<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 20th 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 / HPLC Symposium </strong>and<strong> Waters Corporation / ASMS </strong>and technical note by<strong> KNAUER!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Comprehensive characterization of oligonucleotides and related impurities using advanced LC/Q-TOF analytical workflows</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_oligonucleotide_lc_q_tof_mp_536_asms_2026_en_agilent_b896ffee63.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Therapeutic oligonucleotides are synthetic, short nucleic acid sequences designed to modulate gene expression by targeting RNA or DNA with high sequence specificity. However, their inherent structural heterogeneity makes impurity profiling essential, as during GMP manufacturing, impurities like phosphorothioate to phosphodiester, 5′ and 3′ truncations or extensions, depurination, and abasic species can directly impact both product safety and efficacy. Antisense oligonucleotides (ASO) like Nusinersen (7127.171 g/mol) are indicated for the treatment of spinal muscular atrophy (SMA). Their closely related variants coelute with the main peak, complicating their characterization in conventional one-dimensional LC/MS workflows. To address this challenge, a 2D LC/MS strategy was implemented using the Agilent 1290 Infinity III Bio LC system with multiple heart cutting, coupled to the 6545XT AdvanceBio LC/Q-TOF and MassHunter BioConfirm software. The first-dimension separation uses an ion pairing buffer-based method to achieve higher chromatographic peak resolution, while the second dimension provides MS compatible desalting, enabling enhanced mass spectrometric sensitivity and improved detection of low-level impurities.&nbsp;</p><h4><strong>Instrumentation</strong></h4><p>1290 Infinity III Bio 2D-LC &amp; <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6545XT"><strong>6545XT Q-TOF</strong></a> includes:&nbsp;</p><ul><li>1290 Infinity III Bio Flexible Pump (G7131A)&nbsp;</li><li>1290 Infinity III Bio High-Speed Pump (G7132A)&nbsp;</li><li>1290 Infinity III Bio Multisampler (G7137A)&nbsp;</li><li>1290 Infinity III Multicolumn Thermostat (G7116B)&nbsp;</li><li>1290 Infinity III Variable Wavelength Detector (G7114B)&nbsp;</li><li>1290 Infinity III Diode Array Detector (G7117B)&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=2D-LC"><strong>2D-LC System</strong></a> with MHC set up</li></ul><h4><strong>Conclusions</strong></h4><ul><li>A 2D-LC/MS workflow enabled effective separation and identification of coeluting impurities.&nbsp;</li><li>HiRes sampling with multi-injection improved resolution and throughput while preserving 1D separation for MScompatible desalting.&nbsp;</li><li>6545XT AdvanceBio LC/Q-TOF delivered accurate mass and MS/MS data for low-abundance impurity detection.&nbsp;</li><li>MassHunter BioConfirm software enabled automated sequence confirmation and impurity identification.&nbsp;</li><li>This integrated platform offers a robust solution for oligonucleotide characterization in therapeutic development.</li></ul><h3><strong>2. KNAUER: Smart Monitoring &amp; Optimization Solutions for SMB Processes: In-Line and Off-Line Tools for SMB Systems</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/VTN_0048_knauer_in_line_and_off_line_tools_for_smb_systems_50a5f1c1cf.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In liquid chromatography, the purification of target compounds is classically carried out using single column batch chromatography. More efficient approaches include semi – continuous systems with two to three columns and continuous multicolumn systems. The most widely used of the latter is the simulated moving bed (SMB) chromatography which enables the continuous separation of binary or pseudo-binary mixtures. SMB purification is used in various areas such as petrochemical, pharmaceutical or food industry for the production of fine chemicals in different quantities and purities ranging from gram to tons per day. SMB systems vary significantly in size from small lab scale systems operating columns with 8 mm inner diameter (ID) to industrial systems operating columns of onemeter ID or larger.</p><p>Ideally, an SMB process is developed in a smaller lab scale system to reduce solvent and sample consumption compared to development at production scale. Once the separation parameters are established, the SMB process allows for accurate up scaling from lab to production scale. During method development but also production, different tools can be used to monitor and control the process which can be distinguished between in-line and off-line measures. The most crucial parameter, in addition to measuring the pressure, is monitoring the flow rates of the pumps, outlets and/or zones accurately with additional flowmeters. Normally, SMB systems are not equipped with detectors, but UV or RI detectors can be integrated to monitor process stability.&nbsp;</p><p>A standard off-line tool is used to analyse samples taken for one switch or cycle at the raffinate and extract outlets. The resulting chromatograms are used to check, if the separation is working. Further, samples can be taken during the process allowing the depiction of concentration profiles in the different zones. These tools will be described in more detail in the following sections.</p><h4><strong>MATERIAL AND METHODS</strong></h4><ul><li><strong>AZURA Lab SMB system</strong>: SMB, biocompatible, 30 ml/min zone1, 4 ml/min feed, 10 – 130 bar&nbsp;</li><li><strong>AZURA Lab SMB system: </strong>SMB, stainless steel, 30 ml/min zone1, 4 ml/min feed, 10 – 130 bar&nbsp;</li><li><strong>AZURA Pilot SMB system, standard: </strong>SMB, stainless steel, 250 ml/min zone1, 40 ml/min feed, 2 – 100 bar&nbsp;</li><li><strong>AZURA Pilot SMB system, high flow:</strong> SMB, stainless steel, 400 ml/min zone1, 100 ml/min feed, 2 – 60 bar</li><li><strong>Refractive index detector:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2429"><strong>AZURA® RID2.1L HighFlow detector</strong></a> 100 ml/min&nbsp;</li><li><strong>UV detector: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2428"><strong>AZURA®UVD 2.1S detector</strong></a>, w/o flow cell</li><li><strong>UV detector: </strong>AZURA®UVD2.1S UV detector, fiber optics w/o flow cell</li></ul><h4><strong>CONCLUSION&nbsp;</strong></h4><p>SMB is a continuous separation process that can run for several hours or days without interruption. Therefore, it is important to monitor the process and to be able to adapt to changes during the run. Different tools are available that can be used for process monitoring and method development. These tools can be divided into two main categories: in-line and off-line tools. In-line tools monitor parameters such as pressure and flow rate directly during the run, whereas off-line tools take a sample, which is then analyzed by an HPLC system. The tools described can be added to the KNAUER SMB systems depending on the customer’s needs. The more parameters that are measured, the better the process can be monitored. This is especially helpful during SMB method development.</p><h3><strong>3. Shimadzu / ASMS: Accelerating drug screening in forensic hair analysis by applying high-speed polarity switching in HR 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/TP_180_Accelerating_drug_screening_in_forensic_hair_analysis_by_applying_high_speed_polarity_switching_in_HR_LC_MSMS_168f8cc0b2.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In 2023, the Society of Hair Testing (SoHT) published updated consensus guidelines for the forensic analysis of drugs of abuse in hair, defining recommended targets across eight major drug classes: opiates, cocaine, amphetamines, cannabinoids, opioids, methadone, buprenorphine, and ketamine. Legal drivers, accepted use cases, and degree of prescription differ between US and Europe but in both jurisdictions, mass spectrometry is widely applied to support legally defensible conclusions. The challenge for any drug testing in hair samples, whether it is in forensic and safeguarding contexts, workplace testing or a judicial setting is the need to develop methods capable of detecting expanded search panels with the increased prevalence of new psychoactive substances (NPS) and non-medical prescription drug use. The approach applied in this work considered a LC/QTOF analysis using DDAMS/MS with rapid polarity switching with a novel data processing application, Insight Profiler. The software was designed to support a single click approach to automate data processing of complex data sets in non-targeted analysis from feature detection to compound identification.</p><h4><strong>Materials and Methods</strong></h4><h5><strong>Reversed phase LC Separation: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+X2"><strong>Nexera X2&nbsp;</strong></a></h5><ul><li>Shim-pack Velox Biphenyl (100 x 2.1 mm, 2.7 µm) column; column temp. 40 ºC, flow rate: 0.3 mL/min, 17 min total analysis time. Methanol:water gradient with 2 mM ammonium formate and 0.002% formic acid&nbsp;</li></ul><h5><strong>High resolution QTOF analysis: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-9050"><strong>LCMS-9050&nbsp;</strong></a></h5><ul><li>MS scan m/z 100-1000, 100 msec scan time. Polarity switching time 800 msec.&nbsp;</li><li>MS/MS DDA: 4 scans in positive ion mode (m/z 40-1000, 33 msec), 2 scans in negative ion mode (m/z 40-1050, 33 msec) CE 5-55V (1.998 sec total cycle time).</li></ul><h5><strong>Data processing</strong></h5><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Insight+Profiler"><strong>Insight Profiler</strong></a>, feature detection threshold set to low, compound identification search lists included NIST, HighResNPS, Shimadzu Forensic Toxicology database.</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>The targeted DDA-MS/MS polarity switching approach successfully identified a significant number of unknown compounds in the samples not routinely targeted by triple quadrupole analysis.&nbsp;</li><li>The method using DDA-MS/MS was easily configured to support an expanded DoA target panel to meet the needs of forensic toxicology screening.