<p><strong>The Preliminary Program is available below.</strong></p>
<ul>
<li><a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/15mdcw_guidebook_final_99c11401e3/15mdcw_guidebook_final.pdf"><strong>15th MDCW 2024 - Guidebook</strong></a></li>
<li><a href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/abstract_book_15mdcw_final_010224_3d8a7b7258/abstract_book_15mdcw_final-010224.pdf"><strong>15th MDCW 2024 - Abstract book</strong></a></li>
</ul>
<p>The Guidebook and the Abstract book can be downloaded when available. The Guidebook contains the program and all other pertinent conference information.</p>
<blockquote>
<p><strong>Historical content from the workshop can be found on YouTube via the LabRulez platform: <a href="https://www.youtube.com/playlist?list=PLg-M6fM-05MrGrDggkl_UKzzcHPWPmssh"> 14 MDCW Content (LabRulez)</a></strong></p>
</blockquote>
<p><strong>Thank you to our sponsors for making this event possible</strong>. It is your generous support that enriches the conference program and allows us to operate the conference with <strong>free registration for all attendees</strong>.</p>
<p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/MDCW_Sponzors_and_Partners_15th_Multidimensional_Chromatography_Workshop_MDCW_2024_b46a541625/MDCW-Sponzors-and-Partners-15th-Multidimensional-Chromatography-Workshop-(MDCW)-2024.jpg" alt="MDCW: Sponzors &amp; Partners: 15th Multidimensional Chromatography Workshop (MDCW) 2024"/></p>
<blockquote>
<h3><strong>Sponsors 2024</strong></h3>
<ul>
<li><strong>SepSolve Analytical</strong></li>
<li><a href="https://gcms.labrulez.com/library?instrumentationItems=2&amp;manufacturerItems=24"><strong>JEOL</strong></a></li>
<li><a href="https://gcms.labrulez.com/library?instrumentationItems=2&amp;manufacturerItems=25"><strong>LECO</strong></a></li>
<li><a href="https://gcms.labrulez.com/library?mainauthorItems=41&amp;search=GC+image"><strong>GC Image</strong></a></li>
<li><strong>SpectralWorks</strong></li>
<li><a href="https://gcms.labrulez.com/library?instrumentationItems=2&amp;manufacturerItems=9"><strong>Restek</strong></a></li>
<li><strong>NSF CREST CATSUS</strong></li>
<li><strong>OFFICE OF RESEARCH, SCHOLARSHIP AND CREATIVE ACTIVITIES</strong> (CAL STATE LA)</li>
<li><strong>SIKAND SITI CENTER</strong> (CAL STATE LA)</li>
<li><a href="https://gcms.labrulez.com/library?mainauthorItems=3"><strong>Thermo Fisher Scientific</strong></a></li>
<li><a href="https://gcms.labrulez.com/library?mainauthorItems=40"><strong>Trajan Scientific</strong></a></li>
<li><strong>Vici</strong></li>
<li><strong>Chemistry matters</strong></li>
</ul>
<h4><strong>MEDIA PARTNERS 2024</strong></h4>
<ul>
<li><strong>The Analytical Scientist</strong></li>
<li><a href="https://gcms.labrulez.com/"><strong>LabRulezGCMS</strong></a></li>
<li><a href="https://lcms.labrulez.com/"><strong>LabRulezLCMS</strong></a></li>
<li><strong>LCGC</strong></li>
</ul>
</blockquote>
<h3><strong>Preliminary Program</strong></h3>
<h4><strong>WEDNESDAY January 10, 2024</strong></h4>
<h5><strong>8:30 - 9:00 AM</strong> Registration</h5>
<h5><strong>9:00 - 9:30 AM Opening Remarks</strong></h5>
<h5><strong>9:30 - 10:00 AM KL-1 - From research to routine analysis - the role of GC×GC in the regulatory space</strong></h5>
<ul>
<li>Sarah Prebihalo</li>
</ul>
<h5><strong>10:00 - 10:30 AM KL-2 - Two-dimensional liquid chromatography for small molecule pharmaceutical analysis – more knowledge in less time</strong></h5>
<ul>
<li>Qinggang Wang</li>
</ul>
<h5><strong>10:30 - 11:00 AM</strong> Coffee Break</h5>
<h5><strong>11:00 - 11:20 AM O-1 - Applications of multi-dimensional liquid chromatography in modern day pharmaceuticals</strong></h5>
<ul>
<li>CJ Venkatramani</li>
</ul>
<h5><strong>11:20 - 11:40 AM O-2 - Essential separations: analysis of aroma oils by one-dimensional and two-dimensional gas chromatography and mass spectrometry</strong></h5>
<ul>
<li>Robert Cody</li>
</ul>
<h5><strong>11:40 - 12:00 PM O-3 - Developing a breath test to diagnose valley fever, an endemic fungal pneumonia</strong></h5>
<ul>
<li>Emily Higgins</li>
</ul>
<h5><strong>12:00 - 1:30 PM</strong> Lunch (<strong>Sponsored by JEOL</strong>)</h5>
<h5><strong>1:30 - 1:50 PM O-4 - Sampling body odor for healthcare monitoring: how to avoid the pitfalls of individual&#39;s odor variations and contaminations by the sampling environment</strong></h5>
<ul>
<li>Elsa Boudard</li>
</ul>
<h5><strong>1:50 - 2:10 PM O-5 - A holistic view of river water quality using passive sampling and GC×GC–TOFMS</strong></h5>
<ul>
<li>Matthew Edwards</li>
</ul>
<h5><strong>2:10 - 2:30 PM O-6 - Non-target screening and contaminant profiling of house dust collected across Europe by comprehensive two-dimensional gas chromatography - mass spectrometry and multi-variate statistical evaluation</strong></h5>
