Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 11th November 2024? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applications and other documents by SIELC, Thermo Fisher Scientific, Shimadzu, Waters Corporation, and Agilent Technologies!<h4>1. SIELC: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/241113_Samplify_Brochure_367aa5da2e.pdf">Samplify from SIELC Technologies</a></h4><ul><li>Brochure</li></ul><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/article/4709">What is Samplify</a>?Samplify is an innovative new technology from SIELC, specifically designed for unattended, routine, periodic sampling of virtually any liquid source. Each sample is transferred automatically into an individual destination vial or 96-well plate. Vial trays or plates may then be loaded directly into a variety of analytical systems for further processing.The <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1280">Samplify</a> system consists of two principal components:<ol><li>&nbsp;a sophisticated electro-mechanical sample probe constructed of materials providing chemical and temperature resistance, and</li><li>SIELC’s renowned and highly flexible liquid handler (LHS) for pulling samples from the liquid source and distributing samples into destination locations.</li></ol>The LHS offers many additional capabilities; for example, the addition of quenching reagents into sample vials immediately after acquisition, if required, and thorough probe cleaning to guard against cross-sample contamination. The entire system may be controlled with SIELC’s Samplify Windows app, or via serial port using provided commands.Samplify SpecificationsSamplify Probe<ul><li>Connection: requires Samplify LHS</li><li>Small dimensions: 11 x 1 inch, DIA 1/4 inch. Immersion length up to 6”</li><li>Contact with liquid: Stainless Steel 316 (316L), PEEK &amp; PTFE</li><li>Variable sample volume: from 5 to 500 μL</li><li>Max. working pressure: 120 psi (8 bar)</li><li>Max. working temperature: 200 °C</li></ul>Samplify LHS<ul><li>Instrument Size: 6 x 6.5 x 7 inch (15 x 16 x 17 cm)</li><li>Weight: 5 lb (2.3 kg)</li><li>Collection Options: 48 vial plate (2 mL vials); 96 well plate</li><li>Pressure Max: 250 psi/ 14 bar (4000 μL volume)</li><li>Syringe Capacity Options: 4000 μL</li><li>Valve Options: 7x6</li><li>Volume Accuracy: +/-1 μL (4000 μL volume)</li><li>Probe dead volume: 767 μL</li><li>Syringe draw/refill rates: 48,000 μL/min</li><li>Communication: USB (type B) COM port</li><li>Power: 24 V DC</li><li>Contact with liquid: Stainless Steel 316 (316L), PEEK, PTFE, Vespel</li></ul><h4>2. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_ultrafast_immunosuppressants_lc_ms_5994_7829en_agilent_414e1b7386.pdf">Ultrafast Quantitation of Immunosuppressant Drugs in Whole Blood by Agilent 6475 LC/MS</a></h4><ul><li>Application</li></ul>AbstractAn ultrafast, 2.5-minute quantitation method using liquid chromatography/mass spectrometry (LC/MS) for four immunosuppressant drugs was established using an Agilent 6475 triple quadrupole LC/MS with the RECIPE therapeutic drug monitoring (TDM) kit. This application note emphasizes validation of an ultrafast measurement of tacrolimus, sirolimus, everolimus, and cyclosporine A in whole blood with outstanding sensitivity and interday reliability.IntroductionTDM is essential for ensuring efficacy and minimizing the adverse effects of drug delivery. The need for immunosuppressant drugs for organ and bone marrow transplant patients has been growing annually. Administration of immunosuppressants is strictly monitored as many side effects, including nephrotoxicity and neurotoxicity, must be considered. LC/MS is considered the gold standard for measurement of immunosuppressants due to results showing remarkable sensitivity and specificity.The RECIPE ClinMass TDM kit system for immunosuppressants in whole blood (Munich, Germany) was used on the 6475 triple quadrupole LC/MS for analysis of tacrolimus, sirolimus, everolimus, and cyclosporine A. Validation of the RECIPE TDM kit was implemented to evaluate sensitivity, linearity, and interday repeatability across three consecutive days (n = 3). Sample preparation is straightforward without the need for complicated cleanup or filtration.ConclusionA rapid analysis of tacrolimus, sirolimus, everolimus, and cyclosporine A in whole blood was established on an Agilent 6475 triple quadrupole LC/MS. Together with straightforward sample preparation, the method demonstrates robust measurement of immunosuppressant drugs in biological samples. Ultrafast acquisition times allow the high-throughput analysis of more than 500 samples per day. By coupling with the ready-to-use RECIPE ClinMass TDM kit system, Agilent provides a comprehensive end-to-end solution for therapeutic drug monitoring (TDM) of immunosuppressants.<h4>3. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/tn_003318_lsms_mabs_orbitrap_ascend_biopharma_tn003318_na_en_180dc41f10.pdf">In-depth characterization of monoclonal antibodies</a></h4><ul><li>Application</li></ul>GoalTo assess the performance of the Thermo Scientific™ Orbitrap™ Ascend BioPharma Tribrid™ mass spectrometer for comprehensive monoclonal antibody (mAb) characterization using intact mass analysis and middle-down mass spectrometry (MD-MS) approaches. The MD-MS methods were developed using a combination of powerful ion activation techniques including electron transfer dissociation (ETD), electron transfer higher energy collision dissociation (EThcD), ultraviolet photodissociation (UVPD), and ion manipulation by proton-transfer charge reduction (PTCR).IntroductionmAbs can display structural heterogeneity due to the presence of various post-translational modifications (PTMs), such as glycosylation, oxidation, and deamidation. These modifications can affect their structure, stability, and function. Therefore, in-depth characterization of mAb heterogeneity is critical to ensure the safety, efficacy, and quality of biotherapeutics. The middle-down mass spectrometry (MD-MS) approach has emerged as a promising tool for therapeutic characterization.1-4 It involves the formation of mAb subunits by reduction and/or digestion, followed by tandem MS (MS/MS) fragmentation of these subunits, offering high sequence coverage while involving a straightforward sample preparation.The Orbitrap Ascend BioPharma Tribrid mass spectrometer offers many benefits for biopharmaceutical characterizations. The high mass accuracy and high resolution offered by the Orbitrap technology enable precise mass measurement of intact mAbs or subunits. The Orbitrap Ascend BioPharma MS provides multiple MS/MS fragmentation techniques, including collision-induced dissociation (CID), higher-energy collisional dissociation (HCD), ETD, EThcD, electron transfer and collision-induced dissociation (ETciD), and UVPD, to achieve a full characterization of mAbs. In addition, this powerful instrument offers the PTCR technology with extended mass ranges (up to 16,000 m/z with Native MS option enabled) that can be employed alone or combined with different fragmentation techniques for the characterization of complex biotherapeutics. The Orbitrap Ascend BioPharma MS also benefits from its unique revolutionary architecture by having a second ion-routing multipole (front HCD cell) in the system which improves the transmission of large molecules and increases the sensitivity to detect low-abundance species in complex samples.In this work, intact mass analysis and MD-MS approaches were employed to characterize trastuzumab and its subunits on an Orbitrap Ascend BioPharma Tribrid MS. All the analyses were performed in the intact protein mode at various pressure modes, and for intact trastuzumab the Native MS option was used. Figure 1 shows the main LC-MS workflow employed for intact and subunit analyses of trastuzumab.ConclusionIn this work, intact and middle-down workflows were employed to obtain precise intact mass and high sequence coverage of mAb subunits using the Vanquish Flex UHPLC system and Orbitrap Ascend BioPharma Tribrid mass spectrometer. The Orbitrap Ascend BioPharma MS provides the following advantages for comprehensive biopharmaceutical characterization.<ul><li>The high mass accuracy and high resolution offered by the Orbitrap technology provides precise mass measurement for both intact mAbs (native and denaturing) and their subunits.</li><li>The system provides multiple fragmentation techniques, such as ETD, EThcD, and UVPD, for achieving high sequence coverage for various biopharmaceutical molecules.</li><li>Compared to ETD, EThcD and UVPD provide an improved sequence coverage of mAb subunits due to the formation of additional fragment types.</li><li>The combination of PTCR with EThcD and UVPD led to further increase in sequence coverage of mAb subunits and the number of complementary ion pairs.</li><li>The combination of EThcD, UVPD, and PTCR offers a nearly complete sequence coverage (&gt;90%) for subunits in the size of 20–25 kDa (Fc/2, LC, and Fd’ subunits) and high sequence coverage (&gt;70%) for the HC subunit (≈50 kDa).</li></ul><h4>4. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00814_en_028966d0aa.pdf">Automatic Optimization of Gradient Conditions by AI Algorithm on Synthetic Peptide and Impurities</a></h4><ul><li>Application</li></ul>User Benefits<ul><li>The AI algorithm of LabSolutions MD can automatically optimize gradient conditions to greatly reduce labor of LC method development.</li><li>Anyone can optimize gradient conditions, regardless of their experience in chromatography.</li><li>Gradient conditions that meet the resolution criteria for specified peaks are automatically searched (e.g., principal component and related impurities).</li></ul>IntroductionIn the typical LC method development, the process begins with “preparation” which includes mobile phase preparation, column installation, and creation of analysis schedules, then the analysis is started. After that, the acquired data is analyzed and “preparation” for the subsequent analysis is carried out, followed by starting the next analysis again. The method development progresses by repeating these processes, but in addition to the significant time required to repeatedly create analysis schedules, expertise in chromatography is necessary to explore optimal conditions based on data analysis. In other words, typical method development requires “human intervention”. Therefore, eliminating human involvement and automating such method development processes would be desirable to improve labor efficiency. This article introduces an example of automatic optimization of gradient conditions to meet resolution criteria for synthetic peptide and related impurities using LabSolutions MD (<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c190_e309_96044bc345/c190-e309.pdf">Technical Report C190-E309</a>), a dedicated software for supporting method development.ConclusionAutomatic optimization of gradient conditions using AI algorithm of LabSolutions MD was applied to synthetic peptide and related impurities. As a result, gradient conditions that met the criteria (resolution for FLP &gt; 2.0) were successfully explored. This result indicates that significant labor saving in method development can be expected by LabSolutions MD. This article introduces an automatic optimization of gradient conditions in method development while LabSolutions MD also supports a series of workflow of method development, including screening of mobile phases and columns. For details, please refer to the application news, “<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00780_en_4d0aa014ea.pdf">Efficient Method Development for Synthetic Peptide and Related Impurities (01-00780)</a>”.<h4>5. Waters Corporation / <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/303">HPLC</a>: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/hplc_2024_gauthier_mixers_d9bc1d801d.pdf">COMPARISON OF MIXER PERFORMANCE FOR HPLC METHODS UTILIZING TFA GRADIENTS</a></h4><ul><li>Poster (<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/303">HPLC</a>)</li></ul>INTRODUCTIONSolvent mixing is critical to obtaining optimal LC separations. Currently, there are two commonly available pump mixing designs for reversed phase gradient HPLC separations - high pressure (typically binary) and low pressure (all quaternary) systems. High pressure systems use two independent pumps to deliver different solvents. Mixing occurs at high pressures with solvent composition controlled by the flow rates of the two pump heads. In low pressure systems, solvent composition is controlled by a gradient proportioning valve. Each solvent is delivered in packets (based on the gradient specified in the method) which are mixed as they go through the pump head. Both high and low pressure systems are subject to mobile phase composition fluctuations. Mixers of various volumes and designs are utilized to help minimize these composition fluctuations by reducing baseline noise and oscillations in mobile phase composition.Trifluoroacetic acid (TFA) is a commonly used ion-pairing reagent used in combination with acetonitrile for many gradient reversed phase applications. TFA absorbs strongly at wavelengths below 250 nm. Additionally, TFA is slightly retained on reversed phase columns which results in fluctuations in TFA concentration as the acetonitrile gradient passes through the column. In combination, these factors result in significant baseline disturbances (ripples) when TFA - acetonitrile gradients are used at low wavelengths. These baseline ripples may make peak integration difficult, and can impact the sensitivity and retention time precision of the method.Most modern HPLC systems include a standard mixer in the pump design. Additionally, different mixers may be available to improve mixing performance for specific applications. In this study, mixers of varying volumes and design were evaluated.CONCLUSIONMixing performance is critical to obtaining optimal LC separations. In this study, several HPLC systems and mixers were evaluated using a TFA-Acetonitrile gradient method at a low wavelength which is known to produce baseline ripples. The USP signal to noise ratio was used to determine the impact of the different mixers.The results demonstrate that the sensitivity of the method is impacted by the system/mixer used, and consideration should be given to mixer selection, especially when running methods which are subject to increased baseline noise.