&nbsp;</li><li>Non-targeted analysis using Insight Profiler accelerated data analysis by aligning identified compounds from the same hair donor showing direction of change for pharmaceutical and illicit compounds detected.</li></ul><h3><strong>4. Thermo Fisher Scientific / HPLC Symposium: Enhancing semi-volatile analyte detection in HPLC-CAD using temperature coupling mode for optimized evaporation control</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_004766_hplc_vanquish_cad_fatty_acid_quantification_po004766_na_en_4a0868c2cb.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Polysorbates are widely used in biopharmaceutical formulations but can degrade or contain FAs impurities that must be accurately measured to ensure product quality and safety. Charged Aerosol Detection is commonly used for FA analysis, though its performance depends strongly on EvapT. Higher EvapT improves S/N ratios but can reduce sensitivity for semi-volatile compounds like FAs, while lower EvapT has the opposite effect. The <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2176"><strong>Thermo Scientific Vanquish Charged Aerosol Detector P</strong></a> series introduces a Temperature Coupling Mode that links EvapT with the charging detection module (CDM) temperature, overcoming limitations of earlier systems with fixed CDM temperature of 40 ºC. This coupling improves response and measurement reliability for semi-volatile species, enabling better optimization of FA analysis<sup>1</sup>.</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>Advanced temperature control in CAD improved method sensitivity up to ~47% for semi-volatile fatty acids.&nbsp;</li><li>The best overall S/N was achieved at 25.0 °C EvapT with Temperature Coupling Mode enabled.&nbsp;</li><li>The optimized CAD approach supports more sensitive FA impurities and degradants quantification in pharmaceutical and biopharmaceutical formulations.</li></ul><h3><strong>5. Waters Corporation / ASMS: High mass and spatial resolution MS imaging of soft fruit sample cross-sections using desorption electrospray ionization (DESI)</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009492_282619e388.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><p>This poster demonstrates the use of <strong>desorption electrospray ionization mass spectrometry imaging (DESI MSI)</strong> for visualizing the spatial distribution of metabolites in high-water-content soft fruits, specifically strawberries and raspberries. The authors developed a simple direct-transfer workflow to overcome the challenges associated with imaging delicate fruit tissues and compared three transfer substrates: plain glass microscope slides, nitrocellulose membranes, and Hamamatsu Poropare plates. The goal was to determine which surface best preserves metabolite localization while enabling high-quality mass spectrometry imaging.</p><p>Fresh fruit cross-sections were transferred to each substrate by direct contact for 10 seconds before analysis using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=5&amp;search=DESI+XS"><strong>Waters DESI XS ion source</strong></a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2433"><strong>Waters Xevo™ MRT P10 high-resolution mass spectrometer</strong> </a>operating in negative electrospray ionization mode. MS imaging was performed with a <strong>50 µm pixel size</strong>, using a <strong>95:5 methanol/water</strong> spray solvent, while sucrose (m/z 341.1089) served as the lock mass for accurate mass calibration. High mass resolution enabled tentative assignment of metabolites such as citric acid, asparagine, malic acid, glutamic acid, palmitic acid, stearic acid, and sucrose.</p><p>The comparison of transfer substrates revealed significant differences in metabolite localization and image quality. Glass slides produced the strongest metabolite signals but also exhibited considerable metabolite delocalization during sample transfer, reducing spatial accuracy. Nitrocellulose membranes transferred a broader range of metabolites and provided complementary chemical information, although they also showed greater analyte spreading and suffered physical damage after a single DESI acquisition. In contrast, <strong>Poropare plates</strong> minimized metabolite delocalization and preserved fine structural details within the fruit cross-sections, despite producing somewhat lower signal intensities than glass slides.</p><p>The study concludes that direct transfer combined with DESI MSI is an effective approach for imaging soft fruit tissues that are otherwise difficult to analyze because of their high water content. Among the evaluated substrates, <strong>Hamamatsu Poropare plates</strong> provided the best balance between spatial resolution and preservation of metabolite localization, making them particularly suitable for high-resolution metabolomic imaging, while high mass accuracy facilitated confident tentative metabolite identification.</p></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS 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>

News from LabRulezLCMS Library - Week 31, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 3rd 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, Shimadzu / ASMS, Thermo Fisher Scientific / HPLC Symposium </strong>and<strong> Waters Corporation / ASMS </strong>and application note by<strong> Metrohm!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Ultra-Trace Quantification of N-Nitroso-desmethyl-sumatriptan with Interference Resolution Using LC–TQ</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/1290_infinity_iii_uhplc_6495d_lc_tq_desmethyl_sumatriptan_asms_2026_mp_667_agilent_ebb0888227.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Sumatriptan succinate, an antimigraine drug contains nitrosylating functional groups and is susceptible to forming its own nitrosamine drug substance-related impurity (NDSRI), specifically N-nitroso-desmethylsumatriptan. As a Category 1 genotoxic impurity, its specification limit is established at 0.0428 ppm with respect to the API. In this study, samples and standards were prepared in methanol:water (1:1, v/v). The LC/TQ method was developed with a target limit of detection (LOD) at least 20-fold lower than the specification limit to ensure adequate sensitivity. Analytical data were collected in replicate for a 10 mg/mL API sample, as well as LOQ- and specification-level spiked samples, to evaluate recovery, relative standard deviation (RSD), linearity, and repeatability.</p><h4><strong>Experimental</strong></h4><ul><li><strong>LC System: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+Infinity+III+UHPLC"><strong>1290 Infinity III UHPLC</strong></a></li><li><strong>MS:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6495D"><strong>6495D LC/TQ</strong></a></li><li><strong>Column:</strong> <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Poroshell+120+EC+C18"><strong>Poroshell 120 EC C18</strong></a>, 3x150mmx2.7µm, 40 Deg C</li></ul><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>A sensitive and robust method has been developed for N-nitroso-desmethyl Sumatriptan in Sumatriptan.&nbsp;</li><li>Method LOQ is 10% lower than specification level, RSD of &lt;5%, and linearity across 0.00214 to 0.1 ppm.&nbsp;</li><li>The recovery of NDSRI in Sumatriptan at LOQ level and specification level are 95%.</li></ul><h3><strong>2. Metrohm: Moisture analysis of rebaudioside M by Karl Fischer titration</strong></h3><p><strong>Simplified rebaudioside M moisture determination via volumetric Karl Fischer titration paired with an oven system</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_075_download_59f185c238.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Natural sweeteners like stevia and its derivatives are an increasingly important part of the global sweetener market as more consumers substitute sugar with healthier alternatives. Stevia’s derivatives are significantly sweeter than table sugar. These compounds are estimated to be 50 to 300 times sweeter in comparison. This sweet taste coupled with the fact that the human body cannot metabolize steviol glycosides (i.e., they contribute zero calories to one’s diet), makes them a very attractive sugar replacement.&nbsp;</p><p>The moisture content of stevia materials is a crucial factor when discussing their shelf life and stability. Measuring the moisture content of a stevia derivative, rebaudioside M, using an oven system coupled with volumetric Karl Fischer (KF) titration provided a repeatable approach for quantifying the moisture content of this material.</p><h4><strong>Experimental</strong></h4><p>The analysis was carried out with a Double Pt ring electrode for volumetry (6.00346.100). Testing was executed on the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=220&amp;search=874+Oven+Sample+Processor"><strong>874 Oven Sample Processor</strong></a> (2.874.0120) coupled with 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). Approximately 0.2 g of sample was weighed into an 874 Oven Sample Processor 6 mL vial and placed onto the rack. The oven was set to a temperature of 100 °C, and the evaporated moisture was carried to the volumetric titration vessel by nitrogen gas flow at 70 mL/min. The moisture from the sample was titrated with Hydranal Comp 5 reagent.</p><h4><strong>Conclusion</strong></h4><p>Natural low-calorie sweeteners like stevia derivatives are growing in popularity as people choose healthier alternatives to sugar. Working to develop standardized, specific methodology can help support sweetener industry development, effective quality assessment, and the evaluation of rebaudioside M and other steviol glycosides’ stability.&nbsp;</p><p>This Application Note provides a foundation for the analysis of stevia powder by Karl Fischer titration. An oven system paired with volumetric Karl Fischer analysis provides an accurate, repeatable method to evaluate stevia powder and its derivatives. This method’s compatibility with the 874 Oven Sample Processor allows increased sample throughput through automation, providing operators even more time to complete other important tasks in parallel.