<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 7th July 2025? 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 note by <strong>Agilent Technologies </strong>and posters by<strong> Shimadzu / ASMS, Thermo Fisher Scientific / ASMS </strong>and<strong> Waters Corporation / ASMS!</strong></p><h3><strong>1. Agilent Technologies: Rapid and Sensitive Analysis of Antifungal Agents in Human Serum Using the Agilent 6475 LC/TQ</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_antifungal_human_serum_5994_8338en_agilent_89f89cb4dc.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In addition to minimizing drug-related toxicity, TDM has been hailed as a key step to prevent the emergence of drug resistance. The growing number of invasive fungal infections creates a ripple effect on the rapid advancement of TDM for antifungal agents. Increasing evidence confirms the critical role of TDM in preventing and treating antifungal infections.1 The RECIPE ClinMass TDM kit system for antimycotics in serum (Munich, Germany) was used on a 6475 LC/TQ for the analysis of eight antifungal agents. This application note demonstrates the evaluation and validation of the RECIPE TDM kit, covering sensitivity, linearity, and robustness across five consecutive days (n =&nbsp;5). Quick and simple sample preparation was implemented, providing high-throughput monitoring of antifungal agents in biological&nbsp;samples.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumentation</strong></h5><ul><li><strong>Liquid Chromatography System&nbsp;</strong><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=Agilent+1290+Infinity+II"><strong>Agilent 1290 Infinity II</strong></a> High-Speed Pump&nbsp;</li><li>Agilent 1290 Infinity II Multisampler&nbsp;</li><li>Agilent 1290 Infinity II Multicolumn Thermostat&nbsp;</li></ul></li><li><strong>Mass Spectrometry System&nbsp;</strong><ul><li>Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=6475+LC%2FTQ"><strong>6475 LC/TQ &nbsp;</strong></a></li><li>Agilent Jet Stream Technology Ion Source (AJS)</li></ul></li></ul><h5><strong>Method&nbsp;</strong></h5><p>The optimization of multiple reaction monitoring (MRM) transitions for analytes and ISTDs was carried out using Auto MRM Optimizer in the Agilent MassHunter acquisition software to provide optimal sensitivity and selectivity. Data were processed using the Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=MassHunter+Qualitative+Analysis+software"><strong>MassHunter Qualitative Analysis software</strong></a>, version B.12, and Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=MassHunter+Quantitative+Analysis+software"><strong>MassHunter Quantitative Analysis software</strong></a>, version B.12.</p><h4><strong>Results and discussion&nbsp;</strong></h4><p>Figure 2 shows the chromatograms of quantifier MRM transitions for the eight antifungal agents at the lowest calibration level. Six out of eight antifungal agents had good chromatographic separation across the run time. The retention times of two antifungals, posaconazole and hydroxy-itraconazole, were slightly overlapped. Despite this overlap, measurement integrity can still be maintained due to MRM selectivity.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>A fast and sensitive analysis of eight antifungal agents in serum was validated on an Agilent 6475 triple quadrupole LC/MS. By employing a ready-to-use RECIPE ClinMass TDM kit, this method demonstrates accurate and precise quantitation of antifungal agents in biological samples. Additionally, the streamlined sample preparation method allows high throughput analysis of up to 350 samples per day.</p><h3><strong>2. Shimadzu / ASMS: Robustness Evaluation of PFAS Analysis in Soil Using LC-MS/MS</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_25_WP_137_e932b391c7.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Per- and polyfluoroalkyl substances (PFAS) are widely used in various fields and industries. However, due to their structural stability and resistance to degradation, they accumulate in the environment and are suspected of being harmful to humans. PFAS in soil can accumulate in the human body via agricultural products, thus it is essential to develop sensitive and robust analytical methods for the detection of PFAS in soil with complex matrices.1 This study shows a robustness evaluation by adding 30 PFAS to a soil matrix and using the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=LCMS-8060RX"><strong>LCMS-8060RX</strong></a> to measure these PFAS in the soil matrix 500 consecutive times.</p><h4><strong>Methods&nbsp;</strong></h4><p>For this analysis, LC-MS/MS equipped with a newly designed ESI source was used, and a delay column was installed between the mixer and the autosampler to inhibit the effects of PFAS contamination from the LC system. Six points calibration curves were built, and each calibration point was measured 3 times. A soil sample was prepared referring to part of the soil preparation procedures published by the National Agricultural and Food Research Organization. 2 Thirty PFAS compounds were spiked to the soil sample at 0.1 μg/L after pretreatment and 500 soil sample analyses were performed for the robustness evaluation. This sample contains more than 90% soil matrix. QC samples were also analyzed after every 20 injections of the soil samples.</p><h4><strong>Conclusion</strong></h4><p>The <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=LCMS-8060RX"><strong>LCMS-8060RX</strong></a> performed 500 consecutive measurements of 30 PFAS spiked to a soil matrix sample. The results showed good peak area repeatability, good peak shapes, and good recovery. The newly designed ESI source showed excellent robustness, and stable analysis was achieved over a long period, even for samples with complex matrices.</p><h3><strong>3. Thermo Fisher Scientific / ASMS: Evaluation of a modified Orbitrap Astral Mass Spectrometer for label-free quantitation of proteomic samples</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PO_439_ms_ASMS_25_Astral_Zoom_LFQ_po439_na_en_c1a0b2a11e.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The demand for high-throughput proteomics analysis of complex samples is continually increasing, focusing on greater analysis depth and improved precision and accuracy in quantitation. Label-free quantitation of very complex proteomic samples poses significant challenges for mass spectrometers, requiring faster and more efficient processing of eluting peptide ions and their fragments. The new Orbitrap Astral Zoom mass spectrometer addresses these challenges, offering a higher acquisition rate by improved ion optics switching times and faster ion transfer, higher sensitivity due to ion pre-accumulation, and enhanced spectral processing, leading to deeper coverage with higher confidence.</p><h4><strong>Materials and methods</strong></h4><h5><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Vanquish Neo</strong></a><strong>: Direct injection mode using 25cm x 75 μm ID Aurora Ultimate TS column (IonOpticks)&nbsp;</strong></h5><ul><li>High loads: 37min gradient; 4-45%B and injection-to-injection time 48min (30SPD)&nbsp;</li><li>Low loads: 20min gradient; 1-40%B and injection-to-injection time 28min (50SPD)&nbsp;</li></ul><h5><strong>Mass Spectrometer: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/836"><strong>Orbitrap Astra</strong></a><strong>l and </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom&nbsp;</strong></a></h5><ul><li>Orbitrap (MS1) and Astral (MS2) detectors&nbsp;</li><li>Orbitrap: 240K; m/z range 380-980; AGC 500%; max IT 5ms&nbsp;</li><li>NCE 25; Thermo Scientific FAIMS Pro Duo (low loads): -48V; gas 3.5 L/min</li><li>Astral: DIA; window size depending on loads (in the tables below); m/z 150-2000; AGC 800% (low loads) or 100% (high loads); max IT depending on load; cycle time: 0.6s&nbsp;</li></ul><h5><strong>Data Processing&nbsp;</strong></h5><ul><li>Spectronaut® v19.5 Direct DIA, 6 files (2 x 3 replicates) processed together for each load; all other settings were default&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1782"><strong>Thermo Scientific Proteome Discoverer software </strong></a>3.3.0.54, CHIMERYS 4.0.21</li><li>Human, E.coli, and Yeast FASTA (all w/o isoforms) from UniProt; normalization by Human FASTA</li></ul><h4><strong>Results (High Loads)</strong></h4><p>The new Orbitrap Astral Zoom mass spectrometer takes advantage of ion preaccumulation in the bent trap, increasing the effective MS2 injection time. Its reduced ion transfer overheads result in a higher MS2 acquisition rate of up to 270 scans per second. Additionally, an enhanced spectral processing algorithm was implemented to deconvolute overlapping spectral features in MS2, for better handling spectra with increased spectrum density.&nbsp;</p><p>Using Orbitrap Astral Zoom MS and Spectronaut® 19.5 software, there was a 12-17% increase in IDs at the precursor level, 10-15% at the peptide level (stripped sequence), and 4-9% at the protein groups level. With Proteome Discoverer software, the gain was 12-19% at the DIA precursor level, 12-17% at the peptide level, and 4-7% at the protein group level. The increase in identifications was primarily observed for low-abundant species. Orbitrap Astral Zoom mass spectrometer also yielded, on average, a 15% higher median number of MS2 data points per peak, while maintaining consistently high quantitation precision and accuracy at the MS2 level.</p><h4><strong>Conclusions</strong></h4><p>The novel Orbitrap Astral Zoom mass spectrometer demonstrates improved performance for qualitative and quantitative analysis of complex proteomics samples over a wide range of sample loads spanning four orders of magnitude, from 100 pg to 1µg.</p><h3><strong>4. Waters Corporation / ASMS: Investigating Fire Fighter and E-waste Handlers Exposure to PFAS Using Liquid Chromatography and Cyclic Ion Mobility Mass Spectrometry</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008883_21620a6293.pdf"><strong>Full PDF for download</strong></a></li></ul><p>PFAS are persistent environmental pollutants linked to health risks, including cancer. Monitoring their levels in human biofluids provides insight into exposure pathways. However, the analysis of PFAS isomers is technically challenging due to their structural similarity. To overcome this, the study employs <strong>LC coupled with cyclic ion mobility mass spectrometry (LC-cIM-MS)</strong> using the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/202"><strong>Waters SELECT SERIES Cyclic IMS</strong></a>, which adds a new separation dimension for better specificity.</p><h4><strong>Methods</strong></h4><p>Serum samples from Ghanaian firefighters and E-waste workers were prepared using <strong>solid-phase extraction (SPE)</strong> on 96-well µElution plates. A <strong>22-minute reversed-phase LC gradient</strong> was used for separation. The <strong>Cyclic IMS system</strong>, with ion mobility resolution R~65 and 145, enabled non-targeted PFAS analysis, including the generation of <strong>collision cross section (CCS)</strong> values to support compound identification.</p><h4><strong>Results</strong></h4><ul><li>PFAS compounds such as <strong>PFOS, PFHxS, PFHpS, PFNA</strong>, and <strong>6:2 FTS</strong> were identified in real serum samples.</li><li>The <strong>cyclic IMS</strong> allowed for the separation of coeluting isobaric compounds, such as <strong>PFOS isomers</strong> and <strong>cholic acid biomarkers</strong>, minimizing false identifications (Figure 3).</li><li><strong>Figure 4</strong> lists CCS values and other parameters for PFAS standards and identified analytes from a firefighter serum sample.</li><li><strong>Figure 5</strong> shows ion mobility conformeric profiles for <strong>PFNA</strong>, enabling reliable identification even at low signal intensities.</li></ul><h4><strong>Conclusion</strong></h4><p>The LC-cIM-MS method:</p><ul><li>Significantly improves specificity in PFAS identification.</li><li>Enables both <strong>targeted and untargeted detection</strong> of known and unknown PFAS in complex human samples.</li><li>Can be a key part of future occupational and environmental exposure assessments.</li></ul>