<ul>
<li>Peter Haglund</li>
</ul>
<h5><strong>2:30 - 2:50 PM O-7 - Chemical characterization of the aircraft cabin environment utilizing GC×GC-TOFMS and hard and soft ionization</strong></h5>
<ul>
<li>Kevin Hayes</li>
</ul>
<h5><strong>2:50 - 4:00 PM</strong> Coffee Break and Poster session</h5>
<h5><strong>4:00 - 5:30 PM Guided Discussion 1 - Advantages and Limitations of GC×GC in Government and Industrial Laboratories</strong></h5>
<h5><strong>6:30 PM Networking Event (Food sponsored by Chemistry Matters Inc)</strong></h5>
<h4><strong>THURSDAY January 11, 2024</strong></h4>
<h5><strong>8:30 - 9:00 AM</strong> Registration</h5>
<h5><strong>9:00 - 9:30 AM Opening Remarks</strong></h5>
<h5><strong>9:30 – 10:00 AM KL-3 - On-line multi-dimensional LC/MS: the next-generation tool for real-time monitoring of antibody quality attributes in biopharmaceutical processes</strong></h5>
<ul>
<li>Tomas Bouvarel</li>
</ul>
<h5><strong>10:00 - 10:30 AM KL-4 - From wildfire origins to courtroom verdicts: Exploring arson investigations with multi-dimensional chromatography</strong></h5>
<ul>
<li>Gwen O&#39;Sullivan</li>
</ul>
<h5><strong>10:30 - 11:00 AM</strong> Coffee Break (<strong>Sponsored by SepSolve Analytical</strong>)</h5>
<h5><strong>11:00 - 11:20 AM O-8 - Don’t let the reality of GC×GC-MS data burst your bubble! Or how the &amp;@$#%^&amp; am I supposed to manage all these bits and bytes?!?</strong>*</h5>
<ul>
<li>James Harynuk</li>
</ul>
<h5><strong>11:20 - 11:40 AM O-9 - Streamlining group type analysis with standard GC×GC templates through computer vision-assisted alignment</strong></h5>
<ul>
<li>Daniel Geschwender</li>
</ul>
<h5><strong>11:40 - 12:00 PM O-10 - Chromatographic and statistical workflows for GC×GC-MS data processing</strong></h5>
<ul>
<li>Scott Campbell</li>
</ul>
<h5><strong>12:00 - 1:30 PM</strong> Lunch (<strong>Sponsored by Cal State LA’s California Forensic Science Institute</strong>)</h5>
<h5><strong>1:30 - 1:50 PM 0-11 - Off-line LC×SFC-HRMS/MS method for the non-target analysis of depolymerised lignin</strong></h5>
<ul>
<li>Eliise Tammekivi</li>
</ul>
<h5><strong>1:50 - 2:10 PM 0-12 - Using two-dimensional gas chromatography for determining biogenic components in renewable transportation fuel blends</strong></h5>
<ul>
<li>Rafal Gieleciak</li>
</ul>
<h5><strong>2:10 - 2:30 PM 0-13 - Alkene quantification in plastic waste-derived alternative fuels using GC×GC-FID</strong></h5>
<ul>
<li>Genesis Barzallo</li>
</ul>
<h5><strong>2:30 - 2:50 PM 0-14 - Characterization and quantitative hydrocarbon group-type analysis of plastic-derived pyrolysis oils by GC×GC-TOFMS/FID</strong></h5>
<ul>
<li>Christina Kelly</li>
</ul>
<h5><strong>2:50 – 3:00 - Cutting the ribbon: A visit inside the LECO Complex Chemical Composition Analysis Laboratory</strong></h5>
<ul>
<li>Petr Vozka</li>
</ul>
<h5><strong>3:00 - 4:00 PM</strong> Coffee Break and Poster Session</h5>
<h5><strong>4:00 - 5:30 PM Guided Discussion 2 - Standard Reference Test Mixture for Comprehensive Two-Dimensional Gas Chromatography</strong></h5>
<h5><strong>6:00 PM Wine Tasting Event (Sponsored by LECO)</strong></h5>
<h4><strong>FRIDAY January 12, 2024</strong></h4>
<h5><strong>8:30 - 9:00 AM</strong> Registration</h5>
<h5><strong>9:00 - 9:10 AM Opening Remarks</strong></h5>
<h5><strong>9:10 - 9:40 AM O-15 Robert Synovec - Expanding the scope of tile-based GC×GC–TOFMS data analysis</strong></h5>
<h5><strong>9:40 - 10:10 AM O-16 - Workflow democratization of comprehensive two-dimensional gas chromatography – high-resolution time-of-flight mass spectrometry data</strong></h5>
<ul>
<li>Michael Sorochan Armstrong</li>
</ul>
<h5><strong>10:10 - 10:45 AM</strong> Coffee &amp; Brunch</h5>
<h5><strong>10:45 - 11:05 AM O-17 - Investigating sensory-classified roasted arabica coffee with GC×GC-TOFMS and chemometrics to understand potato taste defect</strong></h5>
<ul>
<li>Caitlin Cain</li>
</ul>
<h5><strong>11:05 - 11:25 AM O-18 - Exploring the cup of coffee using GC×GC-MS combined with multiple combination of headspace extractions</strong></h5>
<ul>
<li>Michael Wilde</li>
</ul>
<h5><strong>11:25 - 11:45 AM O-19 - Advancing fingerprint deposition modeling through the integration of comprehensive two-dimensional gas chromatography and time-of-flight mass spectrometry for age estimation</strong></h5>
<ul>
<li>Elena Mosham</li>
</ul>
<h5><strong>11:45 - 12:00</strong> AM Break</h5>
<h5><strong>12:00 - 12:20 PM O-20 Cai Huamin - Direct flow modulation method for comprehensive two-dimensional gas chromatography</strong></h5>
<ul>
<li>Cai Huamin</li>
</ul>
<h5><strong>12:20 - 12:40 PM O-21 - LC×SFC valve technologies: guidelines towards a successful online modulation</strong></h5>
<ul>
<li>Margaux Sanchez</li>
</ul>