</p><h3><strong>3. Shimadzu / ASMS: Quantitative analysis of 6 beta blockers on an LCMS-8045RX</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/WP_131_Quantitative_analysis_of_6_beta_blockers_on_an_LCMS_8045_RX_f596f609f4.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Beta-adrenergic blocking agents, commonly known as beta blockers, competitively inhibit the binding of catecholamines such as epinephrine and norepinephrine to β-adrenergic receptors, thereby reducing heart rate and blood pressure. These drugs are widely prescribed for the treatment of hypertension, angina and heart failure<sup>1</sup> . However, beta blockers may also be misused by athletes resulting in their inclusion on the World Anti-Doping Agency (WADA) prohibited list<sup>2</sup> . Owing to both their therapeutic importance and potential misuse, sensitive and selective analytical methods are required for reliable detection and quantification. Liquid chromatography tandem mass spectrometry (LC-MS/MS) offers high sensitivity and specificity for such analyses.</p><h4><strong>Method</strong></h4><p>Nadolol, metoprolol, propranolol, atenolol &amp; carvedilol were purchased from Sigma Aldrich and Thermo Fisher Scientific. Standards were prepared in 1 mg/mL in LCMS grade methanol. <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+40"><strong>Nexera 40-series HPLC system</strong></a> connected to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-8045RX"><strong>LCMS-8045RX</strong></a> was used for data acquisition. The mixture of standards was further diluted in LCMS grade methanol (Sigma Aldrich) and Sigmatrix urine diluent to create the standards for the calibration curves. A Shim-pack Velox Biphenyl column was used for the chromatographic separation. All analytes were ionized with electrospray ionization (ESI) in positive ion mode.</p><h4><strong>Conclusion&nbsp;</strong></h4><ul><li>Superior sensitivity in complex matrices: Limit of Detection (at accuracy ±20% and S/N &gt; 3) of 0.010 ng/mL for all the analytes evaluated in this study.</li><li>Excellent linearity and accuracy: Linear responses (with R2 &gt; 0.99) observed across the evaluated concentration range, and consistent accuracy within ±20% for all 17 calibrants included in this study.&nbsp;</li><li>Optimized throughput: Automated interface and MRM optimization via LabSolutions Connect MRM ensured maximum signal-to-noise determination for this study, while the high-organic flush at the end of each run, maintained column integrity</li></ul><h3><strong>4. Thermo Fisher Scientific / HPLC Symposium: A switchable 2D-LC platform in PAT: routine UV monitoring or MS-based characterization of mAb PQAs directly from the bioreactor</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_004764_hplc_vanquish_2dlc_mabs_analysis_bioreactor_samples_po004764_na_en_7a99c1b683.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Monitoring quality attributes throughout the upstream processing of mAbs is critical due to potential effects of biological variability on product safety and efficacy. Thus, there is a growing need for streamlined analytical workflows that provide timely and reliable insights to enable fast and informed process decisions.</p><h4><strong>Materials and methods</strong></h4><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/743"><strong>Thermo Scientific Vanquish Flex Simple</strong></a> Switch 2D-LC system for loop heart-cutting consisting of Quaternary Pump F (VF-P20-A), Binary Pump F (VF-P10-A-01), Dual Split Sampler FT (VF-A40-A-02), 2x Column Compartment H (VH-C10-A-03), and Diode Array Detector FG (VF-D11-A-01)&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1490"><strong>Thermo Scientific Orbitrap Exploris MX Mass Detector</strong></a> (BRE725536) with BioPharma option (BRE725539)&nbsp;</li><li>Thermo Scientific MAbPac Protein A column, 12 µm, 4 x 35 mm (PN 082539)&nbsp;</li><li>Thermo Scientific ProPac 3R SCX, 2 x 50 mm, 3 µm (PN 43103-052068)&nbsp;</li><li>Thermo Scientific MAbPac SEC-1, 5 µm, 4 x 300 mm (PN 074696)</li></ul><h4><strong>Data analysis&nbsp;</strong></h4><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/76"><strong>Thermo Scientific Chromeleon 7.3.2 Chromatography Data System (CDS) </strong></a>and <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1837"><strong>Thermo Scientific BioPharma Finder 5.2 software</strong></a></p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>Switchable 2D-LC-UV/MS offers a streamlined approach for at-line monitoring of mAb titer, charge and size variants directly from the bioreactor in &lt;1h.&nbsp;</li><li>UV monitoring provides quick and simple trendlines, while HRAM-MS allows deep characterization at intact level.&nbsp;</li><li>Near real-time information supports in-time process decisions to protect yield and product quality.</li></ul><h3><strong>5. Waters Corporation / ASMS: SOFTWARE TOOLS FOR AUTOMATED LC/MS ANALYSIS OF CRITICAL QUALITY ATTRIBUTES OF mRNA MOLECULES</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009414_52de0bb71a.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><p>This poster presents an automated LC-MS workflow for evaluating three critical quality attributes (CQAs) of mRNA therapeutics: <strong>5′-capping efficiency, Poly(A) tail length and heterogeneity, and mRNA sequence integrity</strong>. A custom firefly luciferase (Fluc) mRNA construct containing a Cap-1 structure, 1,919 nucleotides, and a Poly(A) tail was used as the model sample. Importantly, all three CQAs were assessed using a <strong>single LC-MS assay</strong>, supported by specialized waters_connect software tools designed to streamline nucleic acid characterization from sequence entry through final data processing.</p><p>The analytical platform consisted of a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>Waters ACQUITY Premier Binary UPLC System</strong></a><strong> with TUV detector coupled to a </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1148"><strong>Xevo MRT Q-Tof Mass Spectrometer</strong></a>, which uses multi-reflectron time-of-flight technology. Separations were performed on an ACQUITY Premier OST 1.7 µm, 300 Å, 2.1 × 150 mm column, while data-independent acquisition was carried out in MSE mode. Data processing used the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1544"><strong>waters_connect</strong></a><strong> Informatics Platform together with SYNTHETIC Library 2.0, MAP Sequence 2.0, and INTACT Mass 1.9</strong> applications. For sequence mapping, the mRNA was independently digested using four endonucleases—RNase T1, RapiZyme MC1, RapiZyme Cusativin, and human RNase4—providing complementary cleavage patterns.</p><p>The workflow produced detailed information on both capping and Poly(A) tail characteristics. The Fluc mRNA showed <strong>100% capping efficiency</strong>, with 62.7% carrying an m7GpppAm Cap-1 structure and 37.3% an m7GpppGm Cap-1 structure; no uncapped digestion product or Cap-related impurities were detected. Poly(A) tail analysis identified ten major species ranging from <strong>98-mer to 107-mer</strong>, resulting in an average Poly(A) tail length of <strong>102.3 nucleotides</strong>. The Xevo MRT Q-Tof provided high-resolution measurements—approximately 100,000 resolution in the examples shown—and very good mass accuracy for the detected Poly(A) species.</p><p>For sequence integrity, combining the four complementary enzymatic digestions achieved <strong>93.7% unambiguous mRNA sequence coverage</strong>, demonstrating the value of a multi-enzyme approach for comprehensive sequence confirmation. MAP Sequence 2.0 also automatically distinguished structural isomers using elevated-energy fragment-ion information, helping resolve isobaric and isomeric digestion products with less manual interpretation. Overall, the poster demonstrates that high-resolution MSE acquisition on the <strong>Xevo MRT Q-Tof combined with automated waters_connect informatics</strong> can provide an integrated and efficient approach for comprehensive characterization of key mRNA quality attributes.</p></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS Library - Week 32, 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

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

News from LabRulezLCMS Library - Week 34, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 14th September 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>and posters by <strong>Shimadzu / AOAC </strong>and<strong> Thermo Fisher Scientific / Metabolomics!</strong></p><h3><strong>1. Agilent Technologies: Improved Analysis of Intact Proteins and Peptides by Reversed Phase HPLC Using the Altura Ultra Inert PLRP-S 1000 Å Column</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/an_altura_ultrainert_column_HPLC_analysis_5994_9322en_agilent_2b3a542647.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Intact protein analysis by reversed-phase HPLC (RP-LC) plays a vital role in quality control for determining the purity of biotherapeutic proteins and improving the identification and quantification of critical quality attributes (CQAs). When coupled to mass spectrometric detection, it allows several things. First, an accurate molecular weight to be determined; second, the identification of variants containing post‑translational modifications (PTMs) and proteoforms; and third, the antibody-to-drug ratio in the case of antibody drug conjugates (ADCs).<sup>1</sup>&nbsp;</p><p>While many RP columns have a silica-based stationary phase to enable broader functionalization, residual acidic silanol groups can interact with basic residues in peptides, proteins, and other biomolecules, resulting in significant peak tailing and loss of chromatographic performance. Polystyrene/divinyl benzene (PS/DVB)-based stationary phases do not contain unintentional adsorption sites. Additionally, larger pore sizes have demonstrated superior chromatographic efficiency through less diffusion restriction into the pore volume and reduction of size exclusion mechanisms, degrading the RP-based selectivity.<sup>2</sup>&nbsp;</p><p>Wide-pore columns like the PLRP-S 1000Å provide an exceptional performance with biomolecules, particularly when combined with MS-compatible mobile phase conditions such as formic acid.