News from LabRulezLCMS Library - Week 46, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 18th November 2024? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applications, presentations, and posters by Metrohm, Thermo Fisher Scientific, Shimadzu, Waters Corporation, and Agilent Technologies!<h4>1. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/why_use_hilic_and_hic_chromatography_oct082024_51637eb877.pdf">Why Use HILIC and HIC Chromatography?</a></h4><ul><li>Presentation</li></ul><h5>Agenda</h5><ul><li>What is HILIC and when should you consider it?</li><li>How to approach HILIC method development<ul><li>Agilent HILIC column options</li><li>Mobile phase considerations</li></ul></li><li>Common HILIC application areas</li><li>Tips and tricks for successful HILIC column use and care<ul><li>Column equilibration</li><li>Sample solvent compatibility</li><li>Inert HILIC solution for metal-sensitive compounds</li></ul></li><li>What is HIC and its separation mechanism?</li><li>Requirements for HIC<ul><li>Factors affecting selectivity</li></ul></li><li>Common HIC application areas<ul><li>Post-translational modification (PTM) analysis</li><li>Separation of NIST mab (RM 8671)</li><li>Monitoring oxidation in mAbs</li></ul></li></ul><h5>Summary</h5>When to consider a HILIC column:<ul><li>Are your analytes unretained with RPLC?</li><li>Are your analytes at least somewhat soluble in acetonitrile?</li><li>Are you using MS detection?</li><li>Do your analytes interact with metals in the LC system?</li></ul>Keep the sample solvent in mind for HILIC analyses: prepare the sample in as much acetonitrile as possible, and keep injection volumes as small as possible.<ul><li>Most common support issue with HILIC methods</li></ul><h4>2. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_06_saip_lc_077_en_e0b92b59d4.pdf">Simultaneous Quantitation of 32 PFAS in Baby Food by LC-MS/MS</a></h4><ul><li>Application</li></ul>User Benefits<ul><li>A simple QuEChERS extraction procedure has been employed for quantifying the PFAS with normal dSPE cleanup.</li><li>This method complies with all acceptance criteria (as per AOAC SMPR 2023.003) without using ISTDs.</li><li>Method with shorter run time can contribute to achieving high throughputs in testing laboratories.</li></ul>IntroductionPFAS (Per- and polyfluoroalkyl substances) are a class of highly persistent chemicals widely known as "forever chemicals" due to their strong resistance to environmental degradation (Figure 1). Found in products like firefighting foams, non-stick cookware, and water-resistant fabrics, PFAS are now recognized as major environmental and health concerns. These substances accumulate in soil, water, and living organisms, including humans, where they may cause serious health impacts over time.Given their potential for long-term contamination, the detection and quantification of PFAS are critical. Advanced analytical methods, particularly LC-MS/MS with Multiple Reaction Monitoring (MRM), offer the specificity and sensitivity needed to accurately measure PFAS concentrations. However, one of the primary challenges in PFAS analysis is minimizing background contamination from PFAS residues within the LC system and during sample collection and preparation. Effective strategies to reduce these sources of contamination are essential for reliable results in PFAS quantification.n this application news, we describe a single laboratory validation study with a rapid extraction of trace level concentrations of 32 PFAS (Table 1) in infant formula (baby food) involving the use of the QuEChERS as an extraction technique followed by mass spectrometric analysis using a Shimadzu LCMS-8060NX triple quadrupole mass spectrometer coupled to a Shimadzu Nexera X3 liquid chromatograph (Figure 2).Conclusion<ul><li>A simple, sensitive, and rapid LC-MS/MS method has been developed to quantify 32 PFAS compounds in infant formula.</li><li>This method utilizes a QuEChERS-based extraction technique for efficient sample preparation.</li><li>With Shimadzu’s LC-MS/MS, the method demonstrated high sensitivity and reproducibility, achieving low relative standard deviations (RSDr and RSDR) in accordance with AOAC SMPR standards at trace levels.</li><li>This approach offers a reliable solution for multi-PFAS analysis in infant formula, making it highly applicable for testing laboratories focused on food safety.</li></ul><h4>3. Thermo Fisher Scientific / <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/170">RAFA</a>: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PFAS_analysis_strategy_story_direct_injection_DLLME_LC_MS_MS_LC_Orbitrap_GC_Orbitrap_7592743c1a.pdf">PFAS analysis strategy story – direct injection, DLLME, LC-MS/MS, LC- Orbitrap / GC-Orbitrap</a></h4><ul><li>Poster / <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/170">RAFA</a></li></ul><h5>Abstract</h5>Purpose: This work summarizes key components of PFAS analysis. The choice between direct injection and automated sample preparation depends on the instrument's dynamic range, detection limits, and matrix complexity. Complex matrices like waste/industrial water, soil, food, and biological samples require specific preparation techniques to mitigate matrix effects and ensure accurate quantification. Techniques such as Dispersive Liquid-Liquid Microextraction (DLLME) can significantly improve concentration factors and reduce matrix interference, enhancing overall method performance. Additionally, the choice of the analyzer is a critical consideration.Methods: Direct injection of water sample was performed on Thermo Scientific TSQ Altis Plus triple quadrupole mass spectrometer. For those sample prepared with automated dispersive liquid-liquid microextraction (DLLME), acquisition was performed on a Thermo Scientific Orbitrap Exploris MX high resolution mass spectrometer.Results: The methods presented achieves high-level sensitivity for PFAS analysis in drinking water, detecting compounds in the low ng/L range. Using DLLME, 56 PFAS compounds were quantified to low part per trillion levels from just 15 mL of sample. With a FAPAS®-Drinking Water proficiency test, we validated the three strategies for PFAS analysis: direct injection on TSQ Altis Plus and the DLLME extract injected on both Orbitrap Exploris MX and Thermo Scientific Orbitrap Exploris GC.<h5>Conclusions</h5><ul><li>Compared to traditional SPE workflows, direct injection improves sample throughput in laboratories by significantly reducing the required sample preparation.</li><li>The DLLME method is a promising technique for extracting and pre-concentrating PFAS from drinking water and various other matrices. Its reduced sample volume facilitates easier handling, transportation, and storage.</li><li>Both methods lower costs and environmental impact due to minimal solvent usage and the elimination of filters or SPE cartridges.</li><li>The ease of use and robustness of both LCMS methods are based on fixed configuration including SOP with detailed hardware and consumables, a complete acquisition and processing method with customized view settings and reports, and all data handling performed with Chromeleon CDS 7.3.2.</li></ul><h4>4. Waters Corporation / <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/303">HPLC</a>: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/2024_hplc_zabala_cortecs_solid_core_scalability_3ffe31ac22.pdf">SCALABILITY OF SOLID-CORE PARTICLES FOR CHROMATOGRAPHIC ANALYSES</a></h4><ul><li>Poster / <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/303">HPLC</a></li></ul>NTRODUCTIONLiquid Chromatography plays a crucial role in many areas of science. It is widely used for quality control of pharmaceuticals and biologics, research and medical purposes (1). Over the last several decades the gold standard of analysis for these areas of science has been High-Performance Liquid chromatography (HPLC). Typical HPLC systems operate within a 6000 psi pressure limit (2). Consequently, they are commonly paired with columns packed with 3 - 5 μm particles. Although smaller particle-packed columns allow faster separations, their use in HPLC is restricted to shorter lengths due to elevated backpressures (3). Additionally, established methods which are often used in a quality control setting may restrict alterations to particle size or column configuration.Improved column efficiency on an HPLC system can be achieved using solid-core particles. Solid-core particles have a non-porous “solid” center and a porous outer layer(4). Columns packed with solid-core particles offer distinct advantages over those packed with fully porous particles, including higher efficiency and reduced operating backpressure. Waters offers a line of solid-core particle columns known as CORTECS Columns.By utilizing CORTECS Columns, researchers can increase separation efficiency, achieve faster analysis times, reduced solvent waste and decreased column back pressure. In this poster, we delve into the significance of larger solid-core particles for scalability. We compare columns packed with 5 μm CORTECS Prototype Material, CORTECS UPLC μm) Material and CORTECS HPLC (2.7 μm) C18 Material with columns packed with fully porous particles. Additionally, we explore how CORTECS Columns differ from similar offerings on the market.CONCLUSION<ul><li>5 μm CORTECS Prototype Columns have 28% lower back pressure in comparison to 3.5 μm XBridge BEH C18 Columns.</li><li>5 μm CORTECS Prototype Columns have 14% higher optimal efficiency in comparison to 3.5 μm XBridge BEH C18 Columns.</li><li>CORTECS Columns are scalable across all 3 particle sizes shown.</li><li>In comparison, Vendor H and A columns are not scalable across all 3 particle sizes due to the significantly lower retention in the 4 and 5 μm particle size columns, shown in Figure 3.</li></ul><h4>5. Metrohm: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_bat_015_download_c51bc5f0fe.pdf">Differential capacity analysis (DCA) for battery research with INTELLO</a></h4><ul><li>Application</li></ul>Introducing dQ/dE plots, applications, and moreDifferential capacity analysis (DCA) is a powerful diagnostic technique widely used in battery research and development to gain detailed insights into the electrochemical behavior of batteries. DCA allows researchers to identify key electrochemical processes, phase transitions, and degradation mechanisms occurring within the battery during charge and discharge cycles. This technique is particularly valuable for characterizing complex systems such as lithium-ion batteries, where multiple electrochemical reactions may overlap.This Application Note explores the principles and practical applications of differential capacity analysis, highlighting its role in improving battery performance. This application also reveals how INTELLO, with its dedicated suite of battery-oriented commands and its ability to untether during long measurements, is an excellent choice for battery researchers looking to maximize their time and efficiency when conducting DCA.INTRODUCTIONWithin the INTELLO battery cycling environment, it is possible to sample the differential capacity (defined as dQ/dE = |Qn+1-Qn|/(En+1-En), where n is the index of the data point, Q is the value of the charge/discharge capacity, and E is the measured working electrode potential) and plot by default this value versus the measured voltage of the cell. Note that a general introduction to the cycling environment in INTELLO is provided in <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_bat_014_download_6c810739bf.pdf">AN-BAT-014</a> while this Application Note specifically focuses on the dQ/dE plot and what can be derived from it.