<h5><strong>12:40 - 1:00 PM O-22 - Extending analyte boiling point range using thinner film porous layer open tubular columns paired with GC×GC-MS</strong></h5>
<ul>
<li>Lina Mikaliunaite</li>
</ul>
<h5><strong>1:00 - 1:20 PM O-23 - Introducing automated online multicolumn two-dimensional liquid chromatography screening as a rapid and efficient tool for method development of multiple pipeline modalities</strong></h5>
<ul>
<li>Heather Wang</li>
</ul>
<h5><strong>1:20 – 1:40 PM</strong> Closing</h5>
<h5><strong>1:40 PM Food Truck Farewell</strong></h5>
<h3><strong>POSTER LIST</strong></h3>
<h5><strong>P-1 Development of a fisher ratio contrast metric for simultaneous discovery of compounds indicating either molding kinetics or bean geographical region in moisture damaged cocoa beans</strong></h5>
<ul>
<li>Lina Mikaliunaite</li>
</ul>
<h5><strong>P-2 Multi-omics workflow for blood serum screening using GC×GC-TOFMS</strong></h5>
<ul>
<li>Pierre-Hugues Stefanuto</li>
</ul>
<h5><strong>P-3 From data to decisions: using novel software tools for automated pairwise comparison of GC×GC data</strong></h5>
<ul>
<li>Matthew Edwards</li>
</ul>
<h5><strong>P-4 Assessment of exhaled breath voc stability on TENAX® GR thermal desorption tubes</strong></h5>
<ul>
<li>Trenton Davis</li>
</ul>
<h5><strong>P-5 Characterization and comparison of fresh and dried herbs with GC, GC×GC, and TOFMS</strong></h5>
<ul>
<li>Elizabeth Humston-Fulmer</li>
</ul>
<h5><strong>P-6 Comparison of new and used vacuum pump oil using two-dimensional gas chromatography and high-resolution time-of-flight mass spectrometry</strong></h5>
<ul>
<li>Kirk Jensen</li>
</ul>
<h5><strong>P-7 Non-targeted analysis of environmental samples using comprehensive gas chromatography (GC×GC-) with high-resolution time-of-flight mass spectrometry (HRTOFMS)</strong></h5>
<ul>
<li>David Alonso</li>
</ul>
<h5><strong>P-8 Identifying putative volatile biomarkers for S. aureus methicillin-resistant and small-colony variant subtypes</strong></h5>
<ul>
<li>Daniela Gutierrez-Munoz</li>
</ul>
<h5><strong>P-9 Automated QC pooling by thermal desorption tube recollection of gaseous mixtures for metabolomic studies</strong></h5>
<ul>
<li>Allison Ferranti</li>
</ul>
<h5><strong>P-10 Identifying the primary sources of variance in a breath biomarker experiment</strong></h5>
<ul>
<li>Darakshan Zabin</li>
</ul>
<h5><strong>P-11 A feasibility study of sample recollection in the analysis of selected volatile organic compounds in breath samples using GC×GC-ToFMS</strong></h5>
<ul>
<li>Nina Nouribakikomarolya</li>
</ul>
<h5><strong>P-12 Development and application of a web-based simulator for two-dimensional liquid chromatography separations</strong></h5>
<ul>
<li>Dwight Stoll</li>
</ul>
<h5><strong>P-13 Flow modulated GC×GC in combination with atmospheric pressure mass spectroscopy using the SICRIT ionization source</strong></h5>
<ul>
<li>Taylor Hayward</li>
</ul>
<h5><strong>P-14 Comparison of diesel samples measured by using GC×GC-HRTOFMS</strong></h5>
<ul>
<li>John Dane</li>
</ul>
<h5><strong>P-15 Optimization of headspace solid-phase microextraction of bronchoalveolar lavage samples from people with cystic fibrosis and method evaluation</strong></h5>
<ul>
<li>Antao Gao</li>
</ul>
<p><em>The poster list will be updated with last minute posters.</em></p>
<h4><strong>Keynote Speakers 2024</strong></h4>
<p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/MDCW_Keynote_Speakers_2024_Dr_Gwen_O_Sullivan_Dr_Sarah_Prebihalo_Dr_Qinggang_Wang_Dr_Thomas_Bouvarel_1d428b3bb9/MDCW-Keynote-Speakers-2024-Dr.-Gwen-O'Sullivan-Dr.-Sarah-Prebihalo-Dr.-Qinggang-Wang-Dr.-Thomas-Bouvarel.jpg" alt="MDCW: Keynote Speakers 2024: Dr. Gwen O&#39;Sullivan, Dr. Sarah Prebihalo, Dr. Qinggang Wang, Dr. Thomas Bouvarel"/></p>
<h5><strong>Dr. Gwen O&#39;Sullivan</strong></h5>
<ul>
<li>Professor &amp; Vice Dean Research &amp; Scholarship, Mount Royal University</li>
</ul>
<p><strong>Title of Keynote Lecture: From Wildfire Origins to Courtroom Verdicts: Exploring Arson Investigations with Multidimensional Chromatography</strong></p>
<p>Gwen is an environmental chemist specializing in Environmental Forensics, particularly in wildfire forensics, arson investigation, air monitoring, and risk assessment. She combines analytical chemistry and environmental science to study the origins and behavior of pollutants and their environmental impacts.  Over the course of her career, in industry, consultancy, and academia, Gwen has developed technical expertise in the areas of wildfire forensics, environmental chemistry, environmental forensics, air quality, and contaminated land and groundwater. She has worked environmental forensic investigations involving compounds of concerns including ignitable liquids, drilling fluids, petroleum hydrocarbons, polycyclic aromatic hydrocarbons, polychlorinated biphenlys, polychlorinated dibenso-p-dioxins and dibenzofurans, methane, and nitrates. She has also authored numerous scientific articles, edited book series, and successfully competed for research grants both nationally and internationally.​</p>