&nbsp;</p><p>Even so, some undesirable interactions may be observed when using stainless-steel column hardware. Molecules that possess multiple negative charges (including oligonucleotides, phosphorylated peptides and proteins, and proteins with low isoelectric point in general) may interact with exposed metal ions in stainless-steel column hardware. This can result in the need to "deactivate" new columns by making multiple injections of sample until reproducible results are obtained.&nbsp;</p><p>This application note demonstrates how the new <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=10&amp;search=Altura+Ultra+Inert"><strong>Altura Ultra Inert </strong></a>PLRP-S 1000 Å column serves as an effective high-performance workhorse in the analysis of large, intact biomolecules. Developed to effectively block nonspecific adsorption during separations, Ultra Inert technology reduced passivation time 15-fold and delivered ~ 10% greater recovery for mAbs and ADCs and up to 100% for smaller biomolecules like GLP-1s and small globular proteins.</p><h4><strong>Experimental</strong></h4><h5><strong>Instrumentation&nbsp;</strong></h5><ul><li>Agilent 1290 Multicolumn thermostat (G7116B)&nbsp;</li><li>Agilent 1290 Bio multisampler (G7137A)&nbsp;</li><li>Agilent 1290 Bio high-speed pump (G7132A)&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=10&amp;search=6530"><strong>Agilent 6530 Q-TOF MS system</strong></a>&nbsp;</li></ul><h5><strong>Software and data processing&nbsp;</strong></h5><ul><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=10&amp;search=MassHunter+Workstation"><strong>Agilent MassHunter Workstation, version 10.1&nbsp;</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=10&amp;search=MassHunter+Qualitative+Analysis"><strong>Agilent MassHunter Qualitative Analysis software, version&nbsp;B.07&nbsp;</strong></a></li><li>Agilent DAR calculator, version B01.01</li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>Intact mass analysis is a critical methodology to determine the purity of biotherapeutics, but due to the chemical complexity of these analytes, nonspecific adsorption from both silica stationary phase and metal column housing can be highly deleterious to separation performance. The Agilent Altura PLRP-S 1000 Å provides a highly robust solution combining the chemical inertness of polystyrene/divinyl benzene stationary phase with the ultra‑inert Altura hardware to dramatically reduce deleterious peak tailing and increase recovery for biotherapeutics. Herein, we see that analyte recovery for both mAbs, ADCs, GLP-1s, and globular proteins are improved versus stainless-steel, while the Altura PLRP-S column is capable of monitoring both quality critical PTMs such as loss of drug payload as well as accurate quantification of ADC DAR.</p><h3><strong>2. Shimadzu / AOAC: Ambient Ionization Mass Spectrometric Detection of Aroma Released During Gummy Chewing</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/aoac_2026_47_2_34c41f762f.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In recent years, there has been growing interest in evaluating flavor using analytical instrumentation, and retronasal aroma during eating is important. In this study, we proposed an analytical method for measuring retronasal aroma during eating using a single quadrupole mass spectrometer (<a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=1&amp;search=2050"><strong>LCMS-2050</strong></a>) equipped with an ambient ion source (Dark Current Discharge Ionization : DCDI) without pretreatment.</p><h4><strong>Conclusion</strong></h4><p>We developed a simple method for evaluating retronasal aroma using a single quadrupole mass spectrometer with an ambient ionization source. Ambient ionization mass spectrometry (DCDI LCMS-2050) can rapidly measure retronasal aroma during eating. Time-resolved visualization reveals texture-dependent differences in aroma release dynamics among grape-flavored gummies. It is also expected to lead to the visualization of the marriage between food and alcohol. This approach may facilitate objective evaluation of flavor release during consumption and support product formulation and sensory science.</p><h3><strong>3. Thermo Fisher Scientific / Metabolomics: Orbitrap Tribrid Real-Time similarity searching of mzCloud library for guided unknown characterization of tea metabolites</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/po_004849_lsms_rtls_tribrid_apex_small_molecule_metabolomics_po004849_na_en_d0d3156065.pdf"><strong>Full PDF for download</strong></a></li></ul><p>In metabolomics LC-MS data is processed to generate a list of detected compounds with a level of confidence in the identity of each compound based on reference data. This reference data may be spectral data and/or retention time information stored in a library or in silico information generated based on fragmentation rules. These annotated compounds are then used to evaluate biological changes between normal and disease states. One of the major hurdles between collected data and coming to reliable conclusions about the biology is the limited number of standards available to build these libraries. It is common to have hundreds to thousands of compounds detected in a data set that have no library match because there is no commercial standard for that unknown. Instead, there is just an elemental formula and matches from a structure database. These structures can be compared using in silico fragmentation techniques to determine which isomers plausibly match the data. MSn data can help reduce the list of possible matches, but without guidance, ddMS3 may not consistently collect data on the most relevant MS2 fragments to accomplish this.&nbsp;</p><p>In this work we use Real-Time Library Search (RTLS) in a ddMS3 method to help guide the instrument in real time to collect the most relevant data for confirming structural matches.</p><h4><strong>Materials and methods</strong></h4><h5><strong>Test method(s)&nbsp;</strong></h5><p>1 μL aliquots were analyzed using a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/products?category=48&amp;manufacturerItems=3&amp;search=gold"><strong>Thermo Scientific Hypersil GOLD column</strong></a> on a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/744"><strong>Thermo Scientific Vanquish Horizon UHPLC</strong></a><strong> </strong>coupled with a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/561"><strong>Thermo Scientific Orbitrap IQ-X Tribrid mass spectrometer</strong></a> and <strong>Thermo Scientific Orbitrap Tribrid Apex Small Molecule mass spectrometer</strong>. RTLS was run in similarity mode using the offline version of <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1764"><strong>Thermo Scientific mzCloud library</strong></a>.&nbsp;</p><h5><strong>Data analysis&nbsp;</strong></h5><p>Data was processed using <strong>Thermo Scientific Freestyle and </strong><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1759"><strong>Compound Discoverer software</strong></a><strong>.</strong></p><h4><strong>Conclusions&nbsp;</strong></h4><p>Tea extracts were analyzed using RTLS to find the most similar compound in the offline version of the mzCloud library and trigger MS3 on the highest m/z matching and non-matching fragments. This provided additional information to confirm similarity and provide insight on shared sub-structures to the library compound as well as additional information on the portions of the structure that were unique to the experimental compound.</p><h3><strong>4. Waters Corporation: The Quantification of Glucagon-like Peptide Receptor Agonists (GLP-1 RAs) in Plasma Extracts Using Capillary UHPLC-MS/MS</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/720009537_en_0068921516.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><h5><strong>Benefits&nbsp;</strong></h5><ul><li>10-fold improvement in sensitivity&nbsp;</li><li>Robust methodology for &gt;500 injections&nbsp;</li><li>Reduced solvent usage&nbsp;</li><li>No need for complex nanospray MS source</li></ul><p>Obesity represents, perhaps, the largest healthcare challenge, affecting approximately 1.3 billion people globally, contributing to a diverse range of chronic diseases e.g., metabolic, cardiovascular, muscular skeletal, and multiple cancers.1 The rapid growth of obesity and associated global healthcare costs means there is a critical need for safe effective treatments.2 GLP-1 RA initially developed for type 2 diabetes have shown clinical efficacy as weight loss medicines.2 These drugs mimic the action of gut hormones which regulate energy metabolism and appetite by interacting with the hypothalamus, brain stem etc., resulting in weight loss. The success of these GLP-1 RAs is associated with their on-target efficacy and long duration of action,3 e.g., half-life of semaglutide t½ = 160–180 hours3 cf. 1–2 minutes for human GLP-1.4 The long half-life of these GLP-1 RAs results in low, sub ng/mL plasma levels 48–72 hours after dosing, which requires a high sensitivity bioanalytical assay to accurately quantify the plasma concentrations5 and define the PK elimination phase.&nbsp;</p><p>Tandem quadrupole electrospray ionization (ESI) mass spectrometry, operated in multiple reaction monitoring (MRM) mode, coupled with 2.1 mm ID ultra-high performance liquid chromatography (UHPLC) is the dominant technology platform for quantitative bioanalysis. As next generation GIP/GLP-1 RAs promise to be more potent, resulting in lower dosing levels and plasma levels, there is a need for more sensitive analytical methodologies to support drug metabolism and pharmacokinetics (DMPK) studies. Capillary/nano LC-MS/MS have been extensively employed in proteomics to increase analytical sensitivity and enable small volume analysis.5 This sensitivity increase is derived from a combination of the superior ionization efficiency at low flow rates and analyte concentration due to the smaller column geometry.6 This application note illustrates the use of capillary (300 µm) UHPLC-MS/MS (MRM) to affect 10-fold improvement in GLP-1-RAs peak response in human plasma extracts, and detection limits as low as 20 pg/mL for tirzepatide.