<div><p><span><strong>Flame retardant chemicals help prevent fires and save lives. They are widely used in indoor spaces—from homes and offices to airplanes and cars. However, one environment has largely escaped scientific attention: the inside of cruise ships. These floating cities are packed with furniture, electronics, and synthetic materials, yet little is known about the chemicals passengers and crew may be exposed to during long voyages.&nbsp;</strong></span></p></div><p><span>In the&nbsp;largest&nbsp;study of its kind,&nbsp;researchers from RECETOX and the Norwegian Institute of Water Research (NIVA)&nbsp;examined indoor dust from three expedition cruise ships&nbsp;in the North Atlantic Ocean.&nbsp;The ships&nbsp;differed in age and renovation history. Dust samples were collected from a range of locations on <strong>each vessel, including cabins,&nbsp;common areas, and workspaces</strong>. Scientists&nbsp;analyzed&nbsp;dozens of flame retardants, including older chemicals that are now restricted in many countries and newer replacements that are still widely used.&nbsp;</span></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/RECETOX_Nove_poznatky_o_chemickych_latkach_na_vyletnich_lodich_c578ce9b5d.jpg" alt="RECETOX: Revealing hidden chemicals at sea: A makeshift laboratory onboard to assemble passive air samplers." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_RECETOX_Nove_poznatky_o_chemickych_latkach_na_vyletnich_lodich_c578ce9b5d.jpg 208w," sizes="100vw" width="575" height="431"></p><div><p><span>The results revealed that flame retardants were present everywhere - but not evenly distributed. Some areas contained levels up to ten times higher than others, particularly spaces filled with electronics or soft furnishings. The most abundant chemicals were organophosphate flame retardants, especially one called <strong>TCIPP</strong>, which reached extremely high concentrations in some samples.&nbsp;</span></p><p><i>“Older ships had overall higher levels of flame retardants than the newer vessels, which likely reflects the types of materials used in the past and earlier fire‑safety standards. Using exposure models, we also estimated how much of these chemicals people on board may be ingesting or absorbing each day. The estimates suggest that crew members, who spend many months living and working on the ships, may experience higher exposure during routine activities - for example through contact with surfaces or the unintentional ingestion of dust,”</i> says the <strong>study’s lead author, Veronica van der Schyff</strong>.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/RECETOX_Nove_poznatky_o_chemickych_latkach_na_vyletnich_lodich_2_82d0edab27.jpg" alt="RECETOX: Revealing hidden chemicals at sea: Outdoor air sampler setup." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_RECETOX_Nove_poznatky_o_chemickych_latkach_na_vyletnich_lodich_2_82d0edab27.jpg 245w," sizes="100vw" width="770" height="282"></p><p>While strict fire-safety standards are mandatory for ships, there are currently no rules limiting which flame retardant chemicals can be used or how much is allowed. This study highlights an important gap in maritime safety regulations and raises questions about long-term chemical exposure in enclosed ship environments.&nbsp;</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/RECETOX_Nove_poznatky_o_chemickych_latkach_na_vyletnich_lodich_3_0da5788276.jpg" alt="RECETOX: Revealing hidden chemicals at sea: Dust collection with a vacuum cleaner." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_RECETOX_Nove_poznatky_o_chemickych_latkach_na_vyletnich_lodich_3_0da5788276.jpg 245w," sizes="100vw" width="775" height="282"></p><p>As cruise tourism, and the maritime industry, continues to grow, the findings underscore the need for closer monitoring and smarter regulation; ensuring that protecting ships from fire does not come at the cost of crew and passenger health.&nbsp;</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.rsc.org/en/content/articlelanding/2026/va/d5va00257e"><strong>Flame retardants in dust from the indoor environments of expedition cruise ships</strong></a></h4><p>Veronica van der Schyff, Verena Meraldi, Andrew Luke King, Simona Rozárka Jílková, Ondřej Audy, Petr Kukučka, Jiří Kohoutek, Lisa Melymuk</p><p><i><strong>Environ. Sci.: Adv.</strong></i>, 2026,<strong>5</strong>, 86-97</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1039/D5VA00257E">https://doi.org/10.1039/D5VA00257E</a></p><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/3.0/"><strong>CC-BY 3.0</strong></a></h6></blockquote><h4><strong>Abstract</strong></h4><p>Flame retardants (FRs) are widely used in indoor environments to meet fire safety requirements. One understudied environment with respect to indoor chemical exposure to FRs is the maritime environment, particularly the indoor environments of cruise ships. This study presents the first comprehensive assessment of FRs in indoor dust collected from three expedition cruise ships of varying ages and refitting histories. Ten polybrominated diphenyl ethers (PBDEs), 23 alternative halogenated flame retardants (AHFRs), and 16 organophosphate esters (OPEs) were analyzed in dust from 12–16 locations per ship. OPEs, especially tris(1-chloro-2-propyl)phosphate (TCIPP), dominated the chemical profile, with concentrations reaching up to 1786 µg g<small><sup>−1</sup></small>. Concentrations of FRs in different areas on the same ships differed greatly, sometimes by an order of magnitude. Older ships exhibited significantly higher FR levels compared to the newer vessel. Estimated daily intake (EDI) modeling indicated that ship crew members—particularly those working in heavily furnished or electronic-rich areas—may experience elevated exposures through ingestion and dermal contact. Strict performance-based fire test procedures are mandatory for all products onboard ships, but no regulations exist concerning the type of FR used or the concentrations thereof. These findings underscore the need for targeted regulation and further monitoring of chemical exposures in maritime environments, especially given the extended periods that crew members spend onboard.</p><h4><strong>Instrumental analyses</strong></h4><p>Out of 16 OPEs that were analyzed for (Table S1), 15 were detected in the samples at least once: TDCIPP, TCIPP, CDP, EHDPP, oTMPP, ip-TPP, m/p TMPP, TBOEP, TCEP, TEHP, TEP, TiBP, TnBP, TnPP, TPHP. The full list of target OPEs with compound names and identifiers is given in Table S1. OPEs were quantified using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=1290+Infinity"><strong>Agilent 1290 Infinity high-performance liquid chromatograph</strong></a> (HPLC) coupled to an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=6495+"><strong>Agilent 6495 triple quadrupole mass spectromete</strong></a>r operating in positive electrospray ionization mode (ESI+). Chromatographic separation was achieved on an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1952"><strong>ACQUITY BEH C18 column</strong></a> (2.1 mm × 100 mm, 1.7 µm) with a mobile phase gradient of 0.1% formic acid in water and methanol at a flow rate of 0.2 mL min−1. Quantification was performed in multiple reaction monitoring (MRM) mode using isotope dilution with 13C- or deuterium-labeled standards for TPHP, TnBP, TDCIPP, and TnPP.</p><p>Ten PBDE congeners were detected (BDEs-28, 47, 66, 99, 100, 153, 154, 183, and 209) and 16 out of 23 AHFRs (HBB, BEH-TEBP, PBBZ, PBT, PBEB, TBP-DBPE, EH-TBB, DBDPE, TBP-AE, aDBE-DBCH, bDBE-DBCH, gdDBE-DBCH, BTBPE, sDP and aDP) were detected in the samples. The full list of PBDEs and AHFRs is given in Table S1. PBDEs and AHFRs were analyzed using an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890A"><strong>Agilent 7890A gas chromatograph</strong></a> equipped with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=7&amp;search=RTX-1614"><strong>RTX-1614 column</strong></a> (15 m × 0.25 mm, 0.10 µm) and coupled to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=5&amp;search=AutoSpec+Premier"><strong>Waters AutoSpec Premier high-resolution mass spectrometer</strong></a> operated in electron impact ionization (EI+) and selected ion monitoring (SIM) mode with a resolving power greater than 10 000. BDE-209 was analyzed at a reduced resolution of &gt;5000 to improve sensitivity. While PBDEs and AHFRs were measured using the same instrumental setup, distinct GC oven temperature programs and injection conditions were applied for each compound group. Full analytical parameters are provided in the SI (Text S3; Tables S4–S8) and example chromatographs presented in Fig. S3–S7.</p></div>

Revealing hidden chemicals at sea

<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 07, 2026

News from LabRulezLCMS Library - Week 09, 2026