News from LabRulezLCMS Library - Week 47, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 25th November 2024? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applications by Thermo Fisher Scientific, Shimadzu, Waters Corporation, and Agilent Technologies!<h4>1. Thermo Fisher Scientific: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/tn_003155_cl_clinical_lc_orbitrap_ms_hemoglobin_tn003155_na_en_7e093438cb.pdf">Enhancing detection of hemoglobin variants in clinical research using dried blood spot and high-resolution accurate mass (HRAM) Orbitrap mass spectrometry</a></h4><ul><li>Application</li></ul>Application benefits<ul><li>Direct protein extraction from dried blood spots for protein identification and quantitation</li><li>Identification: utilizing a top-down analysis approach to obtain Hb variant sequences for the characterization of structural mutation</li><li>Quantitation: utilizing intact protein precursor isotopic m/z to determine ratios between target chains and variants</li><li>Minimal sample preparation (&lt;1 hr) in 96 well plate format, easily transferrable to automation using a robotic system</li><li>Confident data processing and review using automated software tools, Thermo Scientific™ ProSightPD™ software, and Thermo Scientific™ TraceFinder™ software</li></ul>GoalDevelop a top-down approach for hemoglobin variant detection using dried blood spots and a Thermo Scientific™ Orbitrap Exploris™ 240 mass spectrometerIntroductionHemoglobinopathies and thalassemia are the most common genetically determined disorders. They are caused by pathogenic variants in genes that control the production of hemoglobin subunits. Hemoglobin (Hb, approximately 62 kDa) is a tetramer, consisting of two alpha chains and two beta or beta-like chains. It is responsible for physiological oxygen transport in all vertebrates except for the Channichthyidae. Adult Hb consists of 96–98% Hb A (α2β2), 2.0–3.3% Hb A2 (α2δ2), and less than 1.0% Hb F (α2γ2).1 Hemoglobinopathy is a genetic defect characterized by the abnormal structure of one of the Hb subunits, usually resulting from single amino acid substitution. Thalassemia is characterized by the absence or decreased expression of one of the Hb subunits. The most common hemoglobinopathy is sickle cell disease (SCD, Hb S (β6 Glu→Val)). Around 5.2% of the global population carries significant hemoglobinopathy-causing genes with more than 330,000 affected births occurring annually.2Current techniques used in Hb analysis are electrophoretic and chromatographic assays. However, due to the lack of resolution, they are limited in differentiating isomers (i.e., between Hb C (β6 Glu→Lys) and Hb E (β26 Glu→Lys)), very similar masses (i.e., &lt;1 Da difference between normal Hb, Hb C, Hb E, and Hb D-Punjab (β121 Glu→Gln)), or new variants. Mass spectrometry has gained popularity in clinical research because of its robustness and versatility in analyzing a wide range of samples and analytes from small molecules to proteins. Targeted protein and peptide quantitation joined this trend by applying various proteomics approaches such as bottom-up, middle-down, and top-down methods. Recently, the top-down approach targeting intact protein biomarkers was enabled by high-resolution accurate-mass (HRAM) mass spectrometers such as Thermo Scientific™ Orbitrap™-based instruments. Here, we present the top-down analysis for enhanced detection of various hemoglobin variants using the Orbitrap Exploris 240 mass spectrometer for clinical research.ConclusionThis study successfully demonstrates the application of an LC-MS/MS top-down approach for detecting hemoglobin variants using dried blood spots and the Orbitrap Exploris 240 mass spectrometer. The method enables direct protein extraction with minimal sample preparation, allowing high-throughput analysis. The high resolution of the Orbitrap Exploris 240 MS effectively isolates and identifies hemoglobin variants, even with minimal mass differences, and detects low-abundance variants such as the Hb delta chain. The ProSightPD software enhances data analysis by generating sequence maps for variant identification. This approach provides a robust and efficient workflow for clinical research, offering significant improvements over traditional methods. This technical note demonstrated the feasibility of hemoglobin variant detection workflow, highlighting its potential for broader clinical research applications.<h4>2. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00758_en_25d3e480fb.pdf">MRM Based Free Fatty Acids Profiling in Human Plasma and Serum Using LC-MS/MS</a></h4><ul><li>Application</li></ul>User Benefits<ul><li>Simultaneous analysis of 19 free fatty acids in blood was allowed with simple pretreatment.</li><li>The delay column worked to separate the target fatty acids from the undesirable contaminants.</li><li>LCMS-8060RX newly equipped with CoreSpray enables stable and reliable quantitative analysis for trace amount of compounds.</li></ul>IntroductionFree fatty acids, about 5% of the total fatty acids in the body, are known to be important signal transducers that regulate functions such as insulin secretion. It is also attracting attention as a biomarker for various endocrine disorders1).Gas chromatography (GC) or gas chromatography-mass spectrometry (GC/MS) generally requires pretreatment such as methyl esterification for long-chain fatty acids and polyunsaturated fatty acids analysis. Multiple reaction monitoring (MRM) using liquid chromatography-mass spectrometry (LC/MS) enables highly sensitive quantitative analysis of fatty acids without derivatization. However, fatty acids widely found in the environment, such as palmitic acid and stearic acid, are introduced as impurities in LC system. It has been reported that there is difficulty in accurate quantification of these fatty acids in real samples analysis2).This report presents an example of quantitative analysis of free fatty acids in human plasma and serum using the highly stable LCMS-8060RX system coupled with a delay column.ConclusionSimultaneous analysis of 19 free fatty acids in human plasma and serum was performed using a high-performance liquid chromatograph mass spectrometer LCMS-8060RX. Good linearity was obtained in the range of 1-1000 for all compounds, and we also confirmed that the repeatability at lowest calibration point was less than 10%.The use of a delay column allowed removing the matrix peaks derived from the mobile phase. This analytical method provides more stable and accurate quantitative analysis with simple pretreatment.<h4>3. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_limonin_quantitation_tof_lcms_5994_7954en_agilent_1_c2afbe89e1.pdf">Determination of Limonin in Citrus Flour by Time of Flight (TOF) LC/MS</a></h4><ul><li>Application</li></ul>AbstractIn recent years, citrus flour has become a popular additive to meat and dairy plant-based substitutes as it holds water, emulsifies, binds oil, improves texture and stability over time, and is vegan. Citrus flour contains high concentrations of limonin, a limonoid that results in a delayed bitter taste and is undesirable. Industry processes reduce bitter taste in citrus flour by removal or modification of limonin and other limonoids. The method presented here is useful in the quantitation of limonin in foods, food additives, juices, and plants. This method yields good accuracy, precision, linearity, and range in matrix. The use of an Agilent 6230B Time of Flight LC/MS allows limonin to be distinguished and quantitated. Congeners can also be identified and quantitated.IntroductionThe recent rise in popularity of meat and dairy plant-based substitutes have necessitated the use of citrus fiber or flour to replace starches, gums, chemical emulsifiers, and stabilizers. Citrus flour holds water, emulsifies, binds oil, and is vegan. This natural citrus flour improves texture and stability over time and is particularly useful in baked goods, beverages, dairy products, dressings, meats, sauces, frozen foods, pet foods, dairy alternatives, and plant-based meats.The global citrus flour market size was valued at USD 427.3 million in 2022 and is projected to reach USD 726.9 million by 2032, growing at a compound annual growth rate (CAGR) of 5.7% from 2023 to 2032.1 The citrus flour market is being driven &nbsp;in part by the increased focus on health and well-being throughout the world. Being a high-quality dietary fiber source, citrus flour supports satiety and digestive health. Citrus fiber is becoming a sought-after component in formulas with a health focus as consumers become more conscious of the connection between nutrition and overall health and seek goods that have beneficial nutritional qualities and taste good.Limonin is enriched in citrus fruits and is often found in higher concentrations in seeds, pulp and peel of oranges, grapefruit, lemons, limes, pumellos, bergamots, and mandarins.2 Citrus flour is made from leftover dried fibrous material after the fruit is juiced and can have high concentrations of limonin and other limonoids. Limonin and other limonoid compounds contribute to the delayed bitter taste of some citrus food products and is therefore undesirable.Limonin is a limonoid: a bitter, white, crystalline substance found in citrus and other plants. It is also known as limonoate, D-ring-lactone, and limonoic acid di-delta-lactone.3 Chemically, it is a member of the class of compounds known as furanolactones. Limonin has an exact mass of 470.19406791 g/mol.4 The method presented in this application note is useful in the quantitation of limonin in foods, food additives, juices, and plants. The use of a Time of Flight LC/MS allows excellent quantitation of limonin as well as the characterization of other congeners.ConclusionThe method described in this application note for the determination and quantitation of limonin in citrus flour using an Agilent Time of Flight LC/MS has been shown to be linear, accurate, and precise over typical industrial concentrations. The use of Agilent Time of Flight LC/MS technology also allows the characterization and quantization of congeners and other matrix components. Post-run screening for other compounds is easily accomplished.<h4>4. Waters Corporation: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008552_en_bd88faf6b3.pdf">Metabolomics Workflow using a Xevo™ MRT Mass Spectrometer</a></h4><ul><li>Application</li></ul>AbstractWe demonstrate the acquisition and data processing to identify and pathway profile a typical metabolomic study acquired using a Xevo™ MRT Mass spectrometer coupled with an ACQUITY™ Premier LC System. The resulting data shows a clear unsupervised PCA separation between the three study groups with exogenous or environmental markers being the most significant differences from the different volunteer lifestyles. The Xevo MRT MS delivers rapid, robust data acquisition for large cohort metabolomic studies, capable of providing a high mass resolution of up to 100,000 full width half maxim (FWHM) and consistent sub-ppm mass accuracy, ensuring the analyst has increased confidence in putative feature identification.Benefits<ul><li>Simple and robust workflow delivering excellent data reproducibility and confident results</li><li>A powerful benchtop mass spectrometer routinely providing high mass resolution for both precursor and product ions, enabling separation of compounds with near identical molecular weights e.g. isoforms</li><li>Delivering a consistent mass accuracy &lt;1 ppm RMS, increasing confidence in putative feature identification</li><li>Ability to acquire data at extremely fast acquisition rates, maintaining mass resolution and mass accuracy benefits. Allowing compatibility with shorter chromatographic methods, increasing sample throughput</li><li>Wide dynamic range providing up to 5-orders of linearity, allowing for a single injection to accurately determine the relative concentration of both low and high abundance compounds within a complex matrix</li></ul>IntroductionMetabolomics is an area of research which aims to identify key metabolic markers originating from phenotypic differences e.g. disease state, environmental changes, treatment regime etc. This could be to improve the detection of disease, to assess impact of pollutants, or to assist with personalized/tailored medical treatment. The metabolome is very complex, containing thousands of analytes with a bias towards smaller molecular weight compounds. Once potential biomarkers have been highlighted using statistical analysis of the data, the challenge can be to confidently identify the compounds of interest.Higher mass resolution leads to narrower spectral peaks leading to more accurate mass measurement, allowing for tighter mass tolerances for elemental composition and/or database identification searches, improving the confidence in putative identifications. Many small molecules are also observed share similar molecular weights (isoforms). By increasing the mass resolution of the mass spectrometer data clarity is improved, with a higher mass resolution it is possible to separate two compounds with similar molecular weights. With lower mass resolution these isoforms may have merged to form a single spectral peak, leading to erroneous mass determination and incorrect compound identification.Using a commercially available urine metabolomics study, we demonstrate the benefits of the Xevo MRT QTof mass spectrometer: delivering routine sub-ppm mass accuracy and high mass resolution. This workflow utilizes the software package MARS (MassAnalytica, Barcelona, Spain) for data processing, statistical analysis and putative identification. A more detailed overview of this software and its functionality can be found in the Waters™ application note: Screening Metabolomics of Human urine using a Waters High Resolution QTof Mass Spectrometer and MARS Data Processing Software.1 The resulting data showed significant changes in exogenous or environmental markers for each of the different volunteer lifestyles.ConclusionWe demonstrate that the Xevo MRT Mass Spectrometer coupled with an ACQUITY Premier LC System delivers rapid, robust data acquisition for metabolomic studies. When data is imported into MARS software for data processing this platform provides a powerful tool for acquisition, statistical analysis and putative identification of compounds of interest for metabolomic studies.This workflow provides the acquisition and data processing needed to confidently identify and pathway profile a typical metabolomic study. The resulting data shows a clear unsupervised PCA separation between the three study groups, putatively identifying several exogenous or environmental markers with a sub 1 ppm mass accuracy and fragmentation patterns, which match closely to theoretical. When these analytes are visualized using a trend plot, significant fold changes indicate differentiation between the three smoker levels. The Xevo MRT MS, delivering a high mass resolution of up to 100,000 FWHM and routine sub-ppm mass accuracy, gives the analyst increased confidence in putative feature identification.