News from LabRulezLCMS Library - Week 28, 2025

News from LabRulezLCMS Library - Week 31, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 8th September 2025? 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> Shimadzu </strong>and<strong> </strong>posters by <strong>Thermo Fisher Scientific / HPLC Symposium </strong>and <strong>Waters Corporation!</strong></p><h3><strong>1. Agilent Technologies: Automated Solid Phase Extraction of PFAS from Aqueous Samples</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_1633_automated_spe_wax_carbon_s_5994_8289en_agilent_1fc425207e.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In this study, three types of dual-phase SPE cartridges were evaluated based on the quality control requirements for aqueous matrices as specified in US EPA Method 1633 using automated SPE. The cartridges contained PFAS WAX and Carbon S for PFAS. In the first configuration, a 200 mg bed of PFAS WAX was layered on top of a 50&nbsp;mg bed of Carbon S with the sorbents separated by a frit. In the second configuration, 200 mg of PFAS WAX was mixed with 50 mg of Carbon S before cartridge packing. In the third configuration, 200 mg of PFAS WAX and 10&nbsp;mg of Carbon S were mixed before cartridge packing. All three configurations were evaluated under identical protocols using automated SPE and were compared to results obtained using the manual addition of carbon and separate WAX extraction. The blended sorbent containing 200 mg of PFAS WAX and 10 mg of Carbon S was selected for validation and further evaluation of several environmental matrices including groundwater from residential private wells, effluent from a wastewater storage lagoon, and a landfill monitoring&nbsp;well.</p><h4><strong>Experimental</strong></h4><h5><strong>Equipment and materials</strong></h5><p>The three Agilent dual-phase cartridges used in the study are listed in Table 1. As a performance benchmark, a single‑phase <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=Bond+Elut+PFAS+WAX"><strong>Bond Elut PFAS WAX sorbent</strong></a> cartridge (Agilent, part number 5610‑2151) was used with either Carbon S bulk (Agilent, part number 5610-2095) or Superclean ENVI-Carb (Millipore Sigma, part number 57210-U).</p><p>Samples were extracted using the PromoChrom eight‑channel automated SPE extractors with upside‑down shaker racks (part number SPE-03 with MOD004), anticlogging frits (part&nbsp;number CF-06), high-capacity inline filters (part&nbsp;number&nbsp;F-HC-30), and anticlogging tips (part&nbsp;number F-T-4). Sample analysis was performed using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=1290+Infinity+II+LC"><strong>Agilent 1290 Infinity II LC</strong></a> system consisting of an Agilent 1290 Infinity&nbsp;II high-speed pump (G7120A), an Agilent 1290 Infinity II multisampler (G7167B), and an Agilent 1290 Infinity II multicolumn thermostat (G7116B). The LC system was modified for PFAS analysis using the Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=InfinityLab+PFC%E2%80%91free+HPLC+conversion+kit"><strong>InfinityLab PFC‑free HPLC conversion kit </strong></a>(part number 5004-0006). The LC system was coupled to an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=6495C"><strong>Agilent 6495C triple quadrupole LC/MS</strong></a> equipped with an Agilent Jet Stream technology ion source. Agilent <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=MassHunter+Workstation"><strong>MassHunter Workstation software</strong></a> was used for data acquisition (version 10.1) and <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=Quantitative+Analysis+"><strong>Quantitative Analysis </strong></a>for QQQ (version 12.1) was used for data analysis. Instrumental conditions were determined based on detailed multiparametric optimization experiments developed in‑house.&nbsp;</p><h4><strong>Conclusion&nbsp;</strong></h4><p>The adoption of automated solid phase extraction (SPE) for PFAS analysis in environmental matrices significantly enhances laboratory efficiency and reduces the potential for human error. Our evaluation of five extraction protocols revealed that the blended sorbent containing 200 mg of PFAS WAX and 10 mg of Carbon S provided the best performance in terms of recovery, matrix interference reduction, and fewer outliers. This configuration was successfully applied to various environmental samples, demonstrating its versatility and reliability. The findings support the use of automated SPE with optimized sorbent cartridges as a robust method for PFAS analysis, aligning with the quality control metrics of US EPA Method 1633. Future work should focus on further refining automated SPE techniques and exploring their application to other environmental matrices.</p><h3><strong>2. Shimadzu: Automated Preparation of Calibration Curves Using the Autosampler's Dilution Function</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_00914_en_089a8c34fa.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>The auto-dilution function equipped in the autosampler eliminates the need for manual dilution during calibration curve creation and sample preparation.</li><li>Samples can be automatically diluted to create a calibration curve by specifying the desired dilution factor in the batch table.</li><li>Because the same method file can be used across different dilution factors, only minor adjustments are needed when changing dilution conditions.&nbsp;</li></ul><p>In LC quantification, the dilution ofstandard and sample solutions is typically performed manually using pipettes, which is a laborintensive and time-consuming process. Recent advancements have called for automation to reduce labor and improve efficiency. By automating the dilution process, workflows can be streamlined, leading to increased productivity. The Nexera series autosamplers are equipped with an automatic pretreatment function that enables automated dilution. Using the auto-dilution function, samples can be automatically prepared at any desired dilution factor and directly introduced into the analytical column. This article presents a method to automate the creation of calibration curves and subsequent quantification workflows using the autosampler’s auto-dilution function.</p><h4><strong>Automated Dilution Analysis of Organic Acid Standard Solution</strong></h4><p>Automated dilution analysis was conducted using a 1000 mg/L mixed standard solution of ten organic acids. The analytical conditions are shown in Table 2 (pretreatment program : Table 1). 1.0 mL polypropylene vials were used as mixing vials, and septum-sealed vials were used for the undiluted standard solution. Rinse solution (ultrapure water) was used as the diluent. Fig. 3 shows the chromatogram of the 100-fold diluted organic acid mixed standard solution (concentration after auto-dilution : 10 mg/L for each organic acid). The <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+Organic+Acid+Analysis+System"><strong>Nexera Organic Acid Analysis System</strong></a> (pH-buffered electric conductivity detection) was employed for this analysis.</p><h4><strong>Conclusion</strong></h4><p>By utilizing the auto-dilution function in the autosampler, the standard undiluted solution for calibration curve creation can be automatically diluted at any desired dilution ratio. This eliminates the need for manual sample dilution and streamlines the calibration curve creation workflow. Additionally, since the autodilution function can also be applied to sample solutions, only the preparation of undiluted standard and sample solutions is required, allowing for a fully automated process from calibration curve creation to quantitation. As a result, the reduction in pretreatment work contributes to improved work efficiency and productivity.