News from LabRulezLCMS Library - Week 10, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 15th June 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, Shimadzu </strong>and<strong> Thermo Fisher Scientific, </strong>technical note by<strong> KNAUER </strong>and brochure by <strong>Waters Corporation!</strong></p><h3><strong>1. Agilent Technologies: Large-Volume Dilute-and-Shoot Analysis of PFAS in Drinking Water Using the Altura PFAS Column</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_analysis_pfas_drinking_water_altura_5994_9186en_agilent_a66334e5b0.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Per‑ and polyfluoroalkyl substances (PFAS) are synthetic fluorinated compounds valued for their oil‑ and water‑repellent properties, but their environmental persistence and mobility have driven the development of increasingly stringent regulations for drinking water monitoring. Existing dilute-and-shoot methods, such as EPA 8327 and ASTM D7979, were originally designed for screening PFAS in nonpotable water. These methods typically rely on 10 to 30&nbsp;µL injection volumes, setting practical quantitation limits appropriately 10 ng/L.<sup>1,2&nbsp;</sup></p><p>We present a large‑volume injection workflow that extends the capabilities of these methods toward trace PFAS quantitation in drinking water. Using the Agilent 6495D triple quadrupole LC/MS (LC/TQ) coupled with a 1290 Infinity II LC, we achieved injections of 200 µL of methanol‑diluted water on the Altura PFAS column without requiring SPE concentration. The Altura PFAS column maintained peak symmetry and retention stability under these injection conditions. This configuration enabled a working calibration range of 0.25 to 25 ng/L, extending the low-end sensitivity substantially relative to published dilute-and shoot methods.<sup>1,2&nbsp;</sup></p><p>This performance enhancement simplifies operations by removing labor‑intensive extraction steps, while maintaining sensitivity required for regulatory guidelines thereby supporting high‑throughput PFAS workflows suitable for routine drinking water analysis. The PFAS compounds analyzed were PFBS, HFPO-DA, PFHpA, PFHxA, PFHxS, PFOA, PFOS, PFNA, and PFDA. These compounds were selected due to their relevance to ongoing regulatory actions and proposed maximum contaminant level (MCL) considerations for drinking water.&nbsp;</p><p>Specific highlights of this experiment include:&nbsp;</p><ul><li>Minimized peak tailing and solvent effects with 200 µL injections water/methanol (1:1) injections.</li><li>Increased throughput by elimination of solid phase extraction (SPE).&nbsp;</li><li>Enhanced sensitivity of 6495D LC/TQ at low end (0.25&nbsp;ng/L) for the dilute-and-shoot method in drinking&nbsp;water.</li></ul><h4><strong>Experimental&nbsp;</strong></h4><h5><strong>Instrumentation&nbsp;</strong></h5><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=+1290+Infinity+II"><strong>Agilent 1290 Infinity II LC</strong></a> coupled to <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6495D"><strong>Agilent 6495D LC/TQ system</strong></a> was utilized for the LC/MS/MS analysis. An Infinity&nbsp;II multisampler with an extended multidraw capillary tube (G7137-68307) was connected to the needle seat and injection valve with a union for large volume injection (200&nbsp;µL). The data were acquired with MassHunter acquisition software version 12.2. All LC/MS parameters are shown in Table 1 and 2. PFAS multiple reaction monitoring (MRM) transition methods were imported from the PFAS MRM database (G1736AA) while labelled homologues were optimized to obtain correct MRM transitions (Table 3).</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This study demonstrates a practical large‑volume dilute-and-shoot workflow for the determination of PFAS in drinking water using the Agilent 1290 Infinity II LC coupled to the 6495D triple quadrupole LC/MS, and Agilent Altura Poroshell PFAS column. With 200 µL water samples diluted in methanol can be injected directly, eliminating the need for SPE concentration and significantly reducing sample preparation time. This method exhibits good sensitivity, accuracy, and reproducibility. The Altura PFAS column maintained consistent peak performance and retention stability even at low sub‑ppt concentrations, supporting long‑term reliability for trace‑level PFAS monitoring. Overall, the findings highlight the method potential to support routine, high‑sensitivity PFAS monitoring in drinking water laboratories.</p><h3><strong>2. KNAUER: Size matters - How to perform narrow calibration using the ClarityChrom® GPC Extension</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/VTN_0049_knauer_size_matters_how_to_perform_narrow_calibration_using_the_claritychrom_gpc_extension_3cfdc7a45b.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Gel Permeation Chromatography (GPC), also known as Size Exclusion Chromatography (SEC), is a separation technique that separates molecules based on their hydrodynamic size rather than chemical interactions. In a GPC column, separation is based on the ability of molecules to access the pores of the stationary phase. Smaller molecules can penetrate these pores and therefore spend more time inside the column, resulting in a delayed elution. Larger molecules, on the other hand, cannot enter the pores and pass through the column more quickly, leading to earlier elution.&nbsp;</p><p>As a result, molecules are separated by size in solution, providing the basis for the determination of molecular weight and molecular weight distributions. Calibration is therefore a fundamental requirement for ensuring the accuracy and reliability of the results. The ClarityChrom® GPC Extension enables users to efficiently create and apply different calibration models for precise analysis. The workflow presented here focuses on narrow calibration using standards with defined molecular weights and low polydispersity (PD ≈ 1).</p><h4><strong>Material and Methods</strong></h4><ul><li><strong>Software&nbsp;</strong><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=503&amp;search=ClarityChrom"><strong>ClarityChrom</strong></a>® 10.1 - station single instrument license one time base</li><li>ClarityChrom® 10.1 - GPC license for GPC data processing &nbsp;</li></ul></li><li><strong>Pump: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2372"><strong>AZURA P 6.1L isocratic HPLC pump</strong></a> with 10 ml pump head for normal phase applications, stainless steel&nbsp;</li><li><strong>Degasser: </strong>Analytical 2 channel GPC degasser&nbsp;</li><li><strong>Autosampler:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2375"><strong>AZURA® AS 6.1L</strong></a>, analytical HPLC autosampler, 862 bar&nbsp;</li><li><strong>Detector:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2429"><strong>AZURA® RID 2.1L</strong></a>, analytical refractive index detector&nbsp;</li><li><strong>Thermostat: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2376"><strong>AZURA® CT 2.1</strong></a> ATC00 Capillaries Start-Up Kit with flexible, precut capillaries for analytical HPLC systems with 1/16" connections</li></ul><h4><strong>Conclusion</strong></h4><p>This technical note demonstrates how to successfully create and apply a narrow calibration using the ClarityChrom® GPC Extension. By following the outlined workflow, users can ensure reliable calibration and determination of molecular weight and molecular weight distributions. The described approach supports consistent and reproducible results, making it a valuable tool for routine GPC/SEC analysis. For further optimization and advanced applications, additional related technical and application notes can be consulted.</p><h3><strong>3. Shimadzu: UHPLC Method for Sensitive Automatic Analysis of Thirty-Seven D/L-Amino Acids and for Liquor Profiling</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_01169_en_2dab331398.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>Enables high-sensitivity simultaneous fast analysis of thirty-seven D/L-amino acids using simple operations.</li><li>Good reproducibility of analytical results can be achieved by keeping the derivatization reaction time constant.</li><li>Statistical analysis software enables easy multivariate analysis of multiple samples.</li></ul><p>Recent advances in analytical techniques have revealed the presence of D-amino acids in fermented foods and biological samples and clarified their role in the taste, preservation, and aroma of foods , and as potential disease biomarkers. Therefore, the demand for D/L separation of amino acids is increasing. Because D-amino acids are only present in trace amounts in fermented foods and biological systems, unlike L-amino acids, it is necessary to determine the concentration of each D-amino acid by separating them from the high concentrations of Lamino acids.&nbsp;</p><p>A comprehensive method for quantitating the thirty-seven D/Lamino acids was previously reported1), in which two chiral derivatizing reagents were employed to provide different diastereomers for each amino acid, with the instrument automatically switching between two separation methods to analyze each sample twice.&nbsp;</p><p>This article introduces an improved method that employs a single chiral derivatizing reagent to enable simultaneous analysis of D/L-amino acidsin a shorter time.