News from LabRulezLCMS Library - Week 48, 2024

News from LabRulezLCMS Library - Week 49, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 9th December 2024? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applications by Shimadzu, Metrohm, and &nbsp;Waters Corporation, a presentation by Agilent Technologies, and a poster from MSACL by Thermo Fisher Scientific!<h4>1. Shimadzu: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00750_en_bee79113e7.pdf">Analysis of Per- and Polyfluoroalkyl Substances (PFAS) using Triple Quadrupole Mass Spectrometer Part 1 - Fish Fillet</a></h4><ul><li>Application</li></ul>User Benefits<ul><li>The optimized procedure for pretreatment and LC-MS/MS analytical conditions enable accurate quantification of thirty major PFASs targeted by AOAC SMPR from 0.1 μg/kg.</li><li>The method allows the initiation of PFASs analysis in food.</li></ul>IntroductionPer- and Polyfluoroalkyl Substances (PFASs) are a collective name for more than four thousand organofluorine compounds. Perfluorooctane sulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) are representative compounds of PFAS. They are used in a wide range of applications, such as fire retardants, food packaging materials, and non-stick coatings, due to their water-repellent, oil-repellent, heat-resistant, and chemical-resistant properties. Due to their structural stability, PFAS widely remains in the environment. There are concerns about health risks caused by human ingestion of fish that have ingested seawater, river water, or feed contaminated with PFAS. Therefore, quantitative assessment of PFAS levels in fish should be important.This application news introduces a quantitative analysis of PFAS in tuna fillets with LC-MS/MS. Thirty principal PFASs targeted by AOAC INTERNATIONAL, a North American organization that standardizes food testing methods and verifies analytical methods, were analyzed using newly created method, which was investigated from the pretreatment procedure then validated by recovery test. By reducing losses during the pretreatment and optimizing the analytical conditions, good recovery rates were obtained for all compounds.ConclusionThis application news described a quantitative analysis of thirty PFAS targeted by AOAC INTERNATIONAL in tuna fillet. The analysis was performed using a quadrupole mass spectrometer LCMS-8060NX equipped with ultra-high performance liquid chromatograph Nexera X3 UHPLC system. Shim-pack Scepter, which provides good separation and peak shape, was used as the column. A spiked recovery test were conducted, and all compounds showed recovery rate within 80-120% and repeatability below 20% at spiked concentrations of 0.1, 1, 5 μg/kg. In particular, recovery rates of PFOS, PFOA, PFNA, and PFHxS were within 95.5-108.4% at all spiked concentrations. Using optimized pretreatment and analytical methods, accurate quantitation is possible from 0.1 μg/kg.<h4>2. Agilent Technologies: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/getting_the_most_from_your_diode_array_detector_aug292024_a46bb2eeed.pdf">Getting the Most from Your Diode Array Detector</a></h4><ul><li>Presentation</li></ul><h5>Agenda</h5><ul><li>Introduction</li><li>Fundamentals<ul><li>Beer-Lambert law</li><li>UV-vis detection</li><li>DAD and MWD</li><li>DAD spectra collection</li><li>UV spectrum confirmation</li><li>peak purity</li></ul></li><li>Maximizing sensitivity<ul><li>What is sensitivity?</li><li>Factors affecting sensitivity</li><li>Analyte</li><li>Factors affecting sensitivity</li><li>System</li><li>Detector</li></ul></li><li>Spectral acquisition<ul><li>Settings</li><li>Spectrum storage</li><li>Range, step, and threshold</li><li>OpenLab Resources</li></ul></li><li>DAD maintenance<ul><li>Maintenance schedule</li><li>InfinityLab LC performance standard</li><li>Lab advisor</li><li>Care of flow cells</li><li>Flow cells</li><li>Best practices</li><li>Maintenance resources</li></ul></li><li>Troubleshooting</li><li>Additional Resources</li></ul><h4>3. Waters Corporation: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008521_en_ff59413ad8.pdf">HPLC Autosampler Performance II: Improved Injection Precision of USP Methods With the Alliance™ iS HPLC System</a></h4><ul><li>Application</li></ul>AbstractMethod conditions and instrument characteristics can affect the autosampler performance of High-Performance Liquid Chromatography (HPLC) systems. Challenging method conditions, such as low injection volume and highly organic sample diluents, require high precision to meet strict suitability requirements. Instrument characteristics, such as sample aspiration mechanism and injector draw rate, often vary between vendors and may impact the precision performance of the autosampler. This can pose a challenge for analytical laboratories that desire to run methods with strict precision suitability criteria across HPLC systems from different vendors. In this study, the injection precision performance of the Alliance iS HPLC System and similar HPLC systems were compared using four compendial HPLC methods from the United States Pharmacopeia (USP) with strict precision criteria and challenging method conditions. Peak area reproducibility was evaluated as a proxy for autosampler performance of each system.Benefits<ul><li>High precision for a range of sample diluents and injection volumes on the Alliance iS HPLC System</li><li>Meets strict injection precision criteria for challenging USP methods on the Alliance iS HPLC System</li><li>Demonstrates improved precision on the Alliance iS HPLC System over similar HPLC systems for highly organic sample diluent</li></ul>IntroductionFor many regulated methods in the United States Pharmacopeia (USP), injection precision is a common system suitability criterion. Injection precision is a measure of the autosampler performance in a high-performance liquid chromatography (HPLC) system. The autosampler is responsible for delivering precise aliquots of sample to the HPLC system flow path.1 This performance can be impacted by method conditions and instrument characteristics.2,3,4 To ensure that acquired data is accurate and meets suitability requirements of the method, high performance is required from an autosampler.Instrument characteristics, such as sample aspiration mechanism and injector draw rate, vary among vendors due to differences in system design. Sample aspiration is typically controlled by either a metering device or a sampling syringe.1 Injector draw rate is a setting typically set to a default speed that often varies with instrument vendor.4 These different characteristics can complicate running methods across systems from different vendors. A routine method that performs well on one HPLC system may not meet system suitability criteria on a different HPLC system. Therefore, it is important to consider how autosampler performance is affected by instrument characteristics.In this study, four USP Assay monographs were used to examine the impact of instrument characteristics on injection precision of an Alliance iS HPLC System and comparable HPLC systems. The HPLC systems include sampling syringe and metering device aspiration mechanisms and utilize different injector draw speeds. The USP Assay methods have challenging method conditions: varying organic content in the sample diluent (20%–100% organic), low injection volumes (6.6 μL–20 μL), and narrow injection precision criteria (0.73% to 2.0%).ConclusionThe ability of an HPLC system to acquire consistent, repeatable data is critical and requires high performance from an autosampler. This study examined the impact of instrument characteristics, such as sample aspiration mechanisms and injector draw rates, on HPLC performance in meeting precision requirements. Autosampler performance is complex and was found to vary with the method and the system. The metering device has benefits for precision performance over the sampling syringe, using a more finely tuned syringe draw motor and being located in-line with the high-pressure flow path.For fluconazole and ketoconazole USP assays, the Alliance iS HPLC demonstrated the best performance overall, with the lowest peak area %RSDs. The ketoconazole assay had particularly challenging method conditions and produced widely varying results among the HPLC systems. Alliance iS HPLC System demonstrated high precision and produced consistent and reproducible results across the three-day period, meeting the stringent 0.73% peak area RSD requirement.The ketoconazole assay produced disparate results among the HPLC systems using metering devices, which was unexpected. Upon tracking the absolute peak area of ketoconazole for each system, evaporation and carryover were ruled out as causes of the peak variability. Additionally, despite identical injector draw rates on two of the HPLC systems, their performance varied significantly. While aspiration mechanism and injector draw rate are important factors, they do not fully explain the observed variations in autosampler performance.<h4>4. Metrohm: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_c_198_download_6dcbc46fdf.pdf">Calcium acetate assay in calcium acetate capsules</a></h4><ul><li>Application</li></ul>Method validation according to the U.S. Pharmacopeia (USP)Calcium acetate functions as a phosphate binder in the gastrointestinal tract, helping to lower high phosphate levels in individuals with kidney disease who are receiving dialysis treatment [1,2]. To meet the stringent quality standards for pharmaceutical products, manufacturers and laboratories must use validated methods from the United States Pharmacopeia – National Formulary (USP-NF). Previously, such methods included titration or liquid chromatography (LC) with UV detection. As part of their modernization efforts, the USP has updated the calcium monograph to include ion chromatographic (IC) analysis, which is more straightforward and sensitive than previous methods. For the calcium acetate assay, the USP specifies ion chromatography using a cation-exchange column with L76 column material and non-suppressed conductivity detection to quantify the amount of calcium ions in calcium acetate capsules [3].The current IC method employs a Metrosep C 6 -150/4.0 column (L76) to separate calcium from other ions in calcium acetate capsules. This method has been validated according to USP General Chapters &lt;621&gt; Chromatography [4] and &lt;1225&gt; Validation of Compendial Procedures [5]. All acceptance criteria for the calcium acetate assay in the USP monograph «Calcium Acetate Capsules» are met.SAMPLE AND SAMPLE PREPARATIONThe standard solution nominally contains 0.08 mg/mL of USP Calcium Acetate Reference Standard (Cat#1086334) in water. It is prepared by accurately weighing 80.0 mg of USP Calcium Acetate Reference Standard and transferring it into a clean 1000 mL volumetric flask. It is dissolved and made up to the mark with ultrapure water (UPW).For sample stock solutions nominally containing 6.7 mg/mL of calcium acetate, an appropriate portion of the contents of at least 20 capsules are transferred into a 2000 mL volumetric flask. UPW is added to about 40% of the final volume of the volumetric flask, and the solution is then sonicated for 30 minutes with intermittent shaking. Afterwards, the solution is made up to the mark with UPW and filtered through 0.2 μm filter paper.For sample solutions nominally containing 0.08 mg/mL of calcium acetate, 5.97 mL of sample stock solution are transferred into a clean 500 mL volumetric flask. This is diluted and made up to the mark with UPW. All solutions are sonicated for 5 minutes before injection.CONCLUSIONAccording to the USP monograph for calcium acetate capsules [3], the assay for calcium acetate involves determining calcium content using ion chromatography (IC) on a separation column with L76 packing material (here: Metrosep C 6). The validation results met all requirements of the monograph and adhered to the guidelines specified in USP General Chapters &lt;621&gt; Chromatography and &lt;1225&gt; Validation of Compendial Procedures [4,5]. The described IC method is appropriate for quantifying calcium in calcium acetate capsules.<h4>5. Thermo Fisher Scientific / <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/294">MSACL</a>: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_quantitation_per_polyfluoroalkyl_human_serum_po_en_e61e41c57b.pdf">Quantitation of a Panel of Per- and Polyfluoroalkyl Substances (PFAS) in Human Serum</a></h4><ul><li>Poster (<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/294">MSACL</a>)</li></ul><h5>Abstract</h5>Purpose: Develop an LC-MS analytical method for quantitation of PFAS compound in human serum.Methods: Human serum samples were spiked with 37 PFAS compounds followed by protein precipitation with 4x volume of methanol. The supernatant was analyzed on an LC-MS system equipped with low-PSAF tubing and a delay column to minimize background interferences.Results: LOQs from 0.025 to 2.5 ng/mL were reached for all compounds.<h5>Introduction</h5>Per- and polyfluoroalkyl substances have been monitored in environmental and industrial samples for some time. Wellness panels are becoming more frequent and quantitating PFAS in biological samples are a part of these panels. Due to the evolving regulations and discoveries of potential health effects with these compounds it important to measure a wide range of PFAS compounds.<h5>Conclusions</h5><ul><li>10-minute method for 37 PFAS compounds on the Vanquish UHPLC and TSQ Altis Plus was developed. The method showed good accuracy and precision measurements.</li><li>While this method used simple protein precipitation for sample processing, future work includes developing an SPE method to enhance detection limits.</li></ul>