</p><h3><strong>3. Thermo Fisher Scientific / HPLC Symposium: Wide-ranging polynucleotide separation capabilities using Reversed Phase particles with variable pore geometry</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_wide_ranging_polynucleotide_separation_capabilities_po_en_1fdaba9e08.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Polynucleotides such as DNA and RNA serve many uses in the areas of basic research, industrial manufacturing, therapeutics to up/down regulate cellular functions, and as therapeutic and vaccine intermediates (i.e., as an instructional template to produce proteins that 1) supplement/replace ineffective proteins or 2) function as antigens). CRISPR technology using guide RNA (gRNA, ~100mer) to directly modify cellular chromosomes was recently leveraged to create a customized treatment within 6-months for an infant with CPS1 deficiency1. This approach has provided long-term, life-saving enzyme production negating the need for daily treatments. Associated DNA and RNA such as gRNA and mRNA (1000+mer) require detailed characterization to ensure safety and efficacy (e.g., of sufficient quantity and fidelity in delivery vehicles such as lipid nanoparticles). Here, we present a RP particle with complex pore geometry and the effects of mobile phase and temperature for separating DNA/RNA with therapeutic benefits (siRNA-gRNA-mRNA:~ 20-100- 1000+mer). Semi-prep column separations, common for sample recovery for subsequent analyses or sample enrichment for in vitro or in vivo use, is also shown.</p><h4><strong>Materials and methods</strong></h4><h5><strong>Test method(s)&nbsp;</strong></h5><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=3&amp;search=DNAPac+RP+column"><strong>DNAPac RP columns</strong></a> packed with 4 µm DNAPac RP media include 2.1 × 50 mm (P/N 088924), 2.1 × 50 mm (P/N 088924), and 21.2 × 150 mm (P/N 080922- 1521232). For instruments, mobile phases, gradient conditions, and other chromatographic operating parameters (flow rate, temperature, injection volume, etc.), please reference the figures and associated text. For all analyses, samples were detected by UV absorbance at 260nm. For 21.2x150mm semi-prep separations, a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products?category=40&amp;manufacturerItems=3"><strong>conventional (U)HPLC chromatography system</strong></a> with a binary pump, autosampler and detector without column compartment (ambient temperature separations) was used for all analyses. Ion Pairing Agents (Cation Anion): TEAA – Triethylamine Acetate, HAA – Hexylamine Acetate, HFIP – Hexafluoroisopropanol.&nbsp;</p><h5><strong>Data analysis&nbsp;</strong></h5><p>The <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/76"><strong>Thermo Scientific Chromeleon </strong></a>7.2.10 or 7.3 Chromatography Data Systems (CDS) software was used for data acquisition and analysis.</p><h4><strong>Results&nbsp;</strong></h4><h5><strong>DNAPac RP particle characterization – chemistry and pore structure&nbsp;</strong></h5><p>Figure 1 summarizes the chemical and physical properties of the resin, which is based on polymeric divinylbenzene (top left). Unlike conventional silica particles, the polymeric resin is not susceptible to hydrolytic degradation at neither extreme pH (1-14) nor high temperature (90+oC). The aromatic groups also provide π- π bonding with aromatic nucleotides giving different selectivity from conventional alkyl phases incapable of such interactions. The SEM image visually shows the highly variated porous structure of the particles. Barrett-Joyner-Halenda (BJH) N2 adsorption analysis details the surface area contributions of the different pore sizes. From this analysis it is clear that a continuum of pores from 50Å to 2500Å (suitable for small molecules up to macromolecule adsorption, respectively) contributes to the overall surface area of the particle. Based on the complex geometry and resulting pore structure, we commonly refer to the media as a supermacroporous (SMP) particle.</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>High resolution separation of nucleic acids varying in length from 10 to 10,000 nucleotides is achieved using an SMP particle with a variable pore structure.</li><li>Polymeric SMP particles are compatible with different mobile phase IP compositions, high pH and high separation temperature, which are critical parameters for optimizing the separation of polynucleotides&nbsp;</li><li>SMP particles provide high resolution separations in both analytical and semi-prep formats</li></ul><h3><strong>4. Waters Corporation / ASMS: Detection and Characterization of PFAS Molecules Using Inclusion and Exclusion Features of Data Directed Analysis (DDA)</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008869_fb6d27e0a0.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Polyfluorinated alkyl substances (PFAS) are bioaccumulative and suspected to contribute to increased cancer risk in humans. Monitoring PFAS in biofluids is possible, but their very low concentrations present analytical challenges.</p><p>Data-Directed Acquisition (DDA) isolates ions that meet defined criteria, fragments them at elevated collision energies, and generates product ion spectra. Because PFAS ions show a characteristic <strong>mass defect</strong> due to fluorine atoms, inclusion lists can enhance their detection. Conversely, exclusion lists derived from background matrix analyses help remove interferences, simplifying ion selection for fragmentation.</p><p>Preliminary tests with mixed small-molecule samples demonstrated the utility of these lists before applying them to PFAS, where inclusion lists contained hundreds of entries and exclusion lists thousands.</p><h4><strong>Methods</strong></h4><ul><li><strong>Instrument:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/202"><strong>SELECT SERIES™ Cyclic™ Ion Mobility Mass Spectrometer</strong></a></li><li><strong>Acquisition:</strong> ToF-ESI negative DDA mode, 100 ms survey/MSMS scan times, collision energy ramps optimized by PFAS class</li><li><strong>LC System:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>ACQUITY Premier </strong></a>with PFAS Kit and Atlantis Premier BEH C18 AX Isolator Column (2.1 × 50 mm, 5 µm)</li><li><strong>Analytical Column:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1952"><strong>ACQUITY UPLC HSS T3 C18</strong></a> (100 × 2.1 mm, 1.8 µm) at 35 °C</li><li><strong>Flow Rate:</strong> 0.3 mL/min; <strong>Injection Volume:</strong> 5 µL; <strong>Autosampler Temp:</strong> 6 °C</li><li><strong>Mobile Phases:</strong><ul><li>A: H₂O:MeOH (95:5) with 2 mM ammonium acetate</li><li>B: MeOH with 2 mM ammonium acetate</li></ul></li><li><strong>Samples:</strong> LCMS QC mixture, native PFAS mixture (PFAC30PAR, Wellington Labs), and human serum</li><li><strong>Software:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/635"><strong>MassLynx™ 4.2 for acquisition</strong></a>, <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1544"><strong>waters_connect™ with PFAS library</strong></a> (130 entries) for processing, Tibco Spotfire® for visualization</li></ul><h4><strong>Conclusion</strong></h4><ul><li>ToF-DDA mode on a cyclic ion mobility mass spectrometer is effective for PFAS analysis.</li><li>Inclusion lists based on PFAS mass defect improve real-time detection and intelligent switching.</li><li>Background-derived exclusion lists (up to 9000 entries) further reduce interferences and enhance specificity.</li></ul>