</p><h4><strong>D/L-Amino Acid Analysis by UHPLC&nbsp;</strong></h4><p>In general, LC/MS or multi-dimensional LC is used to analyze D/L-amino acids by HPLC, because it is difficult to separate proteinogenic D/L-amino acids with a single separation mode. However, it is known that LC/MS is susceptible to matrix effects and less quantitative than HPLC. It is also known that the multidimensional LC method requires a long analysis time and very complicated HPLC setup. Therefore, a simple operational method that provides good separation for D/L-amino acids in a short time is needed.&nbsp;</p><p>For food analysis, a small particle column is used to achieve appropriate separation of the small amounts of D-amino acids from the large amounts of L-amino acids and co-existing contaminants. A <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=X3"><strong>UHPLC system (Nexera X3</strong></a>) was employed in this study due to the increased system pressure caused by the use of a small particle column.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>A method was developed for simultaneous separation of OPA/NIBC diastereomers for thirty-seven D/L-amino acids using a simple UHPLC system in approximately half the time of the conventional methods. By optimizing the derivatization reaction, all compounds were determined sensitively, accurately, and precisely. Separation of the target compounds from the contaminants was good in the liquor samples when evaluated using real liquor samples. It is expected to be easily applicable to D/L-amino acid profiling in food and beverage samples without using expensive MS detection or complicated multidimensional HPLC configurations as long as samples are prepared properly. Moreover, D/L-amino acid profiling could be used to research and develop foods containing D-amino acids intended to help to maintain and improve the intestinal environment, and could help in the early detection of diseases and determining optimal treatment strategies through biomarker discovery</p><h3><strong>4. Thermo Fisher Scientific: Screening of per- and polyfluoroalkyl substances (PFAS) in cosmetics: Utilizing a new combustion-ion chromatography system for total organic fluorine (TOF) analysis</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ap_004098_ic_systems_combustion_ic_environmental_ap004098_na_en_a3a1d33a24.pdf"><strong>Full PDF for download</strong></a></li></ul><p>This application note describes a method for <strong>screening per- and polyfluoroalkyl substances (PFAS) in textiles</strong> using total organic fluorine (TOF) analysis by combustion-ion chromatography (C-IC). PFAS are widely used in textiles to provide water, oil, and stain resistance, but increasing concerns about their environmental persistence and potential health effects have led to stricter regulations worldwide. California’s AB 1817 legislation, for example, limits TOF concentrations in textiles to 100 ppm beginning in 2025 and 50 ppm by 2027, creating a need for reliable analytical methods capable of assessing PFAS content in textile products.</p><p>The study evaluates a new <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2150"><strong>Thermo Scientific Cindion Combustion Ion Chromatography System</strong></a>, which combines a Dionex Inuvion IC system with a Cindion combustion/absorption module. The system features an optimized Z-fold combustion tube design that improves combustion efficiency, shortens analysis time, reduces instrument footprint, and allows complete control through Chromeleon software. Unlike surface-sensitive techniques such as PIGE, the combustion-IC approach analyzes the entire sample, providing results that are independent of sample thickness. The method measures total fluorine (TF) after combustion and total inorganic fluorine (TIF) by direct IC analysis, with TOF calculated as the difference between TF and TIF.</p><p>To validate the approach, six textile samples representing waterproof and stain-resistant consumer products were analyzed and compared with results previously obtained using a Nittoseiko combustion-IC system. TOF concentrations ranged from approximately 1 ppm in one nylon fabric to nearly 375 ppm in a polyester baby bib. The values generated by the new Cindion system showed excellent agreement with the reference system, achieving between 100% and 105% of the previously reported results. Reproducibility was also strong, with relative standard deviations below 8% for all samples.</p><p>The authors conclude that the new Cindion C-IC platform provides an accurate, reliable, and efficient solution for PFAS screening in textiles. In addition to matching the performance of the established combustion-IC method, the enhanced system offers a flexible “2-in-1” configuration that allows seamless switching between combustion-IC and standalone IC operation. This improves workflow efficiency, reduces manual intervention, and provides manufacturers and testing laboratories with a practical tool for monitoring compliance with evolving PFAS regulations in textile products.</p><h3><strong>5. Waters Corporation: Advanced Acquisition Modes for the </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2433"><strong>Xevo MRT P10 Mass Spectrometer</strong></a></h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009362_9baa39e7de.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><p>The Waters solution sheet introduces the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2433"><strong>Xevo MRT P10 Mass Spectrometer</strong>,</a> a next-generation high-resolution mass spectrometer designed to provide significantly greater analytical depth, sensitivity, and flexibility for modern omics workflows. Compared with the previous Xevo MRT platform, the instrument delivers a reported <strong>20-fold increase in MS/MS sensitivity</strong>, incorporates Wideband Enhanced Duty Cycle (WB EDC) technology, and supports ultrafast acquisition rates of up to <strong>100 Hz for MS data</strong> and <strong>200 Hz for MS/MS data</strong>. These performance improvements are intended to enhance the detection of low-abundance compounds while maintaining high-quality spectral information across complex biological samples.</p><p>A major focus of the document is the introduction of the new <strong>SONAR Pulse Acquisition Mode</strong>, an advanced data-independent acquisition (DIA) approach. SONAR Pulse improves selectivity by rapidly stepping a quadrupole isolation window across a defined precursor mass range, allowing fragment ions to be associated with narrower precursor windows than in conventional DIA experiments. This strategy reduces spectral complexity, improves confidence in compound identification, and increases the likelihood of detecting low-level analytes that might be missed by traditional data-dependent acquisition (DDA) methods. The method supports precursor and product ion scans up to m/z 2000, multiple quadrupole isolation window sizes, acquisition speeds up to 200 Hz, and full compatibility with WB EDC technology.</p><p>The second major innovation described is <strong>Mixed Mode Acquisition</strong>, a hybrid workflow that combines targeted and untargeted analysis within a single injection. In this approach, high-sensitivity <strong>Tof MRM</strong> quantification is performed simultaneously with untargeted DIA (MSE) acquisition. This enables users to obtain quantitative data for predefined targets while also collecting comprehensive full-scan information for discovery and screening purposes. The workflow integrates seamlessly with Waters software tools, allowing targeted quantification through the MS Quan application and untargeted analysis through UNIFI or export to open data formats such as mzML for processing in third-party software packages including MZmine, MS-DIAL, DIA-NN, PEAKS, and Progenesis QI.</p><p>According to Waters, both acquisition strategies are designed to maximize information obtained from each sample injection. SONAR Pulse emphasizes deeper molecular coverage, improved selectivity, and simplified interpretation of complex DIA datasets, while Mixed Mode provides a unified quantitative–qualitative workflow that combines targeted measurement and discovery screening without compromising sensitivity or acquisition speed. Together, these capabilities position the Xevo MRT P10 as a versatile platform for metabolomics, lipidomics, proteomics, and other multiomics applications where both comprehensive characterization and accurate quantification are required.</p></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS Library - Week 25, 2026

News from LabRulezLCMS Library - Week 26, 2026