News from LabRulezLCMS Library - Week 50, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 6th January 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applications by Shimadzu, Metrohm, and &nbsp;Waters Corporation, a presentation by Agilent Technologies, and a poster from MSACL by Thermo Fisher Scientific!<h4>1. ALS Europe: Environmental Challenges of Pharmaceuticals: Persistence and Accumulation in Ecosystems</h4><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/enviromail_21_europe_environmental_challenges_of_pharmaceuticals_nov2024_ad8337748c.pdf">Full PDF for download</a></li></ul>The drugs are used extensively not only in human and veterinary medicine but are also widely found in livestock feed. Because pharmaceuticals are designed to be effective even at low concentrations, these specific contaminants can exist in the environment at extremely low levels. As with pesticides, these compounds can accumulate in different parts of the ecosystem. Since conventional wastewater treatment plants cannot adequately remove these substances, they are released into the environment, including surface and groundwater, and consequently into drinking water sources.<h5>Pharmaceuticals as "New" Pesticides...</h5>Pharmaceuticals represent a broad and chemically diverse group of substances that is continuously expanding and is characterised by a wide range of clinical effects and extensive use, often leading to overuse, in both human and veterinary medicine. From an environmental perspective, they are classified as organic micropollutants due to their presence in water at low concentrations (ranging from ng/L to μg/L). Both the public and experts are concerned not only about their negative impacts on natural ecosystems but also about their presence in drinking water and the related effects on human health. Their contribution to the emergence of antimicrobial resistance (AMR) is also significant, as it greatly complicates the treatment of infectious diseases and represents a major challenge for current and future medicine.Drugs can enter the environment through various pathways. One of the primary sources of contamination is wastewater from households and health and social care facilities, which contains human urine and faeces, as well as unused or expired pharmaceuticals. Another significant source is wastewater from the pharmaceutical industry. Consequently, wastewater treatment plants (WWTPs) themselves become sources of environmental contamination, as they are unable to effectively remove pharmaceuticals, allowing them to be transported further into the environment [1].ALS Laboratories have developed and accredited a multiresidue methods for the determination of more than 100 different pharmaceuticals and their metabolites in various types of water. All of our analytical methods use the LC/MS/MS technique for analytes determination, which provides high sensitivity, selectivity and precision of measurement and allows the determination of target compounds at the very low limits required for residue analysis.<h4>2. Thermo Fisher Scientific:&nbsp;Orbitrap Astral MS Literature List: Rethink what is possible</h4><ul><li>Guide</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/eb003337_ms_orbitrap_astral_litlist_eb003337_na_en_454d9ad02c.pdf">Full PDF for download</a></li></ul>Bacterial Proteomics, Drug Resistance, Crosslinking-MS, Metaproteomics, Data Analysis, Mamalian Development, Oxidation, Plant Proteomics, Phosphoproteomics, Plasma Proteomics, Single-Cell Proteomics, Reproducibility, Spatial Proteomics, Salivary Proteome, Technology, Tissue Proteomics, Ubiquitylation, Vaccine Research, Whole Proteome<h4>3. Agilent Technologies: Easy and Fast Automation of Sample Preparation</h4><ul><li>Application</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/te_injector_program_sample_preparation_hplc_5994_7703en_agilent_05f73923a6.pdf">Full PDF for download</a></li></ul>Sample preparation using injector workflows with the Agilent 1260 Infinity III Multisampler and Vialsampler.The demand for automated workflows is increasing as the number of samples in the lab continues to grow, but implementing automation in the lab environment is difficult, time-consuming, and costly. This technical overview describes an alternative method for implementing an automation method quickly and easily for sample preparation. This includes derivatization of amino acid samples, sample dilution, and preparation of calibration standards using an Agilent 1260 Infinity III Multisampler or Agilent 1260 Infinity III Vialsampler in combination with injector workflows. The results obtained were excellent in terms of precision, repeatability, and sensitivity, and are independent of the operator's skills.<h5>The 1260 Infinity III LC comprised the following modules:</h5><ul><li>Agilent 1260 Infinity III Binary Pump (G7112B)</li><li>Either: Agilent 1260 Infinity III Vialsampler (G7129A) with Integrated Column Compartment (G7130A), 100 μL analytical head and 100 μL sample loop (default setup)</li><li>Or: Agilent 1260 Infinity III Multisampler (G7167A) with 100 μL analytical head and 100 μL sample loop (default setup) and additional Multicolumn Thermostat (G7116A)</li><li>Agilent 1260 Infinity III Variable Wavelength Detector (VWD) (G7114A), equipped with a 10 mm standard flow cell (14 μL, option #018)</li><li>Agilent 1260 Infinity III Fluorescence Detector Spectra (FLD) (G7121B), equipped with an 8 μL FLD cell (G1321-60005)</li></ul><h5>Agilent OpenLab CDS version 2.8 or later</h5><h5>Columns</h5><ul><li>Agilent InfinityLab Poroshell 120 EC-C18, 2.1 × 50 mm, 2.7 μm (part number 699975-902)</li><li>Agilent AdvanceBio AAA LC column, 3.0 × 100 mm, 2.7 μm (part number 695975-322) with Agilent AdvanceBio AAA guard column, 3.0 × 5 mm, 2.7 μm (part number 823750-946)</li></ul>Injector workflows, in combination with the Agilent 1260 Infinity III Multisampler or Agilent 1260 Infinity III Vialsampler enable automation of certain sample preparation methods such as derivatization of amino acids, sample dilution, and preparation of calibration standards with excellent precision, repeatability, and sensitivity. The injector workflow differs from the conventional injector program in its ability to set up methods faster and easier without error, saving time and cost.<h4>4. Waters Corporation:&nbsp;Evaluation of Modern and Legacy HPLC Systems for the Size-Exclusion Analysis of Aggregation and Fragmentation in a Monoclonal Antibody Drug</h4><ul><li>Application</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008614_en_f03ac5dc38.pdf">Full PDF for download</a></li></ul>Size-exclusion chromatography is a widely used characterization technique for the analysis of aggregation and fragmentation of monoclonal antibody drugs. Traditional high-performance liquid chromatography systems have a large amount of extra-column dispersion which makes size-exclusion data analysis difficult due to band broadening and increased peak tailing. Additionally, biologic analytes may experience non-specific adsorption throughout the chromatographic flow path, further increasing the effects of peak tailing. The Alliance™ iS Bio HPLC System addresses both concerns by offering lower system dispersion than legacy HPLC systems alongside a bio-inert flow path employing MaxPeak™ High-Performance Surfaces Technology.In this work an Alliance iS Bio HPLC System, an Alliance e2695, and a competitive Bio-inert HPLC system are compared using a size-exclusion method for analysis of monoclonal antibody aggregation and fragmentation. Dispersion on each system is determined and the Alliance iS Bio HPLC is shown to have the lowest 4σ dispersion. This translates to lower peak tailing, tighter peak width, and a more accurate measurement of low- molecular weight species of infliximab due to lower monomer peak tailing and better monomer resolution.<h5>Benefits</h5><ul><li>Biocompatible system for use in salty bio-applications</li><li>MaxPeak HPS for reduced off-target analyte interaction results in less peak tailing</li><li>Low system dispersion results in better fragmentation determination</li></ul><h4>5. Shimadzu: Rapid Screening of 501 Emerging Contaminants in Water Using Polarity-Extended Liquid Chromatography-Mass Spectrometry</h4><ul><li>Application</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_03_lcmsms_919_en_1790a25e03.pdf">Full PDF for download</a></li></ul><h5>User Benefits</h5><ul><li>Polarity-Extended Liquid Chromatography combines hydrophilic interaction chromatography and reversed-phase chromatography to achieve simultaneous analysis of polar and weakly polar compounds.</li><li>This method can detect 501 emerging contaminants, offering a broad scope in terms of both quantity and variety.</li><li>The water sample is concentrated using freeze-drying method, effectively recovering both polar and non-polar compounds are recovered well.</li></ul><h5>Introduction</h5>In recent years, water pollution has become increasingly serious, and the problem of emerging pollutants in water has attracted much attention. Traditional analytical methods for emerging pollutants mainly focus on 1-2 categories of emerging pollutants and pay less attention to strongly polar pollutants. The Polarity-Extended Liquid Chromatography, through patented technologies such as polarity splitting, online dilution, and dual gradients, combines a Hilic column (first dimension) and a C18 column (second dimension), which can broaden the polarity analysis range of compounds and achieve simultaneous analysis of polar and weakly polar compounds. Fig. 1 shows the Polarity-Extended Liquid Chromatography-Mass Spectrometry System.In this paper, a method for rapid screening of 501 emerging pollutants was established by using Shimadzu's Polarity-Extended Liquid Chromatography-Mass Spectrometry System. This method solves the problem of simultaneous analysis of strong and weak polar pollutants.<h5>Conclusion</h5>In this study, a method for detecting emerging pollutants in water by combining the Polarity-Extended Liquid Chromatography and LCMS - 8050 series coupling system was established. This method combines hydrophilic interaction chromatography and reversed - phase chromatography to achieve the simultaneous separation of polar and non - polar compounds with a single injection. The detection of 501 emerging pollutants was achieved within 28 minutes. The linearity and repeatability of the method meet the quantitative requirements. After pretreatment operations such as freeze - drying, re-dissolution, and nitrogen blowing of the samples, the recovery rates for most compounds were satisfactory. This method has been successfully used for the rapid screening of new pollutants in tap water and sewage. The combination of Polarity-Extended Liquid Chromatography and mass spectrometry enables the one-injection analysis of compounds with different polarities without significantly increasing analysis time, making it suitable for the rapid screening of emerging pollutants in water.<h4>6. Metrohm:&nbsp;Installation Instruction for ProfIC Vario 7 Anion</h4><ul><li>Manual</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/AB_379_2_1d0cb4a2d3.pdf">Full PDF for download</a></li></ul>The ProfIC Vario 7 Anion is a Professional IC Vario system with Inline Dilution and Inline Dialysis for the fully automatic determination of anions with sequential suppression in very high concentrations in matrices containing emulsions. This system enables users to dilute the sample and eliminate droplets of fat or organic solvents or particles prior to the analysis.