News from LabRulezLCMS Library - Week 37, 2025

News from LabRulezLCMS Library - Week 05, 2026

<p><strong>This study introduces atmospheric solids analysis probe high-resolution tandem mass spectrometry with cyclic ion mobility as a novel approach for characterizing Asian lacquers. Applied to 27 historical samples from Japan, China, Vietnam, and Myanmar, the method enabled classification by geographic origin based on phenol and benzenediol derivatives.</strong></p><p>In addition to lacquer identification, the technique simultaneously detected pigments such as arsenic sulfides and associated resins, providing comprehensive chemical insight. This approach expands analytical capabilities for cultural heritage studies, supporting restoration, conservation, and art historical research.</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572"><strong>Characterization of Asian lacquers by atmospheric solids analysis probe high resolution tandem mass spectrometry coupled with cyclic ion mobility separation</strong></a></h4><p>Vojtěch Zemek, Radek Ryšánek, Petra Krejčí, Lukáš Kučera, Jana Nádvorníková, Adéla Tůmová, Helena Heroldová, Adriana Stříbrná, Petr Bednář</p><p>Journal of Cultural Heritage, 77, 2026, 187-196</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1016/j.culher.2025.11.012">https://doi.org/10.1016/j.culher.2025.11.012</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>In recent years, an expansion of ambient pressure ionization mass spectrometry in various areas is observed [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0024"><span>24</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0025"><span>25</span></a>]. Atmospheric solids analysis probe mass spectrometry (ASAP-MS) is a powerful technique for direct analysis of even very complex samples, such as polymers [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0026"><span>26</span></a>], foods [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0027"><span>27</span></a>], or petrochemical sources and products [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0024"><span>24</span></a>]. ASAP ionization technique is a modification of atmospheric pressure chemical modification (APCI). In conventional arrangement, the sample is attached to a sampling probe tip (a standard melting point capillary is inserted into powder or liquid sample that sticks to its surface) and the probe is consequently placed into the ion source (commonly adapted ESI or APCI source). The analytes are released into the gas phase using hot gas (nitrogen) and ionized in the corona discharge. The formed ions (quasimolecular ions, radical cations or radical anions) are then transferred to the evacuated part of mass spectrometer [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0024"><span>24</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0025"><span>25</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0028"><span>28</span></a>]. Note that especially at higher vaporization temperatures a portion of the analytes is pyrolyzed and a mixture of parent ions and pyrolysis product ions is commonly observed in the ASAP-MS spectra [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0029"><span>29</span></a>]. The main feature of this direct MS mode is a fast detection of the formed products (including those with a higher mass and perhaps a shorter lifetime). In contrast, due to chromatographic separation in py-GC/MS, only relatively stable and volatile products are detected (the chromatographic step provides an additional selectivity here). In addition, electron impact ionization produces significantly different spectra profiles compared to the atmospheric pressure chemical ionization ongoing in the ASAP source. Both techniques are to a certain extent complementary [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0024"><span>24</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0025"><span>25</span></a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0030"><span>30</span></a>].</p><p>There is a direct possibility of coupling mass spectrometry with ion mobility spectrometry (IMS) to significantly improve the selectivity of analysis (and, to certain extent, to compensate the advantage of the chromatographic step in py-GC/MS while maintaining the direct MS analysis speed). During an ion mobility spectrometry experiment, ions of analytes are flying through the ion mobility cell (e.g., a drift tube or a closed-loop path within a traveling wave ion guide in case of the cyclic ion mobility cell) filled with buffer gas (e.g. helium). In this process, ions collide with the buffer gas. These collisions slow down the ions differently based on their size, shape and charge. Ion mobility spectrometry therefore allows separation of the present analytes in the gas phase according to their collision cross sections (CCS). It also allows separation of isomeric compounds and filtration of the matrix signals, resulting in a higher quality of the MS and MS/MS spectra [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0031"><span>[31]</span></a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0032"><span>[32]</span></a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0033"><span>[33]</span></a>].</p><p>ASAP-MS has a high potential for the study of protective and decorative layers on the surfaces of historical objects. To the best of our knowledge, however, ASAP-MS and ASAP-IMS-MS have never been used for characterization of lacquers. This paper deals with the development of ASAP-MS method for characterization of Asian lacquers and its application for classification of oriental historical objects.</p><h4><strong>3. Material and methods</strong></h4><h5><strong>3.3. Instrumentation and experimental setup</strong></h5><p>Analyses were performed using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/202"><strong>Waters Cyclic IMS high resolution tandem mass spectrometer</strong></a> with an integrated cyclic ion mobility cell and atmospheric solids analysis probe (ASAP) used as ion source (Waters, Milford, MA, USA). Samples (∼ 0.1–0.5 mg) were inserted into a melting point capillary (G119/32, manufacturer SAMCO, United Kingdom) through an in-lab radially drilled hole (hole diameter: approx. 1 mm; distance from the bottom end approximately 5 mm). Solution of 2′,4′,6′-trihydroxyacetophenone monohydrate (THAP) in acetone was used as a standard for lock mass correction (<i>c</i> = 1 mg.ml<sup>-1</sup>). The m/z values were calculated as the means from three repeated measurements of appropriate samples. Approx. 1 μl of standard was deposited onto the capillary using a small pipette tip. Following experimental parameters were used: desolvation temperature of 600 °C, source temperature of 100 °C, corona “current” mode (corona current 2.0 μA), cone voltage of 30 V, source offset of 10 V, cone gas flow of 30 l/min, desolvation gas flow of 500 l/min, nebulizer gas pressure of 6 bar and reference capillary voltage of 2.5 kV. As for the ion mobility separation setup, a cyclic ion mobility cell was used in the following sequence: 1. Inject (10 ms), 2. Separate (37 ms), 3. Inject to Pre-Store (0.50 ms), 4. Eject (0.50 ms), 5. Reinject from Pre-Store (0.63 ms), 6. Eject and Acquire (13.20 ms). TW static height was 11 V, TW ramp start height was 15 V and TW ramp end height was 35 V. Acquisition time was 3 min for the MS scan and 1 min for the MS/MS scan used for identification of analytes. In the MS/MS mode, collision energy 30 V was used for pentadecyl and heptadecylcatechols, 35 V for phenols substituted with (CH<sub>2</sub>)<sub>10</sub>C<sub>6</sub>H<sub>5</sub> and 40 V for catechols substituted with (CH<sub>2</sub>)<sub>12</sub>C<sub>6</sub>H<sub>5</sub> and phenols substituted with CH<sub>2</sub>CO(CH<sub>2</sub>)<sub>10</sub>C<sub>6</sub>H<sub>5</sub>, respectively. Scan time 1 s was used for both scans. At the end of each working day, sample V was measured for confirmation that the instrument measured consistently. Values of m/z were calculated by MassLynx software (version 4.2, SCN 1016) after lock mass correction using the signal of protonated molecule of THAP. Theoretical mass of particular analyte was used for lock mass correction in the MS/MS spectra. Centroid top at 80 % and areas of peaks were used for accurate mass and intensity of signals calculation. The maximal accepted difference from theoretical mass (dtm) of signals was 10 mDa. Peak areas were used to compare the abundance of identified analytes among particular samples. Mobilograms from cyclic ion mobility experiments were produced by DriftScope v2.9 software. In mobilograms, spectra were generated by integration at Full Width at Half Maximum (FWHM) of peaks at drift time 1.72 ms.