<p><strong>This study evaluates an immobilized enzyme reactor (IMER) containing peptide N-glycosidase from </strong><i><strong>Rudaea cellulosilytica</strong></i><strong> (PNGase Rc) for rapid online deglycosylation of intact glycoproteins. Human glycoproteins and therapeutic antibodies were used as model substrates to assess reactor performance.</strong></p><p>The PNGase Rc IMER efficiently removed complex sialylated and core-fucosylated glycans, simplifying protein characterization and glycosylation-site analysis. The approach offers a fast and effective solution for bioanalytical workflows, biopharmaceutical quality control, and stability testing of therapeutic proteins.</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.6c00577"><strong>Online Deglycosylation of Monomeric Intact Proteins Using the PNGase Rc Immobilized-Enzyme Reactor</strong></a></h4><p>Katarína Molnárová, Petr Novák, Jana Nováková, and Petr Pompach*</p><p>ACS Omega 2026, 11, 17, 25724–25729</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsomega.6c00577">https://doi.org/10.1021/acsomega.6c00577</a></p><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/"><strong>CC-BY 4.0</strong></a></h6></blockquote><p><strong>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.</strong></p><div><p>Protein glycosylation, in which monosaccharide units are attached to a protein backbone through enzymatic pathways, is involved in many important biochemical processes and is considered one of the most important post-translational modifications. <a href="javascript:void(0);">(1)</a> It affects not only the stability and secretion of proteins, cell–cell interactions, and receptor–ligand recognition mechanisms but also the biological activity, plasma half-life, immunogenicity, pharmacodynamics, and pharmacokinetics of biotherapeutics. <a href="javascript:void(0);">(2−5)</a> Therapeutical monoclonal antibodies (mAbs) are among the best known pharmaceuticals that are based on glycoproteins. <a href="javascript:void(0);">(6)</a> Over 90% of the mAbs are derived from immunoglobulin G (IgG), in which <i>N</i>-glycosylation occurs at Asn297 of the Fc region and is responsible for modulating immune responses and interactions with other proteins. <a href="javascript:void(0);">(7,8)</a> In cancer treatment, mAbs are used to increase the response of the immune system against the tumor cell, thus inhibiting the cancerous cell growth and helping with the destruction and elimination. <a href="javascript:void(0);">(9)</a> Among the most commonly used mAbs are trastuzumab, bevacizumab, cetuximab, or margetuximab, which are used as an additional treatment for breast, colorectal, prostate, or lung cancer. <a href="javascript:void(0);">(10)</a></p><p>Mass spectrometry (MS)-based methods have become a method of choice in the analysis of mAbs that can provide information on sequence, post-translational modifications, and glycosylation profiles. <a href="javascript:void(0);">(11)</a> The enzymatic removal of the attached glycans from the protein backbone can reduce the complexity of the MS analysis, which can lead to a better understanding of the protein structure and modifications. In glycoproteomics, peptide-<i>N</i>-glycosidase F (PNGase F) is most used for glycan removal. It cleaves the linkage between the Asn residue and the <i>N</i>-acetylglucosamine (GlcNAc). <a href="javascript:void(0);">(12)</a> Jmeian et al. developed a monolithic PNGase F enzyme reactor fabricated in fused silica using a glycidyl methacrylate-<i>co</i>-ethylene dimethacrylate polymer and integrated it into an LC–MS workflow. The authors demonstrated the applicability of this system for the characterization of released neutral and acidic <i>N</i>-glycans by LC–MS analysis. <a href="javascript:void(0);">(13)</a> In another study, oriented immobilization of PNGase F onto a methacrylate-based monolithic support via glutathione-<i>S</i>-transferase–glutathione affinity coupling was employed to release <i>N</i>-glycans from denatured ribonuclease B and fetuin, as well as from native IgG. The released glycans and the corresponding deglycosylated proteins were subsequently analyzed by MALDI-MS. <a href="javascript:void(0);">(14)</a></p><p>Gramlich et al. showed the potential of PNGase Rc for <i>N</i>-glycan hydrolysis from both tryptic peptides and native glycoproteins at a low pH. The favorable properties of PNGase Rc, including activity at acidic pH and compatibility with reducing agents such as <i>tris</i>(2-carboxyethyl)phosphine hydrochloride (TCEP) and denaturants like urea, make this enzyme well suited for online intact protein deglycosylation workflows. <a href="javascript:void(0);">(15,16)</a></p><p>In this report, we demonstrate the potential of the PNGase Rc IMER for rapid online deglycosylation of reduced monomeric glycoproteins, including human haptoglobin (Hp), human transferrin, <i>anti</i>-hHD6, and the therapeutic monoclonal antibodies trastuzumab and bevacizumab. The column retained its activity over more than 150 consecutive measurements, highlighting its robustness, suitability for repeated use in bioanalytical workflows, and applicability to pharmaceutical research and development.</p><h4><strong>Experimental Section</strong></h4><h5><strong>Instrumentation and Experimental Conditions</strong></h5><p>Automated sample handling and online deglycosylation were carried out using the HDX workstation (AffiPro, Czech Republic). The scheme of the system is shown on <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.6c00577#fig1">Figure 1</a>. Samples of 50 mM ammonium bicarbonate buffer (pH 8.2) and 40 mM TCEP were placed in a sample tray at 4 °C. Ten microliters of the protein sample at a concentration of 0.03 mg/mL (0.3 μg per injection) were added to 40 μL of 50 mM ammonium bicarbonate and then transferred to 50 μL of 40 mM TCEP, pH 2.3. The disulfide bond reduction was carried at 40 °C for 5 min. The automated sample handling system injected 100 μL of the reaction mixture into the sample loop and switched the injection valve. Online deglycosylation was performed at room temperature using a PNGase Rc IMER (2.1 × 20 mm, AffiPro, Czech Republic) at a flow rate of 50 μL/min, followed by protein desalting on an OPTI-TRAP (0.5 × 2 mm) trap column (Optimize Technologies Inc., Oregon City, Oregon, USA) heated to 55 °C for 10 min with 0.2% formic acid delivered by an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1260+Infinity+III+isocratic+pump"><strong>Agilent 1260 Infinity III isocratic pump</strong></a><strong> </strong>(Agilent Technologies, Santa Clara, California, USA). By switching the trap valve, the protein was eluted by an acetonitrile gradient [(min)/% B] 0/10-9/10-16/70-16.5/90-17/90-18/10-23/10] delivered by the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+Infinity+II+LC"><strong>Agilent 1290 Infinity II HPLC</strong></a> system (Agilent Technologies, Santa Clara, California, USA) at a flow rate of 20 μL/min. The mobile phase A consisted of 5% acetonitrile with 1% propan-2-ol and 0.1% formic acid, and the mobile phase B consisted of 95% acetonitrile with 1% propan-2-ol and 0.1% formic acid. The <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=8&amp;search=maXis+Q-TOF"><strong>maXis Q-TOF mass spectrometer</strong></a> (Bruker Daltonics, Bremen, Germany) was operated in the survey MS mode in a mass range of <i>m</i>/z 50–3000. The acquired data were analyzed and processed by <strong>DataAnalysis 4.4</strong> (Bruker Daltonics) and deconvoluted by UniDec <a href="javascript:void(0);">(17)</a> with the following parameters: data processing range, <i>m</i>/z 500–3000; charge range, 1–80; allowed mass range, 1,000–80,000; sampling rate, 10 Da; peak detection range, 500 Da; and peak detection threshold, 0.1.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2026_11_17_25724_25729_Figure_1_Schematic_of_the_automated_sample_handling_system_for_online_protein_deglycosylation_and_desalting_d4ee48b627.jpg" alt="ACS Omega 2026, 11, 17, 25724–25729: Figure 1. Schematic of the automated sample handling system for online protein deglycosylation and desalting. Protein samples, along with 50 mM ammonium bicarbonate and 40 mM TCEP stock solutions were placed in a sample tray chilled to 4 °C, while a second tray heated to 40 °C was used for disulfide bond reduction with TCEP buffer." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2026_11_17_25724_25729_Figure_1_Schematic_of_the_automated_sample_handling_system_for_online_protein_deglycosylation_and_desalting_d4ee48b627.jpg 245w," sizes="100vw" width="1287" height="386"></p><h4><strong>Results and Discussion</strong></h4><p>The performance of the PNGase Rc IMER for the removal of complex <i>N</i>-glycans from intact proteins was tested using heavily glycosylated human Hp with four glycosylation sites (Asn184, Asn207, Asn211, and Asn241) <a href="javascript:void(0);">(18)</a> located at the β-chain and occupied by complex <i>N</i>-glycans terminated with sialic acid. Haptoglobin phenotype 2-1, used in this study, forms multimers consisting of β-chain and disulfide linked α1 and α2 chains. <a href="javascript:void(0);">(19)</a> The detection of glycosylated Hp β-chain requires reduction of the disulfide bonds by incubating the protein with a reducing reagent. TCEP is a common reducing reagent used for fast reduction of disulfide bonds at various pH levels. Forty degrees Celsius, the maximum temperature of the PAL tray, and 5 min of incubation were sufficient for complete reduction of Hp disulfide bonds. Individual signals corresponding to the glycosylated β-chain were observed in the <i>m</i>/<i>z</i> range of 35,800–37,400 (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.6c00577#fig2">Figure 2</a>a). The limited resolution of the mass spectrometer did not allow assigning the different glycoforms of the haptoglobin β-chain, which is occupied by biantennary, triantennary, or tetraantennary glycans with various amounts of sialic acid and fucose. <a href="javascript:void(0);">(20,21)</a> The nonglycosylated α1 and α2 chains were observed at <i>m</i>/<i>z</i> 9190 and 15,940. When the PNGase Rc IMER was integrated into the flow system, a signal at <i>m</i>/<i>z</i> 27,270 was detected, demonstrating complete deglycosylation of the haptoglobin β-chain (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.6c00577#fig2">Figure 2</a>b).