<h5><strong>Dr. Sarah Prebihalo</strong></h5>
<ul>
<li>Chemist, U.S. Food and Drug Administration</li>
</ul>
<p><strong>Title of Keynote Lecture: From research to routine analysis - The role of GC×GC in the regulatory space</strong></p>
<p>​​​Sarah Prebihalo is a Chemist at the U.S. Food and Drug Administration in Maryland as a part of the Office of Regulatory Science at the Center for Food Safety and Applied Nutrition (CFSAN). Sarah worked as a laboratory technician at Procter and Gamble for 2 years after obtaining her Bachelor’s in Chemistry, before moving to Pennsylvania to obtain her Masters in Forensic Chemistry at Penn State. In 2015 she began working towards her PhD in Chemistry at the University of Washington in Seattle, which she obtained in 2020. After completing a 2 year postdoctoral fellowship at the U.S. Food and Drug Administration, she transitioned to her current role as Chemist and is involved in non-targeted method development for foods and dietary supplements using GC×GC. ​</p>
<h5><strong>Dr. Qinggang Wang</strong></h5>
<ul>
<li>Scientific Director, Chemical Process Development, Bristol Myers Squibb</li>
</ul>
<p><strong>Title of Keynote Lecture: Two-dimensional liquid chromatography for small molecule pharmaceutical analysis – more knowledge in less time</strong></p>
<p>​​​Qinggang Wang, Ph.D., is a Scientific Director in Chemical Process Development in Bristol-Myers Squibb Company.  He received his B.S. in Chemistry and Ph. D. in Analytical Chemistry from Tsinghua University, Beijing, China.  His work has been focused on CMC analytical supports for various projects within BMS portfolio, inclding small molecules, synthetic peptides and oligonuleotides.  He has authored or co-authored 18 peer-reviewed publications and three book chapters in analytical science. His research focuses on application of novel analytical techniques to pharmaceutical analysis.  He is the recipient of BMS BMSIARC award for outstanding achievement in analytical science in 2019.</p>
<h5><strong>Dr. Thomas Bouvarel</strong></h5>
<ul>
<li>Senior Scientist, Department of Analytical Protein Chemistry, Genentech</li>
</ul>
<p><strong>Title of Keynote Lecture: On-line Multi-Dimensional LC/MS: The Next-Generation Tool for Real-Time Monitoring of Antibody Quality Attributes in Biopharmaceutical Processes</strong></p>
<p>Thomas Bouvarel is currently Senior Scientist in the Department of Analytical Protein Chemistry at Genentech (a member of Roche group) in South San Francisco, California. He received his Ph.D. in analytical chemistry from Sorbonne University, France. After completing a postdoctoral fellowship at the University of Geneva, Switzerland, he joined Genentech. His research involves the development and implementation of novel multi-dimensional liquid chromatography methodologies for the characterization and on-line monitoring of biomacromolecules.</p>
<h3><strong>Guided Discussion Groups 2024</strong></h3>
<h5><strong>Advantages and Limitations of GC×GC in Government and Industrial Laboratories</strong></h5>
<ul>
<li>Haleigh Boswell (Chevron Technology Center)</li>
<li>Sarah Prebihalo (U.S. Food and Drug Administration)</li>
</ul>
<p>​Comprehensive gas chromatography (GC×GC) is a common technique used in government and industrial laboratories; however, it has struggled to gain widespread acceptance due to perceived complexity and a lack of standardized and validated methods. Furthermore, the technique is not directly comparable to historical data sets and previously used analytical techniques. Overcoming these challenges and limitations in non-academic laboratories is a critical aspect of research by experts and advanced GC×GC users. Advanced users must be vocal advocates, highlighting the advantages of GC×GC in cases where the additional separation data can be advantageous. By addressing the benefits and limitations of this technique, this discussion will aim to address how we may elevate GC×GC in industrial and government laboratories, including, but not limited to, the role of obtaining employment in these sectors, allowing for further integration into the GC×GC community.</p>
<h5><strong>Preliminary Results in the Development of a System Performance Standard Reference Test Mixture for Comprehensive Two-Dimensional Gas Chromatography</strong></h5>
<ul>
<li>Jean-Marie D. Dimandja (FDA/ORA)</li>
<li>Pierre-Hugues Stefanuto (University of Liege)</li>
</ul>