</p><h4><strong>4. Results and discussion</strong></h4><h5><strong>4.1. Utilization of ASAP-MS</strong></h5><p>In the ASAP-MS spectra of the studied lacquers, signals of a several compounds were observed (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#fig0002"><span>Fig. 2</span></a>). Signals of radical cations as well as protonated molecules of identified analytes were easily visible. Usually a slightly higher abundance of cation radicals compared to protonated molecules was observed (spectra of all samples are listed in Supplementary material B). The processes observed in the ASAP-MS spectra involve the release of alkyl phenol/alkyl catechol monomer(s) and cleavages of alkyl chain(s) after the carbon linked to the phenol/catechol ring (i.e. cleavage after the first, second and third alkyl carbons) and elimination of water either from polymer or released monomers (the pyrolytic/collision-induced fragmentation processes are discussed below in detail). The analysis of provided samples revealed the most important markers of specific types of lacquers.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Journal_of_Cultural_Heritage_77_2026_187_196_Fig_2_Spectra_of_lacquers_prepared_from_Toxicodendron_vernicifluum_Toxicodendron_succedaneum_and_Gluta_usitata_samples_U_V_and_B_0200c24c06.jpg" alt="Journal of Cultural Heritage, 77, 2026, 187-196: Fig. 2. Spectra of lacquers prepared from Toxicodendron vernicifluum, Toxicodendron succedaneum and Gluta usitata (samples U, V and B)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Journal_of_Cultural_Heritage_77_2026_187_196_Fig_2_Spectra_of_lacquers_prepared_from_Toxicodendron_vernicifluum_Toxicodendron_succedaneum_and_Gluta_usitata_samples_U_V_and_B_0200c24c06.jpg 245w," sizes="100vw" width="2750" height="1269"></p><h5><strong>4.1.4. Study of MS/MS spectra of characteristic markers</strong></h5><p>For all the standard materials, the most important markers were subjected to fragmentation after the collision induced dissociation (CID) in the Trap collision cell of the mass spectrometer (MS/MS experiments; all fragmentation spectra and observed diagnostic fragments including differences from theoretical masses are given in Supplementary material B).</p><p>Signals of fragments with an intensity higher than the specified percentage of well known fragments arising from studied compounds were investigated and identified. Diagnostic fragments are given in Table B.2, Supplementary material B. The threshold signal was set for different compounds. For heptadecyl- and pentadecylcatechols, the threshold signal was defined as 5 % of the signal of dihydroxytropylium that is always an integral component of their collision spectra. For heptadecenyl- and pentadecenylcatechols the threshold signal was 2.5 % of dihydroxytropylium. For pentadecatrienyl catechol it was 100 % of dihydroxytropylium while for dodecylphenylcatechol it was 1 % of dihydroxytropylium. In case of 1-(3-hydroxyphenyl)-12-phenyldodecan-2-one, the threshold signal was defined as 17 % of the signal of hydroxyphenylethan-2-one. Finally, for 10-decylphenylphenol and 12-dodecylphenylphenol, 50 % of the signal of methylphenol was used as the threshold signal. These fragments were used for confirmation of the presence of lacquer compounds in routine measurements (at least one MS/MS spectrum was measured in each sample). The threshold signals were suggested and set in order to reach a sufficient yield of diagnostic fragments for unambiguous identification of individual markers. These signals are intended to be used in long term measurement in practice.</p><div><p>Fragmentation of heptadecylcatechols with 0-3 double bonds (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#fig0003"><span>Fig. 3</span></a>a-d) is similar to that of pentadecylcatechols with same number of double bonds. In all cases, the signals of the characteristic fragments are well separated from the signals of the matrix.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Journal_of_Cultural_Heritage_77_2026_187_196_Fig_3_Fragmentation_spectra_of_heptadecylcatechols_possessing_0_3_double_bonds_6149330bc3.jpg" alt="Journal of Cultural Heritage, 77, 2026, 187-196: Fig. 3. Fragmentation spectra of heptadecylcatechols possessing 0-3 double bonds, (MS/MS; m/z of parent ions are: a) 342.2559, b) 344.2715, c) 346.2872, d) 348.3028)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Journal_of_Cultural_Heritage_77_2026_187_196_Fig_3_Fragmentation_spectra_of_heptadecylcatechols_possessing_0_3_double_bonds_6149330bc3.jpg 232w," sizes="100vw" width="3000" height="2017"></p><h5><strong>4.2. Principal component analysis</strong></h5><p>Excellent separation of particular types of Asian lacquers in Score Plot (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#fig0005"><span>Fig. 5</span></a>a-d) was obtained by Principal Component Analysis based on the benzenediol and phenol derivatives described above. The Score Plot contains a set of 20 samples obtained from the Náprstek Museum Prague as well as other samples (BBI, BBO, SBI, SBO, U, V and B) in which lacquer compounds were detected (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#tbl0002"><span>Table 2</span></a>). Note that in three other samples from The Náprstek Museum Prague, the lacquer compounds were not found at all.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Journal_of_Cultural_Heritage_77_2026_187_196_Fig_5_Score_plot_and_bi_plot_from_PCA_analysis_of_lacquers_taken_from_historic_objects_df82e0592a.jpg" alt="Journal of Cultural Heritage, 77, 2026, 187-196: Fig. 5. Score plot and bi-plot from PCA analysis of lacquers taken from historic objects, a. whole Score PCA plot, b. zoom of the T. succedaneum area, c. zoom of the T. vernicifluum area, d. zoom of the G. usitata area, e. whole PCA bi-plot, f. zoom of the T. succedaneum area in the PCA bi-plot, g. zoom of the T. vernicifluum area in the PCA bi-plot, h. zoom of the G. usitata area in the PCA bi-plot." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Journal_of_Cultural_Heritage_77_2026_187_196_Fig_5_Score_plot_and_bi_plot_from_PCA_analysis_of_lacquers_taken_from_historic_objects_df82e0592a.jpg 156w," sizes="100vw" width="3000" height="2994"></p><p>The significance of suggested markers for the studied lacquers across the whole data matrix was confirmed. The effect of particular markers is reflected in related bi-plots (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#fig0005"><span>Fig. 5</span></a>e-h). Qualitatively, the results are in accordance with the former study obtained by py-GC/MS [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S1296207425002572#bib0001"><span>1</span></a>]. Since both cation-radicals and protonated molecules are formed in ASAP source with significant yield of both ion forms, their sum is an input into the data matrix for each substance (e.g., for pentadecenyl catechol, where the input is the sum of intensities I<sub>(m/z</sub> <sub>=</sub> <sub>318)</sub>+ <i>I</i><sub>(m/z</sub> <sub>=</sub> <sub>319)</sub>), see PCA matrix in Supplementary material C. Measured m/z values of the analyzed compounds are in good agreement with the theoretical values calculated for specific elemental compositions (noted differences from the theoretical mass, dtm is in all cases less than or equal to 10 mDa).</p><h4><strong>5. Conclusion</strong></h4><p>The combination of atmospheric solids analysis probe with high resolution tandem mass spectrometry proved to be a fast and effective tool for analysis of historical Asian lacquer objects, their resolution and classification. The developed method is based on profiling of phenol and benezenediols derivatives. The fragmentation of alkylphenols and alkylbenzene diols after collision activated dissociation in Trap and Transfer collision cells was described. Scission of alkyl chains and elimination of water represent the main fragmentation processes important for identification. Cyclic ion mobility separation appeared to be a useful tool for “cleaning” of signals of the lacquer ions from the matrix signals allowing their better identification from the fragmentation spectra. Moreover, ASAP-MS and MS/MS allowed detection of diterpenic resins, triterpenic resins and arsenic sulphide pigments present along with Asian lacquers. Principal Component Analysis provided complete separation of samples into three clusters of Asian lacquers in Score Plot. A simple classification approach based on direct comparison of newly suggested classification parameters (CPs) allows reliable differentiation of lacquer samples according to their provenance. The developed method is now implemented in routine controls of lacquered objects and could be applied to the analysis of resins and ambers obtained from archaeological findings.</p></div></div>