News from LabRulezLCMS Library - Week 2, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 13th January 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you applications by Thermo Fisher Scientific, Shimadzu, a presentation by Agilent Technologies, a manual by Metrohm, and a poster from ASMS by Waters Corporation!<h4>1. Thermo Fisher Scientific: High-resolution DIA proteomics workflow for single-cell samples on the Orbitrap Astral mass spectrometer</h4><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/paper/28638">Full PDF for download</a></li></ul>Assess proteome coverage and sample throughput performance for single-cell samples using a library-free and library-based data-independent acquisition (DIA) method on the Thermo Scientific™ Orbitrap™ Astral™ mass spectrometer.<h5>Introduction</h5>In recent years, there has been a shift to analyzing smaller sample quantities, driven by the interest in profiling the proteome of individual cells. This increased focus on LC-MS analysis of limited sample amounts, e.g., single cells, requires the highest possible sensitivity. At the same time, throughput and chromatographic performance must be preserved to generate sufficiently high-quality data from large data sets to draw meaningful conclusions. This trend toward analyzing smaller sample quantities reflects the need to understand the heterogeneous nature of biology through the dissection of complex systems into their individual parts or, specifically, individual cells. Traditional proteomics approaches read out the average of a sample while single-cell proteomics provides insights into the exact nature of each of the components in such samples.The Orbitrap Astral mass spectrometer delivers a new standard for single-cell samples with deeper proteome coverage and faster throughput. It enables these capabilities through the synchronized acquisition of high-resolution and high-dynamic range full scan spectra with the Thermo Scientific™ Orbitrap™ mass analyzer and high speed and sensitivity MS/MS spectra with the Thermo Scientific™ Astral™ mass analyzer. The Thermo Scientific™ Vanquish™ Neo UHPLC system delivers maximum performance in terms of precise, low flow rates and gradient formation, as well as low injection volumes—an important benefit for single-cell proteomics and limited sample amounts.The Thermo Scientific™ μPAC™ Neo HPLC columns with novel micro-pillar array deliver highly reproducible chromatographic separation and increased sensitivity with maximum resolution. The Thermo Scientific™ FAIMS Pro Duo interface enhances sensitivity by removing background signals.In this technical note, we present a single-cell proteomics workflow (Figure 1). To first evaluate sensitivity and quantitative precision and accuracy and linearity of the workflow, a dilution series from 5 ng to 50 pg of the Thermo Scientific™ Pierce™ HeLa protein digest standard was analyzed.<h4>2. Shimadzu: Automatic Optimization of Gradient Conditions by AI Algorithm - Consecutive Optimization at Different Column Oven Temperatures</h4><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.cz/paper/28642">Full PDF for download</a></li></ul><h5>User Benefits</h5><ul><li>The AI algorithm of LabSolutions MD can automatically optimize gradient conditions to greatly reduce labor of LC method development.</li><li>Gradient conditions are automatically optimized at different column oven temperatures consecutively.</li><li>Automatic optimization of gradient conditions can be applied not only to new method development, but also to existing method to efficiently improve resolution.</li></ul><h5>Introduction</h5>In the typical LC method development, the process begins with “preparation” which includes mobile phase preparation, column installation, and creation of analysis schedules, then the analysis is started. After that, the acquired data is analyzed and “preparation” for the subsequent analysis is carried out, followed by starting the next analysis again. The method development progresses by repeating these processes, but in addition to the significant time required to repeatedly create analysis schedules, expertise in chromatography is necessary to explore optimal conditions based on data analysis. In other words, typical method development requires “human intervention”. Therefore, eliminating human involvement and automating such method development processes would be desirable to improve labor efficiency. This article introduces an approach for automatically optimizing gradient conditions at different column oven temperatures consecutively, identifying the combination of temperature and gradient conditions that meet the resolution criteria.<h5>Conclusion</h5>Automatic optimization of gradient conditions using AI algorithm of LabSolutions MD was applied to a model sample (mixture of seven compounds of small molecule) at different column oven temperatures. As a result, the temperature and gradient conditions that met the resolution criteria were successfully explored. In method development, human intervention, such as analysis batch creation and data analysis, is required to optimize gradient conditions. LabSolutions MD can provide significant labor savings in this area. For more information on LabSolutions MD, please refer to the Technical Report <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/c190_e284_1ca86b48ea/c190-e284.pdf">“Efficient Method Development Based on Analytical Quality by Design with LabSolutions MD Software (C190-E284)”</a>.<h4>3. Agilent Technologies: Optimize Your Polymer Analysis by Selecting the Ideal GPC/SEC Column</h4><ul><li>Presentation</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/paper/28578">Full PDF for download</a></li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/4481">Recorded webinar</a></li></ul>&nbsp;<ul><li>GPC/SEC Separation Mechanism</li><li>Conventional GPC/SEC Workflow</li><li>Considerations for GPC/SEC Column Selection (Key questions to ask)<ul><li>What polymer are you analysing?</li><li>Which solvent (or solvents) is your polymer soluble in?</li><li>What is the expected molecular weight range of your polymer?</li><li>What is the requirement for your analysis or what would you like to improve about your existing GPC/SEC separation?<ul><li>Resolution is important</li><li>Reproducibility of sample chromatography and results</li><li>Speed of analysis or sample throughput is something to improve on</li></ul></li></ul></li><li>Further considerations<ul><li>Know the properties of the sample</li><li>Be familiar with the properties of the columns being considered</li><li>It is important to balance polarities for the sample, solvent, and column packing</li></ul></li><li>Common Column Chemistries for GPC/SEC</li><li>Agilent Magic Triangles</li><li>Column Selection: Porosity</li><li>Individual Pore Versus MultiPorous Particle</li><li>Column Selection: Particle size</li><li>Columns for Low Polarity Organic Eluents</li><li>Columns for Medium Polarity Organic Eluents</li><li>Columns for High Temperature GPC/SEC</li><li>Columns for Fluorinated Organic Eluents</li><li>Columns for Aqueous Eluents: Neutral or weak Anions</li><li>Columns for Aqueous Eluents: Polycations and Strong Polyanions</li><li>Column Selection: Additional Considerations</li><li>Columns in Series</li><li>Wrongly Coupled Columns</li><li>Combination of Individual Pore Size Columns</li><li>Column Selection and Importance of Solvent Choice</li><li>Solvent Selection</li><li>Successful Solvent Choice</li><li>Eluent Modification in Organic GPC</li><li>Common Questions Around GPC/SEC Standards</li><li>Agilent Polymer Calibration Standard Offerings</li><li>Well Characterized Polymer Standards</li><li>Easivial Certificate of Analysis</li><li>Common Questions Around SEC Standards</li><li>Installation and Care of Your Column</li><li>Before Your Analysis</li><li>Column Selection – Additional considerations</li><li>System Tubing</li><li>Your GPC/SEC Toolbox</li></ul><h4>4. Metrohm: Installation Instruction for ProfIC Vario 7 Cation</h4><ul><li>Manual</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.cz/paper/28584">Full PDF for download</a></li></ul>The ProfIC Vario 7 Cation is a Professional IC Vario system with Inline Dilution and Inline Dialysis for the fully automatic determination of cations in high concentrations in matrices containing emulsions. This system enables users to dilute the sample and eliminate droplets of fat or organic solvents or particles prior to the analysis.<h4>5. Waters Corporation: IMPROVED TISSUE HOMOGENIZATION AND SPE-BASED SAMPLE PREPARATIONS FOR THE QUANTITATIVE LC-MS ANALYSIS OF OLIGONUCLEOTIDE THERAPEUTICS</h4><ul><li>Poster/ASMS</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/paper/27580">Full PDF for download</a></li></ul>Efficient extraction of drug analytes is a critical aspect of drug metabolism and pharmacokinetics (DMPK) studies. This has long applied to small molecules and still applies to the bioanalysis of oligonucleotides. Oligonucleotide drugs and their metabolites must be quantified within both biofluids and tissue samples. The newest of oligonucleotide drugs are both extensively modified and conjugated. These modified residues and conjugate moieties can complicate extraction recovery and reproducibility. In this work, we report several key insights on how to achieve improved extractions. Protocols for solvent-assisted proteinase K sample pre-treatments are investigated using a weak anion exchange (WAX) microplate-based solid phase extraction (SPE) device. Direct injection LC-MS quantitation is demonstrated for all three antisense oligonucleotides (ASOs).<h5>CONCLUSIONS</h5><ul><li>Selective extraction and elution of ASO oligonucleotides is feasible from multiple tissue types.</li><li>Extracted ASOs are amenable for either full scan mode analysis on benchtop small footprint TOF MS or MRM analysis by Triple Quad MS</li><li>Reproducible and repeatable data were collected even without the application of an internal standard</li><li>One novel aspect of the SPE eluate is that no further sample preparation is required for subsequent LC-MS analysis saving time and avoiding sample losses during drying and reconstitution</li><li>Eluted nucleic acid components can be readily analyzed by regular ion-pairing reversed phase chromatography and UV/MS-based detection and quantitation</li><li>This robust tissue extraction protocols for improved LC-MS based bioanalysis of ASO drugs was repeatable and highly reproducible across multiple batches of SPE sorbent, providing confidence in the suitability of the optimized protocols</li></ul>

News from LabRulezLCMS Library - Week 3, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 20th January 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you tech. notes by Shimadzu, and applications by Agilent Technologies, Thermo Fisher Scientific, Metrohm, and Waters Corporation!<h4>1. Shimadzu: Importance of Vial Selection in LC and LC/MS Analysis: Effects on Analysis of Alkaline Metals from Glass</h4><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/paper/28641">Full PDF for download</a></li></ul>In recent years, the sensitivity of mass spectrometers and other detectors has improved, enabling trace sample analysis. In LC and LC/MS analyses of trace compounds, vial selection is very important. Certain vial materials can cause unintentional compound adsorption, reducing analytical sensitivity. For instance, polypropylene (PP) vials often adsorb hydrophobic compounds on their surfaces, while glass vials minimize hydrophobic adsorption but may exhibit surface ionic adsorption of silanol bases and basic compounds due to metallic ion interactions. Additionally, the elution of sodium and other alkali metals from glass surfaces can influence analytical outcomes. To address these issues Shimadzu has developed Shim-vial™, a specially treated vial designed to minimize sodium (Na) elution. Comparative studies demonstrated that Shim-vials exhibit significantly lower Na elution levels than conventional vials. Furthermore, results showed a direct correlation between higher Na elution and increased adsorption of basic compounds, suggesting that metallic ions play a key role in this adsorption phenomenon.<h5>Summary</h5>It is evident that reducing Na in glass vials limits adsorption of basic compounds. Further, in LC/MS analysis, analytes become Na adducts due to the presence of Na ions, which has an impact on the sensitivity at the original m/z as well. Because adsorption and the production of Na adducts are so noticeable in the analysis of low concentration compounds, there are likely cases where the results obtained differ from the actual results, without anyone noticing. To prevent such issues, the use of high quality, low adsorption vials is recommended. The Shim-vial H/S series feature very low Na elution amounts due to a special treatment, enabling their use as vials that provide stable analysis results for both basic and acidic compounds.