</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2026_11_17_25724_25729_Figure_2_A_Mass_spectrum_of_human_Hp_without_the_PN_Gase_Rc_IMER_implemented_in_the_system_0ecca84ed4.jpg" alt="ACS Omega 2026, 11, 17, 25724–25729: Figure 2. (A) Mass spectrum of human Hp without the PNGase Rc IMER implemented in the system. The base peak signals of the spectrum correspond to both α1 and α2 chains. The signal of the β chain is spread across its different glycoforms. (B) Mass spectrum of human Hp with the PNGase Rc IMER implemented in the system. The signal of the deglycosylated β chain is higher compared to its glycosylated form and observed only at m/z 27,270. This indicates complete removal of glycans from the Hp β chain." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2026_11_17_25724_25729_Figure_2_A_Mass_spectrum_of_human_Hp_without_the_PN_Gase_Rc_IMER_implemented_in_the_system_0ecca84ed4.jpg 245w," sizes="100vw" width="2015" height="913"></p><p>In a previous study by Krenkova et al., the PNGase F IMER was used for deglycosylation of IgG, RNase B, and bovine fetuin with follow-up mass spectrometry detection of both released glycans and intact proteins using MALDI-TOF MS. <a href="javascript:void(0);">(14)</a> The authors demonstrated an effective method for rapid protein deglycosylation, which, however, requires additional sample handling prior to mass spectrometry measurement. The other study by Jmeian et al., which focused on released <i>N</i>-glycans, implemented a PNGase F IMER with online LC–MS detection. <a href="javascript:void(0);">(13)</a> The authors show the effectiveness of the method by identifying many different glycans released from a single protein or from a complex plasma mixture. Our approach is not directly intended for released <i>N</i>-glycan analysis; instead, it demonstrates the ability to measure intact proteins after rapid online deglycosylation using PNGase Rc at low pH. Samples prepared immediately prior to mass spectrometry analysis using the automated sample-handling platform can reduce variability associated with autosampler residence time, as some proteins may undergo degradation or precipitation during storage in the autosampler.</p><p>Although all glycoproteins in this study were effectively deglycosylated, the method’s efficiency depends on the characteristics of the individual glycoprotein. Therefore, optimizing method parameters─including the isocratic flow rate, glycoprotein incubation time with TCEP, and/or the addition of denaturing reagent─may improve the overall efficiency of the deglycosylation process.</p><p>The PNGase Rc IMER stability over a series of injections was tested by using the trastuzumab antibody. The measurements were carried out with the enzyme column kept at the laboratory temperature. As shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.6c00577#fig5">Figure 5</a>, the results indicate that the column performance remained stable over the course of the 150 measurements, and no glycosylated form of the trastuzumab antibody heavy chain was detected. The activity of PNGase Rc in the presence of 5% acetonitrile and 5% propan-2-ol was evaluated using a bottom-up approach with human 2–1 haptoglobin, which was online-digested by a coimmobilized nepenthesin-2/pepsin IMER. In the absence of an organic solvent, the peptide IEKVVLHPNYSQVD remained fully deglycosylated throughout 30 injections. In contrast, in the presence of organic solvent, a marked loss of enzymatic activity was observed after only a few injections (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsomega.6c00577/suppl_file/ao6c00577_si_001.pdf">Figure 2</a>).</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2026_11_17_25724_25729_Figure_5_Monitoring_the_stability_and_performance_of_PN_Gase_Rc_IMER_4a9b5a9c53.jpg" alt="ACS Omega 2026, 11, 17, 25724–25729: Figure 5. Monitoring the stability and performance of PNGase Rc IMER. Trastuzumab heavy chain was completely deglycosylated after 150 injections." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2026_11_17_25724_25729_Figure_5_Monitoring_the_stability_and_performance_of_PN_Gase_Rc_IMER_4a9b5a9c53.jpg 170w," sizes="100vw" width="996" height="918"></p><h4><strong>Conclusions</strong></h4><p>Here, we demonstrate the potential of the PNGase Rc IMER for the online removal of <i>N</i>-glycans from intact monomeric glycoproteins reduced with TCEP. The column showed high sensitivity toward Hp, which has multiple glycosylation sites with various glycan structures, confirming its suitability for the profiling of complex glycoproteins. Bevacizumab and trastuzumab exhibited similar glycosylation profiles, with core-fucosylated biantennary glycans being the most abundant. Online deglycosylation with the PNGase Rc column resulted in a complete removal of the glycans from the heavy chains of both antibodies, proving that the column can be used for the rapid online deglycosylation of intact therapeutic mAbs. Moreover, the column remained stable over 150 measurements without any loss of activity, even when it was maintained at laboratory temperature. The significantly reduced reaction time, together with full automation and the absence of manual handling steps, substantially improves analytical throughput compared to conventional off-line deglycosylation workflows. These findings highlight the potential of the PNGase Rc IMER in the development of glycoprotein-based biopharmaceuticals, where detailed structural characterization of the protein part is critical for quality control, monitoring batch-to-batch variability, and stability testing.</p></div>

Online Deglycosylation of Monomeric Intact Proteins Using the PNGase Rc Immobilized-Enzyme Reactor

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 20th 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>Bruker / ASMS</strong>, presentation by <strong>MDCW / University of North Dakota </strong>and application note by <strong>Shimadzu!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Extractables Analysis of Food Contact Materials Using High-Resolution GC/MS and LC/MS</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_fcm_extractables_lc_q_tof_wp_311_asms_2026_en_agilent_f5d83c8730.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>Chemicals residing in food contact materials (FCM) can migrate from packaging and containers into food. The FCM include a variety of materials including paper and plastic among others. The substances that migrate from FCM include volatile, semi-volatile and non-volatile compounds and therefore a combination of GC/MS and LC/MS techniques is needed for comprehensive analysis of potential migrants. In this study we evaluated different types of FCM including food vacuum sealer bags, heavy duty plastic food containers as well as lined paperboard containers. Various solvents were assessed for their ability to extract different classes of food packaging-derived chemicals. For increased confidence in compound annotation, high-resolution GC and LC MS platforms were used in this study in combination with application-specific accurate mass libraries.</p><h4><strong>Experimental</strong></h4><h5><strong>GC/Q-TOF&nbsp;</strong></h5><ul><li><strong>MS:</strong> <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?from=1990&amp;mainauthorItems=10&amp;search=7250&amp;to=2026"><strong>Agilent 7250 GC/Q-TOF</strong></a></li><li><strong>GC: </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?from=1990&amp;mainauthorItems=10&amp;to=2026&amp;search=8890"><strong>Agilent 8890 GC</strong></a></li><li><strong>Column: </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?from=1990&amp;mainauthorItems=10&amp;to=2026&amp;search=DB-5Q"><strong>Agilent DB-5Q</strong></a>, 30 m, 0.25 mm, 0.25 µm</li></ul><h5><strong>LC/Q-TOF</strong></h5><ul><li><strong>LC: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+Infinity+II"><strong>Agilent 1290 Infinity II</strong></a></li><li><strong>MS: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Revident"><strong>Agilent Revident LC/Q-TOF</strong></a></li><li><strong>Analytical column:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Poroshell+Aq-C18"><strong>Agilent Poroshell Aq-C18</strong></a> 2.1 x 150 mm, 2.7µm column</li></ul><h4><strong>Conclusions</strong></h4><p>FCM extractions were optimized and successfully analyzed using a variety techniques based on highresolution GC/MS and LC/MS. Combination of different high resolution MS techniques helped to ensure a comprehensive E&amp;L compound coverage. E&amp;L focused accurate mass libraries were key to efficient data analysis.