Characterization of Asian lacquers by atmospheric solids analysis probe high resolution tandem mass spectrometry coupled with cyclic ion mobility separation

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 25th May 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 application note by<strong> Shimadzu, </strong>presentation by <strong>MDCW / University of Washington</strong> and poster by <strong>Waters Corporation!</strong></p><h3><strong>1. MDCW / University of Washington: Implementing Tile-Based Fisher Ratio Analysis of GC×GC-TOFMS Data to Obtain a Master Peak Table of All Detected Analyte Compounds in Many Petroleum-Based Samples</strong></h3><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/O_9_Halvorsen_136808e314.pdf"><strong>Full PDF for download</strong></a></li></ul><section><div><div><div><div><div><div><p>This presentation describes the development of a new chemometric workflow for processing <strong>GC×GC-TOFMS (comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry)</strong> data from petroleum-derived fuels. The work was conducted by researchers from the University of Washington in collaboration with Chevron Technical Center and focuses on creating a comprehensive <strong>Master Peak Table (MPT)</strong> containing all detectable analytes across multiple fuel sample classes. The motivation was that moving from conventional GC to GC×GC dramatically increased chromatographic peak capacity and resolution, but also created a need for more sophisticated data analysis methods capable of handling the much larger number of detected compounds.</p><p>The analytical platform employed <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/37"><strong>GC×GC-TOFMS</strong></a> with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/1289"><strong>thermal-flow modulator</strong></a> and a TOF mass spectrometer detector. Fuel samples were analyzed using an <strong>Rxi-1 column (30 m × 0.25 mm × 0.25 μm)</strong> in the first dimension and an <strong>Rxi-17MS column (2.0 m × 0.18 mm × 0.20 μm)</strong> in the second dimension. The sample set included multiple petroleum products such as hydrobates, reformates, naphthas, FCC gasoline, and blank samples. Log-scale chromatograms revealed numerous late-eluting trace compounds and significant compositional differences between fuel batches that were not readily visible in conventional chromatographic representations.</p><p>To process these highly complex datasets, the researchers implemented a <strong>tile-based Fisher Ratio (F-ratio) chemometric approach</strong> using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/348"><strong>ChromaTOF Tile software</strong></a>. The method divides GC×GC chromatograms into small tiles and identifies regions where analyte signals differ significantly between sample classes by comparing between-class and within-class variance. Instead of relying solely on F-ratio ranking, the workflow incorporates statistical testing against blank samples. Three blank chromatograms were used to establish tile-specific confidence intervals and p-test thresholds, allowing the system to determine whether detected signals represent genuine compounds rather than background noise. This strategy enabled the creation of a unified master peak table while minimizing problems caused by retention-time shifts and reducing the need for manual user intervention.</p><p>Application of the method generated <strong>719 statistically significant analyte hits</strong> across the fuel classes and demonstrated excellent reproducibility, with only <strong>6.3% of classifications showing inconsistent behavior among replicates</strong>. Detected compounds included hydrocarbons and aromatic species such as <strong>1-methylnaphthalene, 1,2,4-trimethylbenzene, β-vatirenene, 2-octene, and tetramethylheptadecane</strong>, whose occurrence patterns aligned well with expected fuel chemistry. The resulting master peak table contained both shared and sample-specific compounds and provided a much more comprehensive representation of petroleum composition than conventional workflows. The authors conclude that the approach should be broadly applicable to other complex sample types and could be extended using alternative chemometric metrics beyond Fisher Ratio analysis to address different experimental objectives.</p><h3><strong>2. Shimadzu: A Simple Method for Determination of β-Sitosterol as a Marker of Vegetable Oil Adulteration in Ghee by GC</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_06_sip_gc_042_en_f4c307005b.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>ShimadzuNexis GC-2030 can be effectivelyused for determination of adulteration of Ghee with vegetable oil.</li><li>The NexisGC-2030 easily meets the acceptancecriteria as per the proposed FSSAI method no.01.097:2022.</li><li>This method is suitable for routine food industry analysis and academic research.</li></ul><p>The most common milk product in Indian cuisine is ghee or clarified butter. Due to its high cost, ghee is adulterated with vegetable oil, to gain commercial benefits. β-sitosterol, a common phytosterol, found in a variety of natural sources, including vegetable fat or oil from plants (Figure 1). It is used as a marker of vegetable oil adulteration in ghee<sup>1</sup>.</p><p>The primary goal of this study is to assess the vegetable oil adulteration in ghee by analyzing β-Sitosterol as a marker using gas chromatography (GC). This will establish a foundation for the rapid detection of ghee adulteration. In this study, a simple, sensitive, and inexpensive method is developed for extraction of β-Sitosterol from ghee which is then subjected to gas chromatography with flame ionization detection for quantitation. The effects of several important parameters influencing the extraction efficiencies of β-Sitosterol including water-immiscible organic solvent (type and volume), volume of water, sonication time, surfactant (type and concentration), and organic modifier (type and volume) were investigated. This method is ideal for routine analysis in the food industry during the manufacturing, processing, and commercial testing of milk fat samples, or for academic research purposes.</p><h4><strong>&nbsp;Sample Preparation and Analysis Conditions</strong></h4><p>Standard and sample preparations were conducted following the guidelines outlined in the proposed FSSAI method No. 01.097:20222. The analysis was performed using a Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexis+GC-2030"><strong>Nexis GC-2030</strong></a> equipped with a Flame Ionization Detector (FID), as shown in Figure 2. The specific configuration and analytical conditions used during the study are provided in Table 1.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>A gas chromatography–based method using GC-2030 was developed for the estimation of β-Sitosterol in ghee. The method exhibits a detection limit of 2 %, enabling the identification of vegetable oil adulteration in ghee at levels as low as 2 %. At this adulteration level, the signal of β-Sitosterol achieved a signal-to-noise (S/N) greater than 3, confirming the reliability of detection at the established limit. This method provides a reliable and effective approach for the quantification of β-Sitosterol, which serves as a marker for vegetable oil adulteration in ghee.</p><h3><strong>3. Waters Corporation: Multidimensional Characterization of Short Chain Chlorinated Paraffins (SCCPs) with GC-APCI and Cyclic Ion Mobility</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009386_3232568115.pdf"><strong>Full PDF for download</strong></a></li></ul><p>This poster presents a multidimensional analytical approach for the characterization of <strong>short-chain chlorinated paraffins (SCCPs)</strong>, a class of persistent environmental pollutants included in the Stockholm Convention due to their environmental persistence and bioaccumulation potential. SCCPs are highly complex mixtures of chlorinated hydrocarbons containing thousands of possible congeners, making their analysis particularly challenging. The study evaluates the use of <strong>gas chromatography coupled with atmospheric pressure chemical ionization, cyclic ion mobility spectrometry, and high-resolution mass spectrometry (GC-APCI-IMS-HRMS)</strong> as a powerful platform for improved SCCP characterization.</p><p>The analytical instrumentation consisted of a modified <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890"><strong>Agilent 8890 gas chromatograph</strong></a> equipped with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=7&amp;search=Rxi-5SilMS"><strong>Rxi-5SilMS capillary column</strong></a><strong> (30 m × 0.25 mm × 0.25 μm)</strong> and connected to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/202"><strong>Waters SELECT SERIES Cyclic IMS</strong></a><strong> high-resolution mass spectrometer</strong> using an <strong>Atmospheric Pressure GC (APGC) ion source</strong>. Unlike conventional electron ionization methods, APCI was operated in negative-ion mode with a chloroform modifier, promoting the formation of characteristic <strong>[M+Cl]⁻ molecular ions</strong>. This significantly reduced fragmentation and provided strong molecular-ion signals, improving both qualitative identification and quantitative analysis of SCCP homologues.</p><p>Using three commercial SCCP technical mixtures (51.5%, 55%, and 63% chlorine content), the researchers demonstrated that GC-APCI-HRMS could selectively detect SCCP homologues according to carbon-chain length and degree of chlorination. Although substantial chromatographic overlap was observed among many homologues, the addition of <strong>ion mobility spectrometry (IMS)</strong> introduced a valuable extra separation dimension. Distinct drift-time versus m/z trendlines were observed for compounds sharing the same number of chlorine atoms, allowing homologues to be grouped and characterized more effectively than by chromatographic retention and mass spectrometry alone. The IMS data also enabled estimation of the relative abundance of individual homologue groups within each technical mixture.</p><p>The authors further explored the resolving power of the <strong>cyclic IMS device</strong> by employing multiple ion-mobility passes (up to eight cycles) to investigate individual SCCP congeners. While complete separation of individual congeners within a homologue group was not achieved, higher ion-mobility resolution revealed measurable differences between early- and late-eluting species and provided additional insight into compositional differences among SCCP mixtures. The study concludes that combining <strong>GC-APCI, cyclic ion mobility spectrometry, and high-resolution mass spectrometry</strong> offers a powerful multidimensional workflow for the characterization of complex chlorinated paraffin mixtures and may improve environmental monitoring and future regulatory analysis of these challenging contaminants.</p></div></div></div></div></div></div></section>