&nbsp;<h4>2.&nbsp;Agilent Technologies: Analysis of 764 Pesticides in Tomato Using an Agilent 6495D Triple Quadrupole LC/MS System</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/paper/28647">Full PDF for download</a></li></ul>Pesticide residue workflow for determination of 764 pesticides in tomato QuEChERS extract<h5>Abstract</h5>A comprehensive LC/MS/MS method for 764 pesticides in QuEChERS tomato raw extract was established using an Agilent 6495D triple quadrupole LC/MS system. With 4th-generation iFunnel technology and novel inlet design, the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?instrumentationItems=31&amp;mainauthorItems=10&amp;search=6495d">6495D LC/TQ system</a> delivers ultimate sensitivity with high precision at sub-millisecond dwell times, without compromising robustness, for the most difficult analytes in complex food matrices. The iFunnel can uniquely be tuned on a compound-by-compound basis for optimal transmission of all analytes in an assay for wide-scope multiresidue pesticide analysis that includes fragile compounds. Speed of acquisition and duty cycle are enhanced with the latest onboard computing, enabling 150% more concurrent dynamic multiple reaction monitoring (dMRM) for extended large-panel assays as well as shortened run times. The 6495D also provides excellent linearity and allows for easy method transfer from previous LC/TQ models. These improvements make it a robust and reliable option for performing routine trace analysis in the most demanding production environments. Overall, the 6495D LC/TQ is a significant upgrade in terms of performance and usability for pesticide analysis.<h5>Conclusions</h5>This study demonstrates the performance of an Agilent 6495D triple quadrupole LC/MS system with an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=Infinity+III">Agilent 1290 Infinity III LC</a> for the analysis of 764 pesticides in tomato QuEChERS raw extract. Enhanced onboard computing enables increased acquisition speed and up to 150% more concurrent dMRMs for extended large-panel assays and shortened run times. With 4th-generation iFunnel technology and tunable settings, users can now select the best iFunnel setting for each compound transition to achieve optimal sensitivity. Good linearity was observed for all 764 target analytes, with R2 ≥ 0.99 for the calibration range 0.1 to 100 μg/L.<h4>3.&nbsp;Thermo Fisher Scientific: Unveiling hidden protein depths: a high-throughput plasma proteomics workflow for enhanced biomarker discovery</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/paper/28546">Full PDF for download</a></li></ul>To develop robust plasma proteomics workflows with different sample preparation and various throughput methods for deep plasma proteomics and superior quantitation by a label-free data-independent acquisition (DIA) strategy on the latest <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/836">Thermo Scientific™ Orbitrap™ Astral™ mass spectrometer</a>.<h5>Introduction</h5>Cancer continues to claim countless lives and holds the second-highest ranking in overall mortality worldwide. The late diagnosis of this disease frequently leads to a poor prognosis, emphasizing the crucial need for improved early detection tools. Present diagnostic tests either lack sensitivity or require invasive biopsies and are not always feasible or comfortable for patients.One of the significant advantages of plasma proteomics is the ease of sample collection through routine blood draws. The analysis of blood plasma for cancer biomarkers presents a promising avenue for early detection, but the complexity of the associated workflows has hindered progress in this area.1The analysis of plasma presents a substantial challenge due to the vast concentration range of proteins in blood plasma. Detecting low abundant proteins, which hold potential as biomarkers, proves challenging as they are often greatly overshadowed by high-abundant proteins. In fact, approximately 99% of the plasma proteome is composed of proteins such as albumin, globulins, and coagulants, effectively overshadowing potentially less abundant protein biomarkers. Therefore, there is a pressing need to develop methods that can accurately identify and quantify these low-abundant proteins in plasma samples.Mass spectrometery-based proteomic analysis, in conjunction with advanced separation technology, is a leading method for studying low-abundant proteins due to its sensitivity, unambiguous peptide identification, and accurate quantitation. The cutting-edge Orbitrap Astral mass spectrometer offers unprecedented sensitivity and reproducibility for low-abundant proteins, which enables deeper plasma proteome coverage and facilitates the discovery of potential biomarkers.<h5>Conclusions</h5>Neat plasma workflows, while easy to handle due to minimal sample preparation, suffer from dynamic range issues, which result in shallow coverage of the plasma proteome compared to enriched or depleted plasma workflows.The use of High Select Depletion Spin Columns for plasma depletion has proven to significantly increase proteome coverage. Compared to neat plasma, proteome coverage is enhanced by 2- to 3-fold. This method provides an economical workflow and is a viable alternative to other depletion strategies used in plasma proteomics research.The Seer Proteograph XT workflow coupled with the Orbitrap Astral mass spectrometer offers the most comprehensive depth of analysis, effectively balancing the need for high-throughput automated workflows with high quantitative precision. Taken together, these workflows with the Orbitrap Astral mass spectrometer enable new possibilities for biomarker discovery from large cohort plasma proteomics studies.<h4>4.&nbsp;Metrohm: Water quality testing with EPA 300.1</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/paper/28651">Full PDF for download</a></li></ul>Boost lab efficiency with automated eluent generation and single-run analysis of anions and disinfection byproductsStandard analytical methods like U.S. EPA Method 300.1 (Parts A and B), ISO 10304-1, and ISO 10304-4 ensure compliance when monitoring water contaminants that affect human health. Disinfection byproducts (DBPs) in particular are linked to cancer and reproductive issues [1–5]. EPA 300.1 Part A and ISO 10304-1 outline the analytical requirements for ion chromatographic determination of major inorganic anions. Harmful DBPs (chlorite and chlorate) are included in ISO 10304-4 and EPA 300.1 Part B (plus bromate and dichloroacetic acid / DCAA). Achieving method detection limits (MDLs) for analytes with significant relative concentration differences can be challenging. The Metrosep A Supp 21 high-capacity anion-exchange column for hydroxide eluents and sequentially suppressed conductivity detection allows for a single-run analysis that meets these needs. <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=220&amp;search=948+Continuous+IC">The 948 Continuous IC Module</a>, CEP automates KOH eluent generation. This eliminates manual preparation and ensures stable retention times along with an ultra-low baseline. Along with a single-standard calibration, this analytical approach provides a highly efficient, sustainable, reliable solution for water testing labs.<h5>CONCLUSIONS</h5>This application focuses on separating and measuring high concentrations of inorganic anions, (e.g., chloride, nitrate, and sulfate) along with lower concentrations of disinfection byproducts (DBPs, i.e., bromate, chlorite, and chlorate) and nitrite and bromide in a single analysis run using ion chromatography. Accurate measurement across a wide concentration range requires a detector with high linearity, such as the IC Conductivity Detector MB (linearity range of 0–15,000 μS/cm), a high-capacity column (<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=220&amp;search=Metrosep+A+Supp+21">Metrosep A Supp 21</a>) for appropriate peak separation, and a low baseline with outstanding signal-to-noise ratio to reach the lowest detection limits.The 948 Continuous IC Module, CEP, in combination with the suppressor designed for hydroxide eluents (MSM-HC Rotor A, Hydroxide), guarantees the best analytical conditions – a high purity eluent, low baseline, and best signal-to-noise ratios. The automatic, almost reagent-free hydroxide eluent production out of a high-purity concentrate (4 mol/L potassium hydroxide solution, Supelco, Merck) and easy, straightforward gradient generation eliminates any manual steps and associated human errors. This provides stable elution conditions, resulting in stable retention times, and is a sustainable, cost-efficient solution for any lab.The Metrosep A Supp 21 column, designed for hydroxide eluents, enables a high resolution of all analytes required in U.S. EPA Method 300.1 Parts A and B as well as in ISO 10304-1 and ISO 10304-4. Originally, these standards intended for the analysis to be performed with two separate methods to determine the highly concentrated standard anions beside the trace anions accurately. Indeed, many methods lack an appropriate resolution and sufficient sensitivity, and two separate methods are necessary for the analyses, dramatically reducing the sample throughput.Metrohm offers a very comprehensive way to combine the two parts of EPA 300.1 without any quality losses by using a setup with the Metrosep A Supp 21 - 250/4.0 separation column in combination with automatic high-purity hydroxide eluent generation and conductivity detection after sequential suppression and automatic inline calibration.With this efficient setup, water laboratories can fulfill regular drinking water standards and increase their overall work efficiency. All-in-all, this is a complete, robust, and efficient solution.<h4>5.&nbsp;Waters Corporation: A Rapid and Comprehensive UHPLC-MS/MS Clinical Toxicology Research Method for the Analysis of Benzodiazepines in Urine</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/paper/28654">Full PDF for download</a></li></ul>This application note describes a clinical toxicology research method for the solid phase extraction and UHPLC-MS/MS analysis of traditional and designer benzodiazepines for clinical and forensic toxicological analysis. Benzodiazepines are widely prescribed and have high rates of abuse.1 The emergence of new designer benzodiazepines has increased concerns of this abuse, as they are initially not controlled and have unknown health risks.2The described research method includes a simplified sample preparation procedure that reduces the number of manual steps, produces high recoveries, consistent matrix effects, and accurate and precise quantitative data. The use of the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=5&amp;search=BEH+C18+">ACQUITY™ UPLC™ BEH™ C18</a> Column results in rapid analysis of a panel of 26 benzodiazepine compounds, while maintaining all required baseline separations for accurate quantification. This combination of sample preparation, UHPLC separation, and MS/MS detection optimizes the workflow and results in a rapid, method for quantification of traditional and designer benzodiazepines.<h5>Benefits</h5>A Rapid and Comprehensive UHPLC-MS/MS Clinical Toxicology Research Method for the Analysis of Benzodiazepines in Urine<ul><li>Rapid, simplified sample preparation protocol resulting in efficient and consistent recovery for all analytes</li><li>All sample pretreatment and extraction performed in-well, eliminating transfer steps</li><li>UHPLC-MS/MS analysis results in excellent separation of 26 benzodiazepines in four minutes</li></ul><h5>Conclusion</h5>This application note describes a comprehensive clinical toxicology research method for the solid phase extraction and UHPLC-MS/MS analysis of a panel of 26 traditional and designer benzodiazepines, which has a number of advantages. The sample preparation method efficiently extracted all compounds included in the panel. The use of the ACQUITY UPLC BEH C18 Column results in rapid analysis (4 minutes) of a large panel of benzodiazepines. The <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?instrumentationItems=31&amp;mainauthorItems=5&amp;search=TQ-S">Xevo TQ-S micro Mass Spectrometer</a> ensures rapid and accurate quantitation of all compounds analyzed over a wide dynamic range. The combination of sample preparation method, UHPLC separation and MS/MS detections results in a rapid, accurate and precise method for the comprehensive analysis of benzodiazepines in urine, including new designer benzodiazepines.