<p>GC×GC system performance is influenced by many parameters, including modulator type, column set, detection method, and data processing software. This discussion will be focused on the development of a standard test mixture that can be used to compare GC×GC system performance across instruments and laboratories.</p>


15th MDCW 2024 (Preliminary Program)

<p><strong>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!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you applications, presentations, and posters by <strong>Metrohm,</strong> <strong>Thermo Fisher Scientific,</strong> <strong>Shimadzu, Waters Corporation,</strong> and <strong>Agilent Technologies</strong>!</p><h4><strong>1. Agilent Technologies: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/why_use_hilic_and_hic_chromatography_oct082024_51637eb877.pdf"><strong>Why Use HILIC and HIC Chromatography?</strong></a></h4><ul><li>Presentation</li></ul><h5><strong>Agenda</strong></h5><ul><li><strong>What is HILIC and when should you consider it?</strong></li><li><strong>How to approach HILIC method development</strong><ul><li>Agilent HILIC column options</li><li>Mobile phase considerations</li></ul></li><li><strong>Common HILIC application areas</strong></li><li><strong>Tips and tricks for successful HILIC column use and care</strong><ul><li>Column equilibration</li><li>Sample solvent compatibility</li><li>Inert HILIC solution for metal-sensitive compounds</li></ul></li><li><strong>What is HIC and its separation mechanism?</strong></li><li><strong>Requirements for HIC</strong><ul><li>Factors affecting selectivity</li></ul></li><li><strong>Common HIC application areas</strong><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><strong>Summary</strong></h5><p><strong>When to consider a HILIC column:</strong></p><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><p><strong>Keep the sample solvent in mind for HILIC analyses:</strong> prepare the sample in as much acetonitrile as possible, and keep injection volumes as small as possible.</p><ul><li>Most common support issue with HILIC methods</li></ul><h4><strong>2. Shimadzu: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_06_saip_lc_077_en_e0b92b59d4.pdf"><strong>Simultaneous Quantitation of 32 PFAS in Baby Food by LC-MS/MS</strong></a></h4><ul><li>Application</li></ul><p><strong>User Benefits</strong></p><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><p><strong>Introduction</strong></p><p>PFAS (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.</p><p>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.</p><p>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).</p><p><strong>Conclusion</strong></p><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><strong>3. Thermo Fisher Scientific / </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/170"><strong>RAFA</strong></a><strong>: </strong><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"><strong>PFAS analysis strategy story – direct injection, DLLME, LC-MS/MS, LC- Orbitrap / GC-Orbitrap</strong></a></h4><ul><li>Poster / <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/170"><strong>RAFA</strong></a></li></ul><h5><strong>Abstract</strong></h5><p><strong>Purpose:</strong> 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<br>analyzer is a critical consideration.</p><p><strong>Methods: </strong>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.</p><p><strong>Results: </strong>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<br>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.</p><h5><strong>Conclusions</strong></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><strong>4. Waters Corporation / </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/303"><strong>HPLC</strong></a><strong>: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/2024_hplc_zabala_cortecs_solid_core_scalability_3ffe31ac22.pdf"><strong>SCALABILITY OF SOLID-CORE PARTICLES FOR CHROMATOGRAPHIC ANALYSES</strong></a></h4><ul><li>Poster / <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/303"><strong>HPLC</strong></a></li></ul><p><strong>NTRODUCTION</strong></p><p>Liquid 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.</p><p>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.</p><p>By utilizing CORTECS Columns, researchers can increase separation efficiency, achieve faster analysis times, reduced solvent waste and decreased column back<br>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.</p><p><strong>CONCLUSION</strong></p><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><strong>5. Metrohm: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_bat_015_download_c51bc5f0fe.pdf"><strong>Differential capacity analysis (DCA) for battery research with INTELLO</strong></a></h4><ul><li>Application</li></ul><p><strong>Introducing dQ/dE plots, applications, and more</strong></p><p>Differential 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.</p><p>This Application Note explores the principles and practical applications of differential capacity analysis, highlighting its role in improving battery performance.<br>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.</p><p><strong>INTRODUCTION</strong></p><p>Within 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"><strong>AN-BAT-014</strong></a> while this Application Note specifically focuses on the dQ/dE plot and what can be derived from it.</p>