News from LabRulezGCMS Library - Week 22, 2026

News from LabRulezLCMS Library - Week 23, 2026

News from LabRulezLCMS Library - Week 24, 2026

News from LabRulezLCMS Library - Week 26, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 10th August 2026? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you posters by <strong>Agilent Technologies / ASMS, Thermo Fisher Scientific / ASMS </strong>and<strong> Waters Corporation / ASMS </strong>and application notes by<strong> Metrohm and Shimadzu!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Impurity Monitoring of GLP-1 Therapeutic Peptide RetatrutideUsing a 2D-LC/TOF System</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/glp_1_impurity_monitoring_2d_lc_tof_asms_2026_mp_388_agilent_eadce3f244.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Retatrutide is a next-generation triple agonist (GLP1/GIP/glucagon) and an emerging candidate among multivalent GLP1–based therapeutics. Its structural complexity and diverse impurity profile challenge conventional one-dimensional LC methods, which often lack sufficient resolving power to separate closely related impurities, sequence variants, and synthetic byproducts.&nbsp;</p><p>In this study, we demonstrate an Agilent multiple heart-cutting 2D-LC platform that enables rapid online solvent exchange and enhanced chromatographic selectivity, allowing targeted isolation of impurity peaks from a TFA-based first-dimension separation. When coupled with the Agilent 6230C Accurate Mass TOF LC/MS system, the workflow delivers fast, sensitive, and accurate mass profiling under MS-friendly second-dimension conditions, providing a robust solution for comprehensive impurity characterization of GLP-1 peptides such as Retatrutide.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumentation&nbsp;</strong></h5><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?instrumentationItems=39&amp;mainauthorItems=10&amp;search=1290+infinity+III+2D-LC"><strong>Agilent 1290 Infinity III 2D-LC system</strong></a><strong> comprised the following modules:&nbsp;</strong><ul><li>1290 Infinity III Bio Multisampler with Thermostat (G7137A)&nbsp;</li><li>1290 Infinity III Multicolumn Thermostat (G7116B)&nbsp;</li><li>1290 Infinity III Diode Array Detector (G7117B) with Max-Light cartridge cell (G7117-60020)&nbsp;</li><li>1260 Infinity III Bio Flexible Pump (G7131C)&nbsp;</li><li>1290 Infinity III Bio High-speed Pump (G7132A)&nbsp;</li><li>1290 Infinity Valve Drive (G1170A) with 2D-LC ASM Valve (G5643B)&nbsp;</li><li>Two 1290 Infinity III Valve Drives (G1170A) with multiple heart-cutting valves (G5642-64000) equipped with 40 µL Bio loops&nbsp;</li></ul></li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6230C"><strong>Agilent 6230C Accurate Mass TOF LC/MS System</strong></a></li></ul><h4><strong>Conclusions</strong></h4><p>Agilent 2D-LC with multiple heart-cutting effectively bridges TFA-driven chromatographic performance with FA-compatible MS detection, overcoming ion suppression limitations.&nbsp;</p><p>The integrated 2D-LC/Accurate Mass TOF workflow delivers confident impurity identification and robust characterization, supporting peptide analysis in both QA/QC and development environments.</p><h3><strong>2. Metrohm: Vinylene carbonate water determination via coulometric Karl Fischer titration</strong></h3><p><strong>Water determination in vinylene carbonate by Karl Fischer coulometric titration made simple with alcohol-free reagents</strong></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_k_076_download_8658665940.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Vinylene carbonate (vc) is commonly used as a battery electrolyte additive in lithium-ion batteries. Its popularity is due to the positive impact it has on anode cyclability and reduction of irreversible capacity. Small amounts of moisture in Li-ion batteries can significantly decrease performance and lifetime. Therefore, moisture levels in electrolyte solutions and their additives are controlled for use in manufacturing. Until recent years, accurate moisture quantification in vinylene carbonate samples was difficult due to side reactions. With the commercial development of alcohol-free coulometric Karl Fischer reagents, accurate determination is now much more accessible to end-users.</p><h4><strong>EXPERIMENTAL</strong></h4><p>This analysis was performed using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=220&amp;search=852+titrando"><strong>852 Titrando</strong></a> (2.852.0060) instrument, equipped with the electrodes listed in Table 1.</p><h4><strong>CONCLUSION&nbsp;</strong></h4><p>During battery manufacturing, control of all moisture present is important to guarantee adequate performance in the finished product. More easily quantifying the moisture contribution from additives such as vinylene carbonate makes this a much simpler task. The introduction of alcohol-free Karl Fischer reagents accomplishes this effectively, allowing the generation of accurate and repeatable moisture data—even for a difficult sample matrix.</p><h3><strong>3. Shimadzu: Non-Targeted Analysis of Metabolites in Alcoholic Beverages Using LabSolutions Insight Profiler</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_01241_en_57b43edb57.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>Using an LC-QTOFMS system with LabSolutions Insight Profiler non-targeted analysis software enables comprehensive comparative analysis of metabolites in food samples.&nbsp;</li><li>Principal component analysis and volcano plots can be used to detect characteristic features in each sample.&nbsp;</li><li>A variety of functions, including MS/MS spectral library searching, enable easy qualitative analysis of components.</li></ul><p>Metabolomics, a technique that analyzes metabolites in living organisms, is increasingly being applied in the food industry for product development and quality control. A particularly powerful approach is non-targeted metabolomics, which aims to analyze not only known metabolites but also unknown compounds without prior assumptions to reveal unexpected chemical differences between samples. Quadrupole time-of-flight mass spectrometry (QTOFMS), with its accurate-mass capability, is well suited for this purpose. However, the large volume of generated data creates challenges for feature identification and data comparison.&nbsp;</p><p>This article presents a case study in which LabSolutions Insight Profiler, a software platform for non-targeted analysis, was used to characterize compounds in beer and beer-like beverages. Peak detection, retention-time alignment, and library searching were performed across multiple datasets. Multivariate analysisrevealed compound profiles that likely reflect the differences in raw materials and manufacturing processes, demonstrating the utility of the approach for beverage characterization.</p><h4><strong>LabSolutions Insight Profiler&nbsp;</strong></h4><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LabSolutions+Insight+Profiler"><strong>LabSolutions Insight Profiler </strong></a>is software for batch processing of LC-QTOFMS data that enables non-targeted analysis through an intuitive workflow. It readily supports easy spectral feature detection, alignment, statistical processing, filtering, list screening, MS/MS spectra-based library searching, principal component analysis (PCA), displaying volcano or box plots, and more. Fig. 1 shows the data analysis workflow.</p><h4><strong>Analysis Conditions&nbsp;</strong></h4><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=nexera+X3"><strong>Nexera X3 UHPLC</strong></a> and<strong> </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=9030"><strong>LCMS-9030 systems</strong></a> were used as the analytical instruments. The LC method included in the LC/MS/MS Method Package for Primary Metabolites was used as the method. The data-dependent acquisition (DDA) mode was used to simultaneously acquire precursor m/z and MS/MS data. Table 2 shows the analysis conditions.