</p><h3><strong>2. Bruker / ASMS: Novel data processing workflow including in-silico derivatization for integrated CI &amp; EI MS data acquired with the GC-ecTOF instrument</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/asms_2026_thp_429_in_silico_derivatization_for_integrated_ci_ei_ectof_fb022d26ba.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>Combined suspect and non-target GC-MS analysis of volatile and semi-volatile compounds holds relevance for environmental monitoring &amp; research, food, flavor &amp; fragrance analysis as well as metabolomics studies. The combination of Chemical Ionization (CI) and Electron Ionization (EI) in the ecTOF instrument (Bruker Daltonics, Bremen, Germany) can improve the identification confidence of unknown compounds, especially in complex samples and when no standards are available. The simultaneous usage of two complementary ionization techniques brings additional advantages for quantification workflows. To leverage these benefits, a novel data processing approach has been developed, and applicability is shown in two study designs.</p><h4><strong>Methods</strong></h4><p>Derivatized samples from two studies were analyzed using the GC-ecTOF instrument. Data were converted to TSF format and processed with prototype versions of MetaboScape and TASQ. Untargeted feature detection was performed on the CI data stream, including de-isotoping, de-adducting for CI-specific ions [M-H]⁺, [M]⁺, [M+H]⁺, [M+NH₄]⁺, [M-CH3 ] + and retention time alignment across all samples.</p><h4><strong>Conclusion</strong></h4><ul><li>Untargeted feature finding and streamlined annotation of ecTOF supported by in-silico derivatization and in-silico fragmentation extends GC-MS analysis for metabolomics and non-target screening.&nbsp;</li><li>In-silico derivatization permits complementary annotation for compounds lacking reference standards.&nbsp;</li><li>Simplified process from identified markers in profiling experiments to target screening and quantitation methods.</li></ul><h3><strong>3. MDCW / University of North Dakota: Identifying the transition from ante-mortem to post-mortem odor in cadavers cadavers in an outdoor environment</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/O_23_Patel_2a1bb7a2fa.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>This presentation investigates how the characteristic odor of a human body changes during the transition from life (ante-mortem) to decomposition (post-mortem). The researchers focused on identifying volatile organic compounds (VOCs) released during the early post-mortem period and determining when the scent profile changes from that of a living person to that associated with human remains. Understanding this transition is particularly important for improving search and rescue operations, where distinguishing between living victims and deceased individuals is essential for deploying search-and-rescue dogs and human remains detection dogs effectively.</p><p>To study this process, VOC samples were collected from body donors at both a morgue and an outdoor decomposition research facility (REST). Air samples were collected using sorbent tubes and ACTI-VOC pumps after controlled VOC accumulation and sampling periods. Chemical analysis was performed using <strong>thermal desorption comprehensive two-dimensional gas chromatography coupled with mass spectrometry (TD-GC×GC-MS)</strong>. The analytical system employed a Restek <strong>Rxi®-624Sil MS</strong> first-dimension column and a <strong>Stabilwax®</strong> second-dimension column, with electron ionization (70 eV) mass spectrometry covering a mass range of <strong>29–300 amu</strong> at an acquisition rate of <strong>250 spectra/s</strong>. Data processing combined <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/41"><strong>ChromaTOF</strong></a> software with <strong>RStudio</strong> for feature alignment, normalization, filtering, and manual verification of VOC profiles.</p><p>The study identified <strong>827 volatile organic compounds</strong>, representing a wide range of chemical classes including nitrogen-containing compounds, esters, halogenated compounds, aromatics, alcohols, ketones, aldehydes, sulfur-containing compounds, ethers, and acids. By comparing experimentally detected VOCs with compounds previously reported in the literature for both living humans and decomposing remains, the researchers identified <strong>33 trans-mortem VOCs</strong> that characterize the transition between ante-mortem and post-mortem odor. VOC profiles were then monitored throughout decomposition for individual donors, allowing the team to visualize how the relative contributions of ante-mortem, trans-mortem, and post-mortem compounds evolved over time.</p><p>The results showed that ante-mortem and trans-mortem VOCs remained detectable during the earliest stages after death, while post-mortem odor compounds became increasingly dominant after approximately <strong>Accumulated Degree Days (ADD) 73.4</strong>, corresponding to <strong>Experimental Day 3</strong>. The authors conclude that although these findings improve our understanding of early decomposition odor chemistry, additional studies across different environments and seasonal conditions are needed to standardize VOC-based approaches and further support forensic investigations and search-and-rescue applications.</p><h3><strong>4. Shimadzu: Gas Analysis for CO2 Conversion Using a GI-30 Auto Gas Injector</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00964_en_2482908145.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The catalytic conversion of carbon dioxide (CO2) to methanol (MeOH) and to hydrocarbons has garnered significant attention as a strategy to realize a sustainable chemical industry. Analytical targets in CO2 conversion studies typically include carbon monoxide (CO), hydrocarbons, alcohols, and other reaction products. Selection of appropriate column and detector combinations must therefore be guided by the nature and concentrations of target analytes.</p><p>In this application news, we demonstrate simultaneous analysis on two parallel columns by using INJ2-way branch unit to permit detection of CO and hydrocarbons together with alcohols such as MeOH. We also present a simplified measurement approach employing a single-column configuration equipped with a thermal conductivity detector(TCD).</p><h4><strong>System Configuration and Analysis Conditions</strong></h4><p>Two reaction schemes using CO2 as feedstock were envisaged: (1) MeOH synthesis and (2) conversion to hydrocarbons. The instrumentation comprised the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?from=1990&amp;mainauthorItems=1&amp;to=2026&amp;search=GI-30"><strong>Auto Gas Injector GI-30</strong></a> and the SPI inlet, which minimizes air ingress and sample adsorption (Fig. 1).&nbsp;</p><p>For the MeOH synthesis application, a Jetanizer -FID—which permits detection of CO and CO2 that are not observable by a conventional FID—was employed. A MICROPACKED-ST packed column provides separation of CO from O2 (ambient contamination); however, higher-boiling hydrocarbons and alcohols such as MeOH are not eluted from this column. To achieve comprehensive analysis, the injector was splitted and an SH-Q-BOND capillary column was used to resolve hydrocarbons and MeOH concurrently. The injection-port splitting is implemented using dedicated hardware (Application News No. 01-00661-EN).&nbsp;</p><p>For the conversion to hydrocarbons scenario, when analytes are permanent gases and C3-or-smaller hydrocarbons, quantitative analysis can be performed with a single MICROPACKED-ST column coupled to a TCD. The TCD responds to differences in thermal conductivity between carrier and analyte gases; measuring low–thermal-conductivity species such as hydrocarbons requires a carrier gas with high thermal conductivity (helium or hydrogen) (Table 1). The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?from=1990&amp;mainauthorItems=1&amp;search=gc-2050&amp;to=2026"><strong>Brevis</strong> <strong>GC-2050</strong></a><strong> TCD</strong> uses a single filament design, resulting in rapid baseline stabilization (~10 minutes), which is advantageous for routine operation.</p><h4><strong>Conclusion</strong></h4><p>Using INJ2-way branch unit enables simultaneous analyses using distinct column-detector combinations within a single chromatographic cycle, permitting comprehensive quantification of reaction products from CO2 conversion— ranging from CO and hydrocarbons to alcohols such as MeOH. For analyses restricted to hydrocarbons up to C3, a streamlined single-column TCD configuration provides sufficient separation and sensitivity. It should be noted that MeOH and hydrocarbons of carbon number ≥ C4 may adsorb or be retained on the MICROPACKED-ST column; periodic column conditioning is therefore recommended.</p></div></div></div></div></div></div></section></div></div></div></div></div></div></section></div></div></div></div></div></div></section>