News from LabRulezLCMS Library - Week 47, 2024

<p><strong>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!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you applications by <strong>Thermo Fisher Scientific,</strong> <strong>Shimadzu, Waters Corporation,</strong> and <strong>Agilent Technologies</strong>!</p><h4><strong>1. Thermo Fisher Scientific: </strong><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"><strong>Enhancing detection of hemoglobin variants in clinical research using dried blood spot and high-resolution accurate mass (HRAM) Orbitrap mass spectrometry</strong></a></h4><ul><li>Application</li></ul><p><strong>Application benefits</strong></p><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><p><strong>Goal</strong></p><p>Develop a top-down approach for hemoglobin variant detection using dried blood spots and a Thermo Scientific™ Orbitrap Exploris™ 240 mass spectrometer</p><p><strong>Introduction</strong></p><p>Hemoglobinopathies 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 <i>Channichthyidae</i>. Adult Hb consists of 96–98% Hb A (α2β2), 2.0–3.3% Hb A2 (α2δ2), and less than 1.0% Hb F (α2γ2).<sup>1</sup> 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 (β<sup>6</sup> Glu→Val)). Around 5.2% of the global population carries significant hemoglobinopathy-causing genes with more than 330,000 affected births occurring annually.<sup>2</sup></p><p>Current 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 (β<sup>6</sup> Glu→Lys) and Hb E (β<sup>26</sup> Glu→Lys)), very similar masses (i.e., &lt;1 Da difference between normal Hb, Hb C, Hb E, and Hb D-Punjab (β<sup>121</sup> 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.</p><p><strong>Conclusion</strong></p><p>This 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.</p><h4><strong>2. Shimadzu: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00758_en_25d3e480fb.pdf"><strong>MRM Based Free Fatty Acids Profiling in Human Plasma and Serum Using LC-MS/MS</strong></a></h4><ul><li>Application</li></ul><p><strong>User Benefits</strong></p><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><p><strong>Introduction</strong></p><p>Free 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 disorders<sup>1)</sup>.</p><p>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 analysis<sup>2)</sup>.</p><p>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.</p><p><strong>Conclusion</strong></p><p>Simultaneous 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%.</p><p>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.</p><h4><strong>3. Agilent Technologies: </strong><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"><strong>Determination of Limonin in Citrus Flour by Time of Flight (TOF) LC/MS</strong></a></h4><ul><li>Application</li></ul><p><strong>Abstract</strong></p><p>In 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.</p><p><strong>Introduction</strong></p><p>The 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.</p><p>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.<sup>1</sup> 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.</p><p>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.<sup>2</sup> 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.</p><p>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.<sup>3</sup> Chemically, it is a member of the class of compounds known as furanolactones. Limonin has an exact mass of 470.19406791 g/mol.<sup>4</sup> 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.</p><p><strong>Conclusion</strong></p><p>The 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.</p><h4><strong>4. Waters Corporation: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008552_en_bd88faf6b3.pdf"><strong>Metabolomics Workflow using a Xevo™ MRT Mass Spectrometer</strong></a></h4><ul><li>Application</li></ul><p><strong>Abstract</strong></p><p>We 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.</p><p><strong>Benefits</strong></p><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><p><strong>Introduction</strong></p><p>Metabolomics 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.</p><p>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.</p><p>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.<sup>1</sup> The resulting data showed significant changes in exogenous or environmental markers for each of the different volunteer lifestyles.</p><p><strong>Conclusion</strong></p><p>We 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.</p><p>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.</p>