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>In this study, compounds in various beer and beer-like beverages were analyzed by non-targeted analysis using an LCMS-9030 quadrupole time-of-flight mass spectrometer system. Analyzing compounds characteristic of each sample with LabSolutions Insight Profiler software confirmed that the resulting profiles reflected differences in raw materials and manufacturing methods.&nbsp;</p><p>LabSolutions Insight Profiler enables efficient non-targeted analysis by processing LC-QTOFMS data with an intuitive workflow. This workflow allows for objective evaluation of the taste, quality, and nutritional value of food products. Furthermore, this method is applicable not only to the analysis of compounds in beverages but also to non-targeted analysis of other types of samples.</p><h3><strong>4. Thermo Fisher Scientific / ASMS: High throughput targeted proteomic workflows with Adaptive Retention Time on the </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom MS</strong></a></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_004699_lsms_art_astral_zoom_proteomics_po004699_asms2026_na_en_78767efdc9.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Advances in MS instrumentation have accelerated the identification of biomarkers, but validating and translating these discoveries into assays for clinical use remains challenging and typically requires robust and accurate targeted approaches. While these often rely on predetermined reference target retention time (RT) windows, analytical column degradation or replacement, aging solvents, sample matrix effects, etc. can cause peptide RT shifts between injections and across longer-term analyses. To accommodate this, targeted MS experiments generally schedule wide target RT windows (&gt;1 min) or rely on heavy labeled peptides to trigger acquisition of endogenous peptides. Both greatly limit the number of quantifiable targets per assay. To overcome this, we utilize adaptive RT (aRT) alignment for live correction of RTs together with the speed and sensitivity of the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom MS</strong></a>. This allows reproducible tracking of &gt;2000 targets with narrow RT windows, high throughputs, such as 300 samples per day (SPD), and hybrid workflows combining targeting, of up to 1000 targets, and discovery.</p><h4><strong>Materials and methods&nbsp;</strong></h4><h5><strong>LC-MS Experiments&nbsp;</strong></h5><p>Experiments were performed using Thermo Scientific Pierce HeLa protein digest resuspended in 0.1% TFA, or individual or pooled human plasma samples. Peptides were separated using a 15 cm Thermo Scientific PepMap analytical columns (150 µm inner diameter) and the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Thermo Scientific Vanquish Neo UHPLC system</strong></a> at throughputs of 60 or 300 SPD. The liquid chromatography (LC) system was interfaced with the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom MS.</strong></a> Reference runs using MS1 and/or data-independent-acquisition (DIA) scans were acquired to obtain reference aRT spectra, and to determine target RTs. For aRT alignment, methods consisting of aRT MS1 and/or DIA scans, as well as targeted MS2 scans with RT correction were optimized. For hybrid DIA workflows, we used aRT MS1 scans for reference acquisition and alignment, combined with narrow window DIA and a targeted MS2 experiment. Observed RT shifts were caused by natural column degradation, sample matrix effects or when indicated induced by variation in gradient flow rate and buffer composition.&nbsp;</p><h5><strong>Data analysis&nbsp;</strong></h5><p>Reference DIA data was analyzed using Spectronaut. Targets lists were then generated from the search output by selecting varying number of targets evenly distributed across the RT dimension. Target RTs for smaller scale assays were manually validated and exported from Skyline, while target RTs for large scale assays were exported from Spectronaut. For alignment runs, DIA and PRM data were analyzed using Spectronaut and Skyline respectively.</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>Adaptive RT alignment on Orbitrap Astral Zoom MS shows robustness against various sources of RT shifts and has high target recovery even for thousands of targets&nbsp;</li><li>aRT enables the use of target acquisition windows &lt;15 s for robust targeting at high throughput&nbsp;</li><li>aRT Hybrid DIA allows targeting of up to 1000 targets with minimal cost to DIA depth</li></ul><h3><strong>5. Waters Corporation / ASMS: BOOSTING SENSITIVITY IN TOP-DOWN PROTEIN STUDIES USING CYCLIC IMS-ENABLED WIDEBAND ENHANCEMENT</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009471_51f2e8b546.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><p>The poster evaluates <strong>Wideband Enhancement (WBE)</strong> as a way to improve sensitivity in top-down protein mass spectrometry. In top-down workflows, intact proteins are fragmented directly, but the signal is distributed across multiple charge states, isotope envelopes, and numerous product ions, which can limit MS/MS sensitivity. WBE addresses this problem by synchronizing ion packets leaving the ion mobility region with the time-of-flight pusher, thereby increasing the number of ions that reach the detector within a selected <i>m/z</i> range.</p><p>Experiments were performed using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2434"><strong>Waters Cyclic IMS P20 Mass Spectrometer</strong></a> equipped with an <strong>electron capture dissociation cell</strong>. Samples were introduced by direct infusion in positive electrospray ionization mode. Two proteins were studied under denaturing conditions: bovine ubiquitin, approximately 8.5 kDa, and bovine carbonic anhydrase II, approximately 29 kDa. Single-pass and bypass ion mobility measurements were carried out with and without WBE, using both <strong>collision-induced dissociation (CID)</strong> and <strong>electron capture dissociation (ECD)</strong>. Data were acquired in <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/635"><strong>MassLynx</strong></a><strong> v4.2</strong> and processed using <strong>DriftScope</strong> and the <strong>waters_connect UNIFI peptide-mapping workflow</strong>.</p><p>For ubiquitin, WBE substantially increased the intensity of CID- and ECD-derived fragment ions. Improvements of up to tenfold were observed across the c- and z-ion series, while bypass ion mobility mode produced the largest overall sensitivity gain. The results indicate that WBE can enhance fragment detection while retaining the benefits of cyclic ion mobility separation and without sacrificing mass-spectral resolution.</p><p>The larger carbonic anhydrase II protein also showed marked improvements. CID fragment signals increased by up to tenfold for lower-<i>m/z</i> ions and about eightfold for higher-<i>m/z</i> fragments. Because ECD is generally less efficient than CID, the benefit of WBE was especially evident in ECD experiments: sequence coverage increased from <strong>54% without WBE to 70% with WBE</strong> in bypass mode. The authors conclude that combining WBE with complementary CID and ECD fragmentation on the Cyclic IMS P20 enables more sensitive and comprehensive top-down protein characterization.</p></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS Library - Week 33, 2026

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European Symposium on Analytical Spectrometry (ESAS) 2026

2026 AOAC INTERNATIONAL Annual Meeting & Exposition

Shimadzu at 2026 AOAC Annual Meeting & Exposition

ICP-MS for Hybrid Photoelectrode Characterization

Modern Methods for Faster Microbial Analysis

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