textile products whilst maintaining high analytical quality even for challenging high-matrix samples.</p></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS Library - Week 34, 2026

News from LabRulezLCMS Library - Week 35, 2026

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

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A Hands‑On Spectroscopy Workshop in Agilent Wood Dale Center of Excellence

Bruker at the 7th European Symposium on Single Cell Proteomics

Shimadzu at 2026 AOAC Annual Meeting & Exposition

ICP-MS for Hybrid Photoelectrode Characterization

Addressing LC Method Optimization - Scaling For Efficiency, Throughput And Reproducibility

Proteoform Studio software, top down made simple