News from LabRulezLCMS Library - Week 4, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 3rd February 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you tech. note by Agilent Technologies, applications by Shimadzu, Thermo Fisher Scientific, Metrohm, and Poster by Waters Corporation!<h4>1. Simultaneous Determination of Five Genotoxic Aryl Sulfonate Impurities in Pharmaceuticals by LCMS-2050</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_03_lcms_053_en_befdf50f8c.pdf">Full PDF for download</a></li></ul><h5>User Benefit</h5><ul><li>A novel method for determining the content of five genotoxic aromatic sulfonate impurities in drugs was established by using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=2050">LCMS-2050 single quadrupole mass spectrometer</a>.</li><li>The pretreatment of this method was simple, and it had a wide linear range and a high accuracy rate.</li></ul><h5>Introduction</h5>Genotoxic impurities (GTIs) refer to substances that directly or indirectly damage cellular DNA, generating gene mutations or in vivo mutagenesis. GITs may can cause damage to human genetic material at extremely low concentrations, which in turn leads to gene mutations and promotes the occurrence of tumors. Because of the potential risks of GITs, it is essential to monitor any potentially existing genotoxic impurities in active pharmaceutical ingredients or medicinal products.In the pharmaceutical industry, when drug active ingredients exist in the forms of alkyl sulfonates, benzenesulfonates, p-toluenesulfonates, and hydroxyethyl sulfonates or sulfonic acid reagents are utilized in the drug synthesis process, sulfonate esters are regarded as potential GTIs. GTIs of sulfonate esters can be classified as alkyl sulfonate esters and aryl sulfonate esters based on different substituents.Previously, relevant literature has reported quantitative detection methods for some GTIs of sulfonate esters, such as GC-MS, GC-FID, LC-MS/MS, and complex derivatization treatment of samples might be necessary. In this study, LC-MS was mainly utilized for the quantitative analysis of five GTIs of aryl sulfonate esters. This method features simple pretreatment and high accuracy, which can offer a reference for the detection of genotoxic impurities of aryl sulfonate esters in drugs.<h5>Conclusion</h5>A novel method for determining the content of five genotoxic impurity aryl sulfonates in drugs was established by using the LCMS-2050. Within the concentration range of 5 - 500 μg/L, the correlation coefficients of the five genotoxic impurity aryl sulfonates were all greater than 0.994. When a mixed standard solution of three concentrations was added to the drugs, the recovery rates of each component ranged from 110.5% to 115.3%. This method features simple pretreatment, excellent specificity and high sensitivity, and can provide a reference for the determination of the content of five genotoxic impurities aryl sulfonates in drugs.<h4>2.&nbsp;Method Transfer from an Agilent 1100 Series Quaternary LC to an Agilent 1260 Infinity III LC</h4><ul><li>Technical Overview</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/te_method_transfer_equivalency_1100_series_1260_infinity_iii_5994_8031en_agilent_1_b429e7bd87.pdf">Full PDF for download</a></li></ul>Proof of equivalency for the transfer of conventional LC methodsMethod transfer from legacy equipment to new instruments, such as the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1260+Infinity+III">Agilent 1260 Infinity III LC</a>, is an important topic for all laboratories throughout different industries. Seamless method transfer ensures that the same methods can still be used, which ensures business continuity and reduced regulatory and financial risks.This technical overview demonstrates method transfer from an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1100">Agilent 1100 Series Quaternary LC</a> to an Agilent 1260 Infinity III LC for conventional LC methods covering diverse gradient conditions. Equivalent results are obtained, which proves that seamless method transfer can be expected for typical, robust, conventional LC methods. In terms of retention time precision, the 1260 Infinity III LC outperforms the 1100 LC, leading to higher trust in the data.<h5>Introduction</h5>Method transfer is an important topic for all laboratories throughout different industries, where HPLC methods are transferred between departments and locations as well as between different LC instruments.1 For validated methods in the pharmaceutical industry, method transferability is compulsory.Method transfer, or the transfer of analytical procedures from one laboratory to another in the pharmaceutical industry requires a documented process that requires comparative testing.2 One example for instrument-to-instrument method transfer is the transfer of conventional LC methods from legacy equipment to new instruments such as a 1260 Infinity III LC.This technical overview demonstrates method transfer from a 1100 Series Quaternary LC to a 1260 Infinity III LC for conventional LC methods. Several methods were chosen that cover diverse gradient conditions including challenging conditions such as a shallow gradient and a gradient starting at a composition extreme. This should prove that equivalent results are obtained when transferring methods from a broad application space of conventional LC methods from the 1100 Series Quaternary LC to the 1260 Infinity III LC.ConclusionThe transfer of conventional LC methods covering diverse gradient conditions from an Agilent 1100 Series Quaternary LC to an Agilent 1260 Infinity III LC leads to equivalent results, thereby proving that seamless method transfer can be expected for typical, robust, conventional LC methods. In terms of retention time precision, the 1260 Infinity III LC outperforms the 1100 LC, leading to a higher trust in the data.<h4>3.&nbsp;Development of Separation Methods for GLP-1 Synthetic Peptides Utilizing a Systematic Protocol and MaxPeak High Performance Surface Technology</h4><ul><li>Poster / HPLC Symposium</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/2024_hplc_bengtson_glp1_synthetic_peptides_7d92bb96e7.pdf">Full PDF for download</a></li></ul>Peptides offer higher specificity than small molecules, and low immunogenicity which makes them excellent candidates for new medications. Specifically synthetic peptides produced through solid phase peptide synthesis allow for more control with more predictable impurities with a relatively low manufacturing cost.An excellent example of upcoming synthetic peptide drugs is Glucagon-Like Peptide-1 Agonists (GLP-1s) which are prescribed for the treatment and management of obesity and type-II diabetes1. Recently, GLP-1 drugs such as semaglutide, have boomed in popularity as a weight management treatment after success in clinical trials.2 Given the prevalence of GLP-1s, it is important that the quality control for this class of pharmaceuticals is supported by versatile, sensitive, and reproducible chromatography methods.Here we address these needs and developed a single HLPC-UV/MS method for the analysis of a variety of GLP-1s. The experiment was based around a systematic protocol which was key in helping to identify high-risk factors and to shorten the method development time. Beyond this <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=5&amp;search=MaxPeak+HPS">MaxPeak high performance (HPS)</a> technology was used to improve chromatographic performance.<h5>Conslusion</h5>The thoughought assessment of the risk before conduction the development of a separation method allowed for the ccreation of a more quality method while reducing time. Asessing the high risk variables showed ther benefit in MaxPeak HPS technology when working with these compounds. MaxPeak HPS technology<h4>4.&nbsp;Quantifying impurities in cationic lipids raw materials with the inverse gradient method using LC-CAD-MS</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003384_pb_cationic_lipids_isq_lc_cad_ms_an003384_na_en_d3a34737de.pdf">Full PDF for download</a></li></ul><h5>Application benefits</h5><ul><li>Enable the quantification of impurities even in the absence of specific reference standards</li><li>Use a single quadrupole mass spectrometer to match impurities based on their retention time and molecular masses</li><li>Use an inverse gradient with <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=3&amp;search=Charged+Aerosol+CAD">Charged Aerosol Detector (CAD)</a> to enable accurate surrogate quantitation when there is large difference in retention times between the lipid standard and its impurities, even in the absence of impurity standards</li><li>Confirm the unit mass of both the lipid standard and its associated impurities using the correlation of CAD and <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=3&amp;search=ISQ">ISQ channels</a></li></ul><h5>Goal</h5><ul><li>Provide instructions, methodologies, and recommended techniques to improve quantification of impurities in cationic lipid components</li><li>Use the Thermo Scientific™ Vanquish™ Flex Inverse Gradient UHPLC System coupled to a Thermo Scientific™ Vanquish™ Charged Aerosol Detetor to provide more accurate estimated quantitation of cationic lipid impurities without the need for reference standards</li></ul><h5>Conclusion</h5>In this study, we have developed an inverse gradient quantification method for cationic lipids impurity analysis when impurity reference standards are not available. For further identification of lipid impurities, <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_002455_bt_lc_cad_hram_ms_lipid_nanoparticle_an002455_na_en_2c6a86ecac/an-002455-bt-lc-cad-hram-ms-lipid-nanoparticle-an002455-na-en.pdf">Application Note 002455</a> can be referenced.<ul><li>The impurity amount can be automatically estimated using another peak or peak group within the same run for this surrogate quantitation in Chromeleon CDS.</li><li>Both inverse gradient configuration and method can be automatically generated via the wizard.</li><li>When there is a significant difference in retention times between the lipid standard and its impurities, using an inverse gradient provides more accurate estimated quantitation than a conventional gradient method.</li><li>The use of the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=3&amp;search=ISQ">ISQ EM MS</a> in conjunction with CAD allowed for confirmation of the m/z of the lipid raw material as well as determination of the m/z for the unknown impurities.</li></ul><h4>5.&nbsp;Using a portable standalone system for easy fermentation monitoring</h4><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_ec_035_download_f48491e484.pdf">Full PDF for download</a></li></ul>In-situ measurements of lactic acid in beer using screen-printed electrodes (SPEs)Lactic acid (2-hydroxypropanoic acid) is primarily found in sour dairy products. In beer, the presence of lactic acid contributes to its acidity and lactic aromas, and usually appears as the result of fermentation with lactic acid bacteria. These bacteria may be purposely introduced to the wort, or they can also appear as a result of an infection.Although lactic acid is essential in beer up to a certain amount, in excess it is considered a defect. Its perception threshold is 0.0044 mol/L. However, in some lambic-type beers, the lactic acid concentration can reach levels higher than 0.0333 mol/L.In this Application Note, an enzymatic sensor based on a screen-printed electrode is used to measure lactic acid in commercial beers as a proof of concept for its potential application during fermentation monitoring.ConclusionIn this study, an electrochemical biosensor for the detection of lactic acid in beer is proposed. The sample with the electrochemical method proposed only needs to be diluted 1:10 with a solution of 0.1 mol/L Tris-NO3 at pH 7.2. Using a simple amperometric assay, it is possible in 75 s to measure the amount of lactic acid in a beer sample without any pretreatment. Measurements obtained are similar to those taken with a traditional L-Lactate Assay kit and non-portable optical devices

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