</p><h4><strong>Experimental</strong></h4><p>Capillary chromatography was performed on an <strong>ACQUITY™ M-class Chromatography System</strong> connected to a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/195"><strong>Xevo™ TQ-XS Mass Spectrometer</strong></a> (Waters Corporation, Wilmslow, UK) equipped with a microflow probe. Capillary UHPLC separations were performed on an <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1952"><strong>ACQUITY Premier Peptide CSH C18</strong></a>, 300 Å, 1.7 µm, 300 µm x 50 mm Chromatography Column.</p><p>MS analysis was performed at unit mass resolution using positive ESI at a capillary voltage of 3.0 kV, with a cone voltage of 32 V. The cone gas flow, desolvation gas flow, and desolvation gas temperature were 50 L/h, 300 L/h and 600 °C, respectively. The data were analyzed using <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1544"><strong>waters_connect™ Software</strong></a><strong>,</strong> and MRM transitions used to monitored for the MS/MS detection of liraglutide, exenatide, semaglutide and tirzepatide were as follows: liraglutide 938.7 → 1128.4, exenatide 838 → 396, semaglutide 1029.2 → 1238.1, and tirzepatide 1204.2 → 396.2. Data analysis was performed using <strong>MS Quan Software.</strong></p><h4><strong>Conclusion</strong></h4><p>Bioanalysis plays a critical role in the drug discovery and development processes providing data to support DMPK, safety assessment, pharmacokinetics/pharmacodynamics (PK/PD), and clinical development studies. The development of new, more potent medicines, innovating delivery platforms, micro sampling, and new approach methodologies (e.g., organ on a chip) all require greater levels of analytical sensitivity. Capillary scale UHPLCMS/MS offers the potential to improve bioanalytical detection limits up to 10-fold, without the need for long analysis times and complex operation associated with nano spray LC-MS/MS. Here, the application of capillary (300 µm ID) scale chromatography for the detection of GLP-1 RAs in human plasma extracts at levels as low as 20 pg/mL with robustness over 500 injections was demonstrated.</p></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS Library - Week 38, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 21st September 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>KNAUER </strong>and<strong> Shimadzu, </strong>technical note by <strong>Thermo Fisher Scientific </strong>and poster by <strong>Waters Corporation / SOFT!</strong></p><h3><strong>1. KNAUER: Precise Catechin Profiling in Various Types of Tea</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/VFD_0198_knauer_precise_catechin_profiling_in_various_types_of_tea_d607cde5ba.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Fresh tea leaves contain high concentrations of catechins, which have many beneficial properties. These include antioxidant, anti-inflammatory as well as antimicrobial effects, and it is even claimed that they have the potential to prevent cancer [1]. In addition, the taste and mouthfeel of a tea strongly depend on its catechin profile. The catechin content of tea leaves varies based on cultivation area, age and variety, as well as on how they are fermented, processed and packed. Therefore, the catechin content is an important marker for the quality of tea.&nbsp;</p><p>The analysis of catechins can be challenging. The structural similarity of the catechin isomers and other closely related compounds result in similar behavior and a difficult separation (Fig. 1). Catechins possess many phenolic hydroxyl groups, which are prone to secondary interactions, like hydrogen bonding. Classical as well as highly endcapped C18 columns offer only limited retention and selectivity for catechins. Therefore, the KNAUER column portfolio has been expanded to include a pentafluorophenyl (PFP)-modified stationary phase (<strong>Eurospher II 100-3 PFP column </strong>50 x 2 mm). It offers optimal separation of the catechins based on hydrophilic, hydrophobic and π-π-interactions. The column withstands acidic eluents (pH 1.5–10) as well as 100 % aqueous conditions, which are beneficial for the retention of hydrophilic compounds. The KNAUER Gradient Prediction Tool assisted with the challenging method development which is described in detail in the TechNote “The Gradient Prediction Tool: Method Development for the Separation of Catechins from Tea”. Here, the application of the optimized method for the identification and quantification of catechins in tea extracts is shown. The seven compounds specified in ISO-14502-2 (2005), as well as two additional catechins known as (+)-gallocatechin and (–)-gallocatechin gallate, were quantified.</p><h4><strong>MATERIAL AND METHODS</strong></h4><ul><li><strong>Pump: </strong><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/2374"><strong>P8.1L</strong></a>; high pressure gradient&nbsp;</li><li><strong>Liquid Handler:</strong> <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1454"><strong>LH 8.1L </strong></a>With FastWash station, and Robotic cooler. Loop: 20 µl.</li><li><strong>Thermostat: </strong><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/2376"><strong>CT 2.1L&nbsp;</strong></a></li><li><strong>Detector:</strong> <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/2424"><strong>DAD 6.1L&nbsp;</strong></a></li><li><strong>Flow cell: </strong>Analytical LightGuide flow cell (50 mm, 6 µl)&nbsp;</li><li><strong>Software:</strong> ClarityChrom 10.1</li></ul><h4><strong>CONCLUSION&nbsp;</strong></h4><p>The application note demonstrates the reliable separation and quantification of catechins and caffeine in tea extracts using the new KNAUER PFP column. Using an optimised gradient predicted with the KNAUER Gradient Prediction Tool, nine tea-related compounds were separated in under 23 minutes. The tested tea samples showed different catechin content highlighting how strongly tea composition depends on the product type and processing.</p><h3><strong>2. Shimadzu: New Derivatization Method for Quantitative Analysis of Δ⁹-THC-COOH in Urine</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/an_01_01215_en_c98174629b.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>The risk of limited availability of stable isotope-labeled standards can be avoided by synthesizing internal standards through derivatization.&nbsp;</li><li>The derivatizing agent IPPAH and its corresponding stable isotope IPPAH-d6 can be synthesized easily and inexpensively from acetone (or acetone-d6).&nbsp;</li><li>This approach achieves sufficient sensitivity and quantitative accuracy for the determination of Δ⁹-THC-COOH in urine.</li></ul><p>In Japan, the Cannabis Control Act and the Narcotics and Psychotropics Control Act were amended in December 2024. While cannabis was legalized for industrial and medical uses, stricter cannabis regulations have been enacted to prevent harm from its abuse. The primary psychoactive cannabinoid, delta-9-tetrahydrocannabinol (Δ⁹-THC), is extensively metabolized in the body and is excreted mainly in urine and feces as 11-nor-9-carboxy-THC (Δ⁹-THC-COOH) and its glucuronide conjugates. Consequently, Δ⁹-THC-COOH must be analyzed to confirm cannabis use. For LC-MS/MS quantitation, the stable isotope-labeled internal standard Δ⁹-THC-COOH-d3 is commonly used to correct for matrix effects. However, most suppliers of stable isotope standards are located in the U.S., making these standards difficult to obtain due to import procedures. Furthermore, there may be additional importrelated supply risks for stable isotope standards in the future.&nbsp;</p><p>This Application News describes a technique for quantitating Δ⁹-THC-COOH using an internal standard that is synthesized easily and inexpensively by derivatization with IPPAH (1- isopropylpiperidine carboxylic acid hydrazide), which characteristically reacts with carboxyl groups, and its corresponding stable isotope IPPAH-d6.</p><h4><strong>Analysis Conditions&nbsp;</strong></h4><p>LC-MS/MS analysis conditions are shown in Table 1. The <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=1&amp;search=Nexera+XR"><strong>Nexera XR</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=1&amp;search=LCMS-8050"><strong>LCMS-8050 systems</strong></a> were used.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>Derivatization with IPPAH and its stable isotope analog, IPPAHd6, enabled the simple and inexpensive preparation of an internal standard. This approach provides sufficient sensitivity and accuracy for the determination of Δ⁹-THC-COOH in urine. Most stable isotope-labeled standards are supplied by foreign manufacturers, creating a risk of delays or difficulties in procurement due to import/export regulations. By synthesizing the internal standard through derivatization, this risk can be minimized.</p><h3><strong>3. Thermo Fisher Scientific: High-throughput quantitative proteomics with Evosep Eno and the Orbitrap Astral Zoom Mass Spectrometer</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/tn_004544_ov_astralzoom_evosepeno_htp_proteomics_tn004544_na_en_f31db9084e.pdf"><strong>Full PDF for download</strong></a></li></ul><p>High-throughput proteomics is a critical enabling technology for large clinical studies, high-content drug screening, and systems biology research, allowing for comprehensive and quantitative analysis of complex proteomes across large sample cohorts within practical timeframes. As biological and translational studies expand in scale and complexity, the ability to generate deep and reproducible proteome measurements across thousands of samples has become increasingly essential for robust biomarker discovery, network-level systems modeling, and downstream analyses. In these contexts, accurate and precise protein quantitation must be maintained without sacrificing throughput, placing stringent demands on the performance and robustness of both LC instruments and mass spectrometers.