News from LabRulezGCMS Library - Week 30, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 27th July 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, Shimadzu / ASMS, Thermo Fisher Scientific / ASMS </strong>and<strong> Waters Corporation / ASMS </strong>and application note by<strong> KNAUER!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Down in the Weeds: Automated Fast Screening Workflow for Cannabinoids in Whole Blood Using High Resolution Mass Spectrometry</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_blood_cannabinoids_lc_q_tof_mp_694_asms_2026_en_agilent_02f13ac14e.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Distinguishing psychoactive tetrahydrocannabinol (THC) isomers and their metabolites from nonpsychoactive isobars and novel semi-synthetic cannabinoids like hexahydrocannabinol (HHC) is increasingly important to forensic toxicologists, as is the ability to remain up to date with novel compounds that are introduced into the population. This study describes an automated two-step chromatographic workflow that utilizes an initial fast screen method followed by reinjection with specific chromatography to resolve isobars if a suspect is detected in the fast screen on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Revident"><strong>Revident LC/Q-TOF</strong></a><strong> </strong>with<strong> </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+infinity+II+lc"><strong>1290 Infinity II LC</strong></a> (Figure 1). This allows for a larger number of samples to be screened more quickly while ensuring chromatographic resolution of isomers for confirmation. The data acquisition mode enables laboratories to interrogate data retrospectively to determine if novel compounds were present in any given sample.</p><h4><strong>Conclusions</strong></h4><ul><li>Clear and concise software workflow for quick screening analysis&nbsp;</li><li>Baseline resolution of THC isomers and interferences in longer method to allow for confident identification&nbsp;</li><li>All Ions acquisition method allows for retrospective data interrogation with fragment analysis</li></ul><h3><strong>2. KNAUER: Scaling up LNP formulation using a Reynolds number-based methodology</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/VPH_0084_knauer_scaling_up_lnp_formulation_using_a_reynolds_number_based_methodology_e05e67ca78.pdf"><strong>Full PDF for download</strong></a></li></ul><p>LNPs have become an essential enabling technology for RNA-based therapeutics and next-generation drug delivery systems. As these applications progress from laboratory research [1,2] to commercial manufacturing, process robustness and scalability become increasingly important. Beyond scalability, consistent product quality is critical.&nbsp;</p><p>In pharmaceutical development, predefined critical quality attributes (CQAs) such as particle size, PDI, encapsulation efficiency and active pharmaceutical ingredient (API) integrity define whether a formulation meets its intended performance and regulatory requirements. These CQAs are established during early formulation development and must be maintained throughout scaleup to ensure product consistency, pharmaceutical efficacy and reproducibility.</p><p>LNPs are typically generated by controlled mixing of a lipid phase in ethanol with an aqueous buffer containing the nucleic acid payload. The rapid solvent exchange initiates lipid self-assembly and determines the resulting nanoparticle characteristics. Because particle formation occurs on timescales comparable to the mixing process, the interplay between hydrodynamics and nanoparticle assembly is a key determinant of final product quality. Even minor variations in mixing conditions can influence particle size distribution, encapsulation efficiency, and overall formulation consistency.&nbsp;</p><p>To establish robust and scalable manufacturing processes, the underlying transport phenomena must be described independently of an operating scale. Dimensionless numbers provide a powerful framework for this purpose. The Reynolds number (Re) characterizes the flow regime and mixing intensity by relating inertial and viscous forces, while the Damköhler number (Da) describes the relationship between the characteristic timescales of mixing and nanoparticle formation. Together, these parameters provide a quantitative basis for understanding and controlling LNP self-assembly.</p><h4><strong>RESULTS&nbsp;</strong></h4><h5><strong>R&amp;D Evaluation and Hydrodynamic Characterization&nbsp;</strong></h5><p>The experimental study was initiated on <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=503&amp;search=IJM+NanoScaler"><strong>KNAUERs IJM NanoScaler</strong></a>, where multiple LNP formulations were developed and characterized under defined process conditions. During this phase, formulation parameters such as lipid composition, flow rate ratio (FRR), and total flow rate (TFR) were systematically varied to establish target CQAs, particularly particle size and PDI. In addition to recording volumetric flow parameters, the corresponding hydrodynamic conditions were quantified by calculating Re for each experimental setting, thereby the prevailing flow regime within the impingement zone.&nbsp;</p><h5><strong>Determination of a Critical Reynolds Number&nbsp;</strong></h5><p>Particle size was evaluated to depend on the Re using the <strong>IJM NanoScaler </strong>(Fig. 1). At Re below 500 particle sizes of 100 nm and larger were observed, indicating insufficient mixing and heterogeneous supersaturation conditions. With increasing Re, particle size decreased until reaching a plateau region at around 52 nm. Above a critical Reynolds number of ~ 750, further increases in flow rates did not significantly affect particle size. This plateau defines the hydrodynamic condition required to achieve minimal particle size for the given formulation.</p><h4><strong>CONCLUSION&nbsp;</strong></h4><p>A critical Reynolds number defining stable particle size and PDI was successfully identified on the R&amp;D-scale IJM NanoScaler. Operating above this threshold ensured consistent nanoparticle characteristics within a defined plateau region.</p><p>By transferring these hydrodynamic conditions to the benchtop system, predefined CQAs were reliably maintained across scales. The data demonstrate reproducible particle size and PDI during scale-up while enabling a substantial increase in throughput. These findings highlight that a Reynolds number driven approach provides a robust and scalable framework for predictable LNP manufacturing using IJM technology.</p><h3><strong>3. Shimadzu / ASMS: High-Throughput Ultra-Short-Chain PFAS Analysis in Drinking Water using LC-MS/MS with Automated Sample Preparation</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/TP_125_High_Throughput_Ultra_Short_Chain_PFAS_Analysis_in_Drinking_Water_using_LC_MSMS_with_Automated_Sample_Preparation_69e7985cce.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Ultra-short- and short-chain PFAS are highly mobile and persistent contaminants that are challenging to measure in drinking water due to high polarity, low molecular weight, poor chromatographic retention, and susceptibility to laboratory background contamination. This study evaluates a high-throughput LC–MS/MS workflow with automated sample preparation for targeted quantification of ultra-short and short-chain PFAS in drinking water. Method performance was assessed using native background, matrix spike recovery, precision, LOQ accuracy, calibration performance, and continuing calibration verification.</p><h4><strong>Method</strong></h4><p>Nine target PFAS were evaluated: TFA, TFMS, PFPrA, PFMOAA, PFEtS, PFBA, PFPrS, TFSI, and PFBS. Samples and calibrants were prepared in acidified 50:50 PFAS-grade water/methanol using PFAS-grade water provided by MilliporeSigma and an automated ePrep sample preparation system equipped with PFAS-free accessories.</p><p>Chromatographic separation was performed on a polar-embedded IBD column with a delay column to improve retention and minimize background interference. Analysis was performed on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-8065XE"><strong>Shimadzu LCMS-8065XE triple quadrupole system</strong></a> within an 8-minute total cycle time with a 10 µL injection volume (figure 2). Drinking-water samples were collected from seven local household sources and spiked at multiple concentration levels. Samples were ran in replicates to evaluate recovery, precision, and method robustness.