News from LabRulezLCMS Library - Week 48, 2024

News from LabRulezLCMS Library - Week 49, 2024

Metabolomics and sensory evaluation of white asparagus ingredients in instant soups unveil important (off-)flavours

<p><strong>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!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you applications by <strong>Shimadzu</strong>,<strong> Metrohm</strong>, and<strong> &nbsp;Waters Corporation</strong>, a presentation by <strong>Agilent Technologies</strong>, and a poster from <strong>MSACL </strong>by <strong>Thermo Fisher Scientific</strong>!</p><h4><strong>1. Shimadzu: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00750_en_bee79113e7.pdf"><strong>Analysis of Per- and Polyfluoroalkyl Substances (PFAS) using Triple Quadrupole Mass Spectrometer Part 1 - Fish Fillet</strong></a></h4><ul><li>Application</li></ul><p><strong>User Benefits</strong></p><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><p><strong>Introduction</strong></p><p>Per- 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.</p><p>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.</p><p><strong>Conclusion</strong></p><p>This 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.</p><h4><strong>2. Agilent Technologies: </strong><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"><strong>Getting the Most from Your Diode Array Detector</strong></a></h4><ul><li>Presentation</li></ul><h5><strong>Agenda</strong></h5><ul><li><strong>Introduction</strong></li><li><strong>Fundamentals</strong><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><strong>Maximizing sensitivity</strong><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><strong>Spectral acquisition</strong><ul><li>Settings</li><li>Spectrum storage</li><li>Range, step, and threshold</li><li>OpenLab Resources</li></ul></li><li><strong>DAD maintenance</strong><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><strong>Troubleshooting</strong></li><li><strong>Additional Resources</strong></li></ul><h4><strong>3. Waters Corporation: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008521_en_ff59413ad8.pdf"><strong>HPLC Autosampler Performance II: Improved Injection Precision of USP Methods With the Alliance™ iS HPLC System</strong></a></h4><ul><li>Application</li></ul><p><strong>Abstract</strong></p><p>Method 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.</p><p><strong>Benefits</strong></p><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><p><strong>Introduction</strong></p><p>For 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.<sup>1</sup> This performance can be impacted by method conditions and instrument characteristics.<sup>2,3,4</sup> To ensure that acquired data is accurate and meets suitability requirements of the method, high performance is required from an autosampler.</p><p>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.<sup>1</sup> Injector draw rate is a setting typically set to a default speed that often varies with instrument vendor.<sup>4</sup> 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.</p><p>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%).</p><p><strong>Conclusion</strong></p><p>The 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.</p><p>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.</p><p>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.</p><h4><strong>4. Metrohm: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_c_198_download_6dcbc46fdf.pdf"><strong>Calcium acetate assay in calcium acetate capsules</strong></a></h4><ul><li>Application</li></ul><p><strong>Method validation according to the U.S. Pharmacopeia (USP)</strong></p><p>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].</p><p>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.</p><p><strong>SAMPLE AND SAMPLE PREPARATION</strong></p><p>The 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).</p><p>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<br>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.</p><p>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.</p><p><strong>CONCLUSION</strong></p><p>According 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.</p><h4><strong>5. Thermo Fisher Scientific / </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/294"><strong>MSACL</strong></a><strong>: </strong><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"><strong>Quantitation of a Panel of Per- and Polyfluoroalkyl Substances (PFAS) in Human Serum</strong></a></h4><ul><li>Poster (<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/294"><strong>MSACL</strong></a>)</li></ul><h5><strong>Abstract</strong></h5><p><strong>Purpose:</strong> Develop an LC-MS analytical method for quantitation of PFAS compound in human serum.</p><p><strong>Methods:</strong> 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.</p><p><strong>Results: </strong>LOQs from 0.025 to 2.5 ng/mL were reached for all compounds.</p><h5><strong>Introduction</strong></h5><p>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.</p><h5><strong>Conclusions</strong></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