&nbsp;</p><p>To meet these increasing analytical demands, the Evosep Eno was developed as a high‑throughput LC system that combines robustness, ease of use, and highly reproducible chromatography. It offers six standardized methods: 30, 60, 100, 200, 300, and 500 samples per day (SPD), allowing users to select the throughput that aligns best with their study goals.1 These predefined methods ensure consistent gradient delivery, highly stable retention times, and reproducible system performance across instruments and laboratories.2 By reducing LC‑related variability and simplifying everyday operation, the Evosep Eno offers a strong and consistent foundation for large‑scale proteomics workflows, particularly those relying on short gradients and high reproducibility required for downstream quantitative analysis.</p><h4><strong>Experiment</strong></h4><h5><strong>Instrumentation&nbsp;</strong></h5><ul><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=291&amp;search=evosep+eno"><strong>Evosep Eno&nbsp;</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1959"><strong>Orbitrap Astral Zoom Mass Spectrometer&nbsp;</strong></a></li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/2464"><strong>Thermo Scientific™ EASY-Spray™ Ion Source&nbsp;</strong></a></li><li>Evosep™ Pod for EASY-Spray Ion Source</li></ul><h5><strong>Software&nbsp;</strong></h5><ul><li>Biognosys Spectronaut® 19.7 software&nbsp;</li><li>MacCoss Lab Software Skyline-Daily V25.1</li></ul><h4><strong>Summary&nbsp;</strong></h4><h5><strong>Seamless and easy integration for high-throughput proteomics&nbsp;</strong></h5><p>Evosep Eno integrates seamlessly with the Orbitrap Astral Zoom Mass Spectrometer, supported by EASY-Spray source-compatible columns, emitters, and the Evosep Pod column oven for a simple, streamlined, high-throughput workflow.&nbsp;</p><h5><strong>Deep proteome coverage at 500 SPD&nbsp;</strong></h5><p>Optimized MS parameters for the standard 500 SPD Evosep Eno gradient enabled identification of more than 6,500 protein groups and 71,000 modified peptides from three replicates of 200 ng Pierce HeLa Digest/PRTC Standard.</p><h5><strong>Reproducible quantitation across standard gradients&nbsp;</strong></h5><p>Across all standard Evosep Eno gradients, the workflow delivered highly reproducible label-free quantification, with median protein group %CVs at or below 5.2%, while identifying more than 10,500 protein groups and 190,000 modified peptides from five replicates of 200 ng Pierce HeLa Digest/PRTC Standard at 30 SPD.&nbsp;</p><h5><strong>Robust chromatography at ultra-high throughput&nbsp;</strong></h5><p>Chromatographic performance remained stable and robust at 500 SPD, with nearly 100 consecutive runs showing PRTC retention time standard deviations below 0.4 seconds and a median of 6 DPPP.&nbsp;</p><h5><strong>Strong linearity for confident quantitation&nbsp;</strong></h5><p>Quantitative performance remained strong at 500 SPD, with PRTC peptides showing excellent linearity across the active gradient (R² &gt;0.98) when spiked from attomolar to femtomolar concentrations.</p><h3><strong>4. Waters Corporation / SOFT: COMPARATIVE EVALUATION OF HIGH RESOLUTION MASS SPECTROMETRY ACQUISITION STRATEGIES FOR THE DETECTION AND ANALYSIS OF ILLICIT DRUG SUBSTANCES</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/720009592_0bd2b5ee6a.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><p>The poster compares two high-resolution time-of-flight mass spectrometry acquisition strategies for toxicology screening: targeted <strong>Tof-MRM</strong> and data-independent <strong>Tof-MSE</strong>, both implemented on a Waters <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1148"><strong>Xevo MRT MS</strong></a> coupled to an <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/199"><strong>ACQUITY UPLC I-Class FTN PLUS System</strong></a>. The aim was to determine whether these approaches could meet routine service requirements for drug testing while also broadening the number of substances that can be detected beyond conventional targeted panels. Urine samples were prepared across a wide concentration range for 20 target analytes, and the methods were also applied to 20 anonymized authentic urine samples.</p><p>Both workflows used a 15-minute LC separation on an <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1952"><strong>ACQUITY HSS C18 column</strong></a> under positive electrospray ionization. In the targeted Tof-MRM mode, selected precursor ions were isolated and fragmented, with quantifier and qualifier ions monitored for sensitive quantitative analysis. In contrast, Tof-MSE operated in a data-independent mode, alternating between low and elevated collision energies to collect accurate-mass precursor and fragment-ion information for a broad range of compounds. Data were processed in the waters_connect platform using MS Quan for Tof-MRM and UNIFI with the Waters Toxicology Library, containing more than 2,100 drugs and metabolites, for Tof-MSE.</p><p>The targeted Tof-MRM method provided the highest sensitivity, with limits of detection ranging from <strong>0.05 to 0.5 ng/mL</strong> in fortified urine. The broader Tof-MSE workflow achieved LODs of approximately <strong>0.5 to 5 ng/mL</strong>. When both strategies were applied to authentic urine samples, they showed excellent qualitative agreement. Importantly, Tof-MSE detected additional compounds outside the predefined target panel, including commonly encountered medications, benzodiazepines, antidepressants, and illicit drug substances that would not have been captured by the targeted method alone.</p><p>Overall, the study shows that Tof-MRM can deliver sensitivity comparable to conventional tandem-quadrupole LC-MS/MS for targeted urinary drug analysis, while Tof-MSE adds broader sample characterization and retrospective screening capability. Used together, the two acquisition strategies provide a flexible approach that combines sensitive quantification of predefined analytes with expanded screening for unexpected or previously untargeted drug substances in complex biological samples.</p></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS Library - Week 39, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 29th September 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 technical note by <strong>KNAUER,</strong> application note by <strong>Shimadzu </strong>and posters by<strong> Thermo Fisher Scientific / HPLC Symposium </strong>and <strong>Waters Corporation / AOAC!</strong></p><h3><strong>1. KNAUER: Efficient separation of di(2-ethylhexyl) phthalate (DEHP) from oil matrices using GPC</strong></h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/VTN_00_XX_knauer_applichrom_gpc_f1d7f1a236.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Phthalates are chemical compounds primarily used as plasticizers in polymers to enhance the flexibility and elasticity of materials such as polyvinyl chloride (PVC) [1]. Since plasticizers are not covalently bound to the polymer chains, they have the potential to leach into the contacting media and contribute to contamination [2]. With the widespread and increasing use of plastic materials, the risk of phthalate release and human exposure continues to rise. As a result, and due to their potentially harmful effects on human health, phthalates have attracted growing scientific and regulatory attention in recent years [1]. Oil-rich food products can leach lipophilic phthalates from their packaging [3]. Throughout the production and packaging process, polymeric components such as tubing, containers, and caps may serve as potential sources of contamination. For the analysis of phthalates in such oil matrices, sample cleanup is an essential step. Gel permeation chromatography (GPC), based on sizeexclusion principles, is widely applied as an effective cleanup technique prior to subsequent analytical determination.</p><h4><strong>MATERIALS &amp; METHODS</strong></h4><p>The samples were dissolved in the eluent mixture and filtered through a 0.45 µm PTFE filter prior to analysis. For both olive oil and canola oil, an additional sample spiked with DEHP was prepared and likewise filtered before analysis. Chromatographic analysis was performed using an isocratic method with an eluent composition of ethyl acetate/heptane (50:50 v/v) at a flow rate of 1.0 mL/min. Detection was carried out by UV absorbance at 254 nm. The injection volume was 8 µL using a full-loop injection mode. The column temperature was maintained at 25°C. Separation was achieved on an <strong>AppliChrom® OleoSep column </strong>(10 µm, 300 × 8 mm). The <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1630"><strong>AZURA® Semi Preparative GPC System</strong></a> was used.</p><h4><strong>CONCLUSION</strong></h4><p>GPC sample preparation is an effective approach for separating phthalates from high-molecular-weight matrices such as edible oils. In this study, the successful separation of di(2-ethylhexyl) phthalate (DEHP) from three different oil samples was demonstrated. Based on these results, it can be assumed that other phthalates with lower molecular weights (&lt; 390 Da) can also be effectively separated under same conditions. The KNAUER AZURA® GPC semi preparative system (Fig. 4) in combination with the AppliChrom® OleoSep GPC column provides a robust and efficient setup for sample preparation in phthalate analysis, offering rapid separation, high resolution, and minimal solvent consumption due to the short analysis time.</p><h3><strong>2. Shimadzu: Analysis of Chloride and Sulfate Ions in Bioethanol Using the </strong><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=1&amp;search=Nexera+IC"><strong>Nexera IC Ion Chromatograph</strong></a></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/an_01_01211_en_55cbf3e64f.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>Analysis of chloride and sulfate ions in fuel ethanol can be conducted in accordance with ASTM D7319-221) .</li><li>Accurate quantitative determination, exhibiting excellent linearity and repeatability, can be achieved at concentration levels significantly below the limits specified by the ASTM criteria.