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This 8-minute LC–MS/MS method enabled high-throughput analysis of ultrashort- and short-chain PFAS in drinking water. TFA background observed in blanks and unspiked samples emphasized the need for contamination control and matrix-specific background assessment. Practical LOQs were supported at 10 ng/L for most analytes and 50 ng/L for PFMOAA. Recovery and precision were generally acceptable from 100–1000 ng/L, with higher variability at 10 ng/L and for PFMOAA, indicating areas for further optimization. Calibration and CCV performance supported reliable quantification across the reportable range.</p><h3><strong>4. Thermo Fisher Scientific / ASMS: Unlocking the archived proteome: High-throughput, deep FFPE proteome profiling using the Orbitrap Astral 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_004694_lsms_protein_ffpe_orbitrap_astral_proteomics_po004694_asms2026_na_en_7cd59d64aa.pdf"><strong>Full PDF for download</strong></a></li></ul><p>FFPE tissue specimens are central to clinical pathology and translational cancer research, enabling long-term storage while preserving morphology for histology and molecular analysis. Widely available through biobanks, they support retrospective studies, biomarker discovery, and precision oncology—especially when paired with detailed clinical data. Compared to fresh tissues, FFPE samples are more accessible, scalable, and cost-effective for proteomics.</p><p>However, FFPE proteomics is technically challenging. Formaldehyde-induced crosslinking complicates protein extraction and digestion, while paraffin removal and crosslink reversal add complexity. Traditional workflows are labor-intensive, time-consuming, and prone to variability, limiting reproducibility and throughput. Although recent advances in sample preparation have improved performance, residual contaminants can still affect instrument robustness and scalability.&nbsp;</p><p>To address these challenges, we implemented a streamlined FFPE proteomics workflow that simplifies processing and improves peptide yield and reproducibility. Using FFPE lung tissue and the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2465"><strong>Thermo Scientific OptiSpray Ion source</strong></a> with the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/836"><strong>Orbitrap Astral Mass spectrometer</strong></a><strong> </strong>across two LC platforms, we achieved sensitive detection of low-abundance peptides from 20– 200 ng inputs. Combined with fast LC methods and acquisition rates of 60, 180, and 500 samples per day, this approach enables deep, scalable profiling. The automated OptiSpray Ion source also reduces instrument contamination, supporting robust, high-throughput analysis of archived clinical tissues for biomarker discovery and translational research.</p><h4><strong>Experimental procedure&nbsp;</strong></h4><h5><strong>Sample preparation&nbsp;</strong></h5><p>Lung tumor and lung normal samples were de-paraffinized using xylene and sequential ethanol washes. The optimized protein extraction protocol and Thermo Scientific EasyPep Mini MS sample prep kit was used to prepare the digest samples from FFPE sections of normal and tumor lung samples. Protein concentration was measured using Thermo Scientific Pierce Rapid Gold BCA Protein Assay kit. The peptides were quantified using the Thermo Scientific Pierce Fluorometric Peptide Assay Kit before LC-MS/MS analysis. For <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=291&amp;search=Evosep+ENO"><strong>Evosep ENO</strong></a>, peptides were loaded on EvoTips .&nbsp;</p><h5><strong>LC-MS analysis&nbsp;</strong></h5><p>Samples were injected onto an Thermo Scientific OptiSpray µPAC Neo Cartridge (P/N OS-UPAC050NAN) and Thermo Scientific OptiSpray µPAC Neo High-Throughput Cartridge (P/N OS-UPAC005CAP) and separated using 20 min (60 SPD) and 6.8 min (180 SPD) gradients, respectively, in direct injection mode at 55°C on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Thermo Scientific Vanquish Neo UHPLC System</strong></a>. For 500 SPD (2.3 min) separation, samples were processed on Evosep ENO using an Evosep EV1182 Performance Column at 40 °C. Detailed LC and MS parameters are provided in Tables 1–2.&nbsp;</p><h5><strong>Data analysis Spectronaut® Software&nbsp;</strong></h5><p>The raw DIA files from both the labeled and unlabeled samples were analyzed together using Biognosys Spectronaut® Software in directDIA mode. Exported output files were imported to R Studio (2023.09.0 Build 463) with R (v4.3.1) for downstream data analysis and visualization.</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>End-to-end FFPE proteomics is completed in under one day, integrating rapid sample preparation, fast LC–MS, and streamlined data analysis.&nbsp;</li><li>Deep proteome coverage is achieved from FFPE lung tissue, with up to ~8,600 protein groups and &gt;100,000 peptides identified from 200 ng input in 20 min.</li><li>Increasing throughput by up to ~8× (60 to 500 SPD) with moderate loss in depth, retaining ~70% of proteins at 180 SPD and ~45% at 500 SPD.&nbsp;</li><li>Robust quantitative performance is maintained at low sample input (20 ng) and across acquisition speeds, with median CVs ≤10%.&nbsp;</li><li>The workflow enables reliable differential expression and pathway analysis at scale, demonstrating its utility for biological insight into lung tumor and normal tissues.</li></ul><h3><strong>5. Waters Corporation / ASMS: Identification of Novel Per-and-Polyfluoroalkyl Substance (PFAS) Isoform in Textile Using a Multi-Reflecting Time-ofFlight Mass Spectrometer Technology</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009415_0b95241dfd.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><p>The poster presents a non-targeted LC-MS/MS workflow for identifying <strong>per- and polyfluoroalkyl substances (PFAS)</strong> in textile materials using high-resolution mass spectrometry. As concerns over PFAS exposure continue to grow, conventional targeted methods often capture only a limited number of compounds. The authors therefore combined <strong>data-dependent acquisition (DDA)</strong> with high-resolution accurate-mass analysis to characterize PFAS profiles more comprehensively, enabling the identification of novel PFAS isoforms and halogenated contaminants with high confidence.</p><p>The analytical workflow was based on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>Waters ACQUITY Premier UPLC system</strong></a> equipped with a PFAS solution installation kit and an <strong>ACQUITY Premier BEH C18 (2.1 × 50 mm, 1.7 µm) column</strong>, coupled to the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2433"><strong>Waters Xevo MRT P10 multi-reflecting time-of-flight (MRT) mass spectrometer</strong></a>. Textile reference material was extracted according to <strong>EN 17681-1:2025</strong>, and LC-MS/MS data were acquired in <strong>data-dependent acquisition (Top 5 DDA)</strong> mode. Data processing and compound identification were performed using the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1544"><strong>waters_connect™ Software Platform</strong></a>, combining accurate precursor and fragment masses with isotopic information.</p><p>A key innovation of the study was the implementation of <strong>mass defect-directed DDA</strong>. By creating a database of nearly <strong>19,600 unique PFAS-related compounds</strong> and using their characteristic mass defects to guide precursor selection, the workflow reduced the number of non-specific MS/MS spectra by approximately <strong>25%</strong>. This allowed the instrument to focus on PFAS-like compounds more efficiently, increasing the number of informative fragmentation spectra and improving the identification of previously unknown PFAS species. The approach successfully identified compounds such as <strong>N-ethyl perfluorooctane sulfonamidoethanol (N-EtFOSE)</strong> in textile extracts with excellent mass accuracy (1.1 ppm).</p><p>The authors conclude that <strong>mass defect-driven DDA</strong> significantly enhances non-targeted PFAS screening by reducing unnecessary MS/MS acquisitions while increasing the number of confidently identified PFAS and PFAS-like compounds. They also suggest that this strategy can be extended beyond PFAS analysis to other classes of persistent environmental contaminants, including <strong>polychlorinated biphenyls (PCBs)</strong> and <strong>polybrominated biphenyls (PBBs)</strong>, making it a promising approach for broader environmental and materials analysis.</p></div></div></div></div></div></div></section></div></div>

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RECETOX (Research Centre for Toxic Compounds in the Environment) is an independent department of the Faculty of Science of Masaryk University in Brno, which has been established in 1983. RECETOX is focused on the research and education in cross-cutting area of Environment and Health. It addresses interactions among chemicals, environment, and biological systems, including consequences at local, regional, and global levels.

RECETOX - Centrum pro výzkum toxických látek v prostředí

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