</li></ul><p>First-generation bioethanol produced from raw materials such as corn and sugarcane has been utilized to achieve carbon neutrality. However, research and development for second-generation bioethanol produced from non-food, cellulose-based raw materials is also underway to avoid competition with food crops. In Japan, eight companies, including Toyota Motor Corporation, have formed the “Research Association of Biomass Innovation for Next Generation Automobile Fuels” (raBit) to advance research on next-generation bioethanol technologies. Shimadzu participates as a supporting member and promotes research and development through analytical technology cooperation.</p><p>&nbsp;It is known that the presence of chloride and sulfate ions in fuel ethanol can form engine residue, leading to reduced engine performance. ASTM D4806-252) specifies fuel ethanol quality as criterion of chloride ion must not exceed 6.7 mg/kg and that of sulfate ion must not exceed 4 mg/kg. ASTM D7319-22 includes test methods for chloride and sulfate ions in fuel ethanol using ion chromatography.&nbsp;</p><p>In this application, we present an example of the analysis of chloride and sulfate ions in bioethanol using the <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=1&amp;search=Nexera+IC"><strong>Nexera IC</strong></a> in accordance with ASTM D7319-22.</p><h4><strong>Conclusion</strong></h4><p>Chloride and sulfate ions in bioethanol were determined using a Nexera IC system in accordance with ASTM D7319-22. The method offers high sensitivity, linearity, and repeatability, enabling reliable quantification at concentrations well below ASTM-specified limits, thus supporting effective quality control and regulatory compliance of fuel ethanol.</p><h3><strong>3. Thermo Fisher Scientific / HPLC Symposium: LC-MS analysis of intact and subunit-level mAb enabled by a novel monodisperse supermacroporous reversed-phase platform</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/po_004763_ccs_surepac_protein_reverse_phase_mabs_separation_po004763_na_en_56199ec50d.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Monoclonal antibodies (mAbs) are structurally complex biotherapeutics that require multi-level analytical characterization to ensure product quality, safety, and efficacy. LC-MS analysis is routinely applied at the intact protein and subunit levels to assess molecular mass, heterogeneity, and structural integrity. Enzymatic subunit generation, such as IdeS digestion, enables targeted domain-level characterization while reducing analytical complexity compared to full peptide mapping. Achieving high-performance reversed-phase separations across intact and subunit-level workflows remains challenging, as chromatographic columns optimized for intact proteins often compromise performance of smaller subunits. Consequently, multiple columns are required to support comprehensive mAb characterization.&nbsp;</p><p>In this study, we evaluate a reversed-phase separation column based on a novel 2.5 μm monodisperse supermacroporous (SMP) polymeric stationary phase for unified LC-MS analysis of monoclonal antibodies under intact, reduced, and IdeSdigested conditions. The SMP resin’s uniform particle size and highly accessible pore structure enable efficient separation of both small and large analytes, including intact mAbs, reduced subunits (LC and HC), and IdeS-generated fragments such as scFc and F(ab′)₂. Using the SurePac Protein RP MDi column, baseline separation of these species was achieved within a 10- minute gradient, providing a fast, all-in-one LC-MS approach for mAb variant characterization.</p><h4><strong>Materials and methods</strong></h4><h5><strong>Instruments&nbsp;</strong></h5><p><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/744"><strong>Thermo Scientific Vanquish Horizon UHPLC system</strong></a>; <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/401"><strong>Thermo Scientific Orbitrap Exploris 480 mass spectrometer</strong></a> with <strong>Thermo Scientific OptaMax NG ion source</strong>.&nbsp;</p><h5><strong>Data analysis&nbsp;</strong></h5><p>The UHPLC system with mass spectrometer were operated with <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1758"><strong>Thermo Scientific Xcalibur 4.7 software</strong></a>. Full MS spectra of intact mAbs and mAb fragments were analyzed using Thermo Scientific Freestyle 1.8 and BioPharma Finder 5.4 software that utilizes the ReSpect and Xtract algorithms for molecular mass determination.</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>A SurePac Protein RP column enabled a rapid (10 min) separation of mAb LC, HC, scFc, and F(ab′)₂ fragments, with major proteoforms identified by mass agreement.&nbsp;</li><li>The SurePac Protein RP column supports comprehensive intact and subunit-level mAb characterization in a single workflow, with strong separation performance across mAb fragments.</li></ul><h3><strong>4. Waters Corporation / AOAC: IMPROVED PURIFICATION OUTCOMES FOR PROBLEMATIC COMPOUNDS USING AN INERT COLUMN WITH POLAR SORBENT</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/720009616_AOAC_f65ea1b771.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><p>Whether the goal is to obtain enough intermediate for the next step in a synthetic scheme, to polish a final product, or to create a suitable standard for compound identification, preparative liquid chromatography remains a primary technique for isolating compounds from complex mixtures. Recovering the target compound at the desired purity and yield in the least amount of time is of utmost importance.&nbsp;</p><p>Polar targets that do not retain, or “sticky” compounds that seemingly disappear on the column are two groups that many consider to be ’problematic’ in purification. “Sticky” compounds, also known as non-specific adsorbers (NSAs), are metal-sensitive targets what can adsorb to positively charged metal surfaces in the LC system flow path and column, making them difficult to detect and collect effectively. Although other methods, such as column pre-conditioning, can be implemented for isolating compounds known to be interactive, this option can be time-consuming and lead to sample loss and excessive solvent waste.&nbsp;</p><p>Although lab scale purifications in which tens to hundreds of milligrams of target compound are isolated from crude mixtures are still performed routinely, the trend toward smaller scale purification is becoming more prevalent. Laboratories are increasingly opting to isolate only a few milligrams of target compound for preliminary studies. Successful target candidates are then isolated in greater amounts to satisfy ensuing experiments. Whether the objective is to isolate a small amount of target compound for exploratory studies, or to purify greater amounts for their use as reference standards, a column which can resolve eluting impurities efficiently is required.&nbsp;</p><p>Echinacea is an herbaceous flowering plant in the daisy family<sup>1,2</sup> and is one of the most important medical herbs widely used to treat the common cold and other infectious diseases.<sup>3</sup> One of the most abundant compounds in echinacea is chicoric acid (Figure 1), a phenylpropanoid and caffeic acid derivative.<sup>4,5</sup> In this scale-up study, chicoric acid, a suspected “sticky” target polar compound was isolated from a complex echinacea tea extract using two inert XSelect HSS T3 MaxPeak Premier OBD Columns with different particle sizes and dimensions (3.5 μm 10 x 100 mm and 5 μm 10 x 150 mm). The MaxPeak Premier OBD preparative HPLC columns are considered ’inert’ because they are enabled with Waters High Performance Surface (HPS) Technology. The chicoric acid isolated using the 3.5 μm column was of equivalent UV purity to the product isolated using the 5 μm column, with a 34% savings in run time. Smaller particle preparative isolations using columns with inert hardware are a practical option for those laboratories where reduced amounts of target are needed for projects conducted on accelerated timelines.</p><h4><strong>METHODS</strong></h4><ul><li><strong>Analytical Columns and flow rate:</strong> ACQUITY Premier HSS T3 and <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1952"><strong>ACQUITY UPLC HSS T3 Columns</strong></a>; 1.8 μm, 2.1x50 mm; 0.35 mL/min&nbsp;</li><li><strong>Prep Columns and flow rate:</strong> XSelect HSS T3 OBD Prep Column and XSelect Premier HSS T3 OBD Prep (custom) Columns, 5 μm, 10x150 mm; XSelect Premier HSS T3 OBD Prep Column, 3.5 μm, 10x100 mm; 5.4 mL/min</li></ul><h5><strong>Instrumentation&nbsp;</strong></h5><ul><li><strong>Analytical:</strong> <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/198"><strong>ACQUITY UPLC H-Class System</strong></a>; Quaternary Solvent Manager, Sample Manager FTN-H, Column Manager, TUV Detector, <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1543"><strong>ACQUITY QDa Detector&nbsp;</strong></a></li><li><strong>Prep:</strong> Waters AutoPurification System; 2545 Binary Gradient Module, 2767 Sample Manager, System Fluidics Organizer, 2998 Photodiode Array Detector</li></ul><h4><strong>CONCLUSIONS&nbsp;</strong></h4><ul><li>Chicoric acid was analyzed and isolated using analytical and preparative MaxPeak Premier HSS T3 Columns with inert surfaces, which increased the peak area and height for improved detection and collection.&nbsp;</li><li>Chicoric acid was successfully isolated using 3.5 and 5 μm XSelect Premier HSS T3 OBD Prep Columns and fraction pool analysis showed equivalent UV purity, which suggests the viability of incorporating small particle preparative chromatography into the purification workflow.&nbsp;</li><li>3.5 μm preparative columns improve purification process efficiency and promote sustainability by reducing method run time, solvent usage, and fraction lyophilization time.&nbsp;</li><li>Inert MaxPeak Premier column hardware, OBD Technology, and small particle preparative columns are well-suited for the demands of the purification laboratory when results must be generated efficiently to satisfy accelerated production timelines</li></ul></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS Library - Week 40, 2026

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 5th October 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>Metrohm </strong>and posters by <strong>Shimadzu / ASMS, Thermo Fisher Scientific / Metabolomics </strong>and <strong>Waters Corporation / ASMS!</strong></p><h3><strong>1. Metrohm: Carbonate in lithium carbonate by potentiometric titration</strong></h3><p><strong>Determination of carbonate in lithium carbonate by potentiometric titration according to draft standard ISO 10662</strong></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/an_t_251_download_c1c530d784.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Lithium carbonate is one of the main lithium salts in cathode materials used for lithium-ion batteries. Accurate carbonate and overall purity determination in this raw material are essential because even trace impurities can affect key physicochemical properties, ultimately influencing electrochemical behavior in downstream applications. This is especially significant in battery-grade materials, where strict compositional tolerances are required to ensure consistent manufacturing performance, long-term cell stability, and overall safety. This Application Note describes carbonate content determination in lithium carbonate on an automated OMNIS system with Dis-Cover lids. The ISO 10662 draft method quantifies the main content of lithium carbonate to enable a precise assessment of material purity.</p><h4><strong>EXPERIMENTAL</strong></h4><p>The analysis is carried out on an <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=220&amp;search=OMNIS+Titrator"><strong>OMNIS Advanced Titrator</strong> </a>with an <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=220&amp;search=OMNIS+Sample+Robot"><strong>OMNIS Sample Robot</strong></a> equipped with a dUnitrode and Dis-Cover lids (Figure 1). A blank analysis is performed with a start volume of hydrochloric acid and titrated until after the equivalence point. Samples are titrated with hydrochloric acid until after the second equivalence point.</p><h4><strong>CONCLUSION</strong></h4><p>The OMNIS Titrator and OMNIS Sample Robot with Dis-Cover lids provide a fast and reliable determination of carbonate in lithium carbonate according to draft standard ISO 10662. The OMNIS system can be expanded to other titration applications as required.</p><h3><strong>2. Shimadzu / ASMS: Comprehensive Untargeted Metabolomic Analysis from Five Stages of Blueberry Development by High Resolution Accurate Mass Spectrometry</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/MP_459_Comprehensive_Untargeted_Metabolomic_Analysis_from_Five_Stages_of_Blueberry_Development_by_High_Resolution_Accurate_Mass_Spectrometry_bc0aadf181.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Metabolomic studies of blueberry cultivars and growth stages have been conducted to identify optimal cultivation conditions maximizing antioxidant production. Many of these studies utilize reversed phase (RP) chromatography and target fragmentation data collection at the most abundant chemical species as observed by electrospray ionization mass spectrometry (ESI MS). However, this strategy may miss important metabolites suppressed by matrix effects or unfavorable ionization. A comprehensive untargeted metabolomic study was performed to determine how diverse chromatographic separation and multiple fragmentation strategies could impact the identification of additional metabolites. The expanded metabolomics data was used to assess differences across fruit developmental stages and determine if unique metabolomic populations could be identified between stages.</p><h4><strong>Methods</strong></h4><p>All samples were analyzed in triplicate and in a randomized order using a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=1&amp;search=nexera+hplc"><strong>Nexera HPLC</strong></a> and a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=1&amp;search=9050"><strong>Shimadzu LCMS-9050 Q-TOF</strong></a>. To maximize feature identification across the blueberry developmental stages, both RP and hydrophilic interaction liquid chromatography (HILIC) were used. Mass spectrometry data was collected with ESI in positive and negative mode using data-independent analysis (DIA) and data-dependent analysis (DDA), generating 8 different analytical methods in total.</p><h4><strong>Conclusions</strong></h4><p>The Shimadzu LCMS-9050 provided a comprehensive analysis of plant extracts when complementary chromatographic and MS analysis modes were utilized. All five growth stages showed distinct metabolimic populations. Overall differentiation of groups is captured by any of the analytical methods employed, but the same approach can be used to get a more holistic approach to metabolome coverage. If reduced analysis time is preferred, a combination of HILIC DDA and RP DDA methods characterize most metabolites.</p><h3><strong>3. Thermo Fisher Scientific / Metabolomics: Pushing the limits of structural lipidomics: enhanced sensitivity and MS³-driven annotation on Orbitrap Tribrid Apex Small Molecule MS</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/po_004763_ccs_surepac_protein_reverse_phase_mabs_separation_po004763_na_en_56199ec50d.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Advances in lipidomic analysis require mass spectrometry deliver high sensitivity, rapid acquisition, and efficient parallel use of multiple mass analyzers. Orbitrap Tribrid Apex Small Molecule MS was evaluated to meet these demands through improved sensitivity, faster polarity switching, and enhanced parallelization between the Orbitrap analyzer and linear ion trap analyzer. High-resolution MS enables effective resolution of isobaric lipid species, while alternative fragmentation strategies with rapid MSⁿ, supports confident lipid identification and structural annotation of lipid classes. The parallel operation of the Orbitrap analyzer and linear ion trap analyzer minimizes duty-cycle limitations while maximizing data density and throughput. Leveraging these instrument enhancements, robust lipidomics workflows were demonstrated through method evaluation with lipid reference materials and application to complex biological samples from plants.</p><h4><strong>Materials and methods</strong></h4><p><strong>Instrumentation and methods: </strong>A <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1988"><strong>Thermo Scientific Accucore C30 HPLC Column</strong></a> (150 mm x 2.1 mm, 2.6 µm particle size) connected to a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/744"><strong>Thermo Scientific Vanquish Horizon UHPLC System</strong></a> and a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=3&amp;search=Orbitrap+Tribrid+Apex"><strong>Orbitrap Tribrid Apex Small Molecule MS</strong></a> were used to acquire the data.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>We have successfully demonstrated the utility of the Orbitrap Tribrid Apex Small Molecule MS for structural lipidomics, using various fragmentation strategies on an LC timescale. We applied this to study lipid extracts from a plant and annotated around 1700 high grade lipids.</p><h3><strong>4. Waters Corporation / ASMS: Tandem Quadrupole DESI Imaging To Visualize Spatial Distribution of Gefitinib and Related Metabolites in Rat Liver</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/720009433_4e913e0193.pdf"><strong>Full PDF for download</strong></a></li></ul><div><div><section><div><div><div><div><div><div><p><span>This poster presents a targeted DESI-MS/MS imaging workflow for visualizing the spatial distribution of gefitinib and its metabolites in rat liver after a single therapeutic subcutaneous dose. The study addresses a common limitation in drug-distribution studies: spatial localization is often assessed using radiolabeled compounds, which may not be available during early drug discovery. DESI offers a label-free ambient ionization approach with minimal sample preparation, enabling direct mapping of drugs and metabolites in tissue.</span></p><p><span>Male Wistar rats received gefitinib at 10 mg/kg, while plasma, urine, and liver samples were collected over a 24-hour period. Plasma and urine were analyzed by LC-MS/MS for pharmacokinetics and metabolite identification, whereas fresh-frozen liver sections were analyzed by targeted DESI MRM imaging on a </span><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/2100"><span><strong>Xevo TQ-Absolute XR tandem quadrupole mass spectrometer</strong></span></a><span>. Liver sections were cryosectioned to 10 µm thickness and analyzed using DESI with a methanol/water solvent containing formic acid.&nbsp;</span></p><p><span>The targeted DESI imaging experiment detected gefitinib together with six metabolites in liver tissue. Signal intensities were generally highest at approximately 1 hour after dosing, but the compounds remained detectable at 24 hours. Importantly, this was achieved at a therapeutically relevant dose rather than the much higher doses often required for imaging studies. The spatial imaging data also showed good agreement with LC-MS/MS pharmacokinetic profiles, particularly for gefitinib and the M11 metabolite.&nbsp;</span></p><p><span>Overall, the poster demonstrates that tandem quadrupole DESI MRM imaging can complement conventional LC-MS/MS by adding spatial information to quantitative pharmacokinetic and metabolite data. The approach enables label-free mapping of drug distribution directly in tissue and may therefore provide a useful tool for drug metabolism and disposition studies during discovery and development.</span></p></div></div></div></div></div></div></section></div></div>

News from LabRulezLCMS Library - Week 41, 2026

News from LabRulezLCMS Library - Week 42, 2026

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

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4th European Sample Preparation Conference - 3rd Green and Sustainable Analytical Chemistry Conference (EuSP 2026 | GSAC 2026)

Thermo Fisher Scientific Mass Spectrometry Users’ Meetings 2026

Thermo Fisher Scientific Analytical solutions forum

Validated Method for PFAS Testing in Food, Including Meats

Confidence in PFAS Data: Smarter Sample Prep, Contamination Control, Highly Sensitive and Robust MS

From sample to result: advanced sample prep strategies for food and environmental matrices