<p><strong>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!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you applications by <strong>Shimadzu</strong>,<strong> Metrohm</strong>, and<strong> &nbsp;Waters Corporation</strong>, a presentation by <strong>Agilent Technologies</strong>, and a poster from <strong>MSACL </strong>by <strong>Thermo Fisher Scientific</strong>!</p><h4><strong>1. ALS Europe: Environmental Challenges of Pharmaceuticals: Persistence and Accumulation in Ecosystems</strong></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"><strong>Full PDF for download</strong></a></li></ul><p>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.</p><h5><strong>Pharmaceuticals as "New" Pesticides...</strong></h5><p>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.</p><p>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].</p><p><strong>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.</strong></p><h4><strong>2. Thermo Fisher Scientific:&nbsp;Orbitrap Astral MS Literature List: Rethink what is possible</strong></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"><strong>Full PDF for download</strong></a></li></ul><p><strong>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</strong></p><h4><strong>3. Agilent Technologies: Easy and Fast Automation of Sample Preparation</strong></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"><strong>Full PDF for download</strong></a></li></ul><p><strong>Sample preparation using injector workflows with the Agilent 1260 Infinity III Multisampler and Vialsampler.</strong></p><p>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.</p><h5><strong>The 1260 Infinity III LC comprised the following modules:</strong></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><strong>Agilent OpenLab CDS version 2.8 or later</strong></h5><h5><strong>Columns</strong></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><p>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.</p><h4><strong>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</strong></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"><strong>Full PDF for download</strong></a></li></ul><p>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.</p><p>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.</p><h5><strong>Benefits</strong></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><strong>5. Shimadzu: Rapid Screening of 501 Emerging Contaminants in Water Using Polarity-Extended Liquid Chromatography-Mass Spectrometry</strong></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"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></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><strong>Introduction</strong></h5><p>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.</p><p>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.</p><h5><strong>Conclusion</strong></h5><p>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.</p><h4><strong>6. Metrohm:&nbsp;Installation Instruction for ProfIC Vario 7 Anion</strong></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"><strong>Full PDF for download</strong></a></li></ul><p>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.</p>

News from LabRulezLCMS Library - Week 2, 2025

Synthesis and absolute configuration of cyclic synthetic cathinones derived from α-tetralone

<p><strong>This webinar series demonstrates the use of the Thermo Freestyle 1.8 SP2 QF1 software for processing LCMS product-ion mass spectra &nbsp;with the NIST 23 Mass Spectral Search Program (v.3.0). &nbsp;Spectra are easily exported from Freestyle to NIST Search for component identifications utilizing the NIST MSMS libraries and any other available user, crowd-sourced, and commercial MSMS libraries. &nbsp;Freestyle is a very convenient software package for processing data obtained with the their Orbitrap LCMS instruments. &nbsp;In one run both the MS1 and MS2 spectra are obtained in both positive and negative ion modes. &nbsp;The Diode arrary and UV channels can also be easily displayed for targeting the desired species noted in LC analyses.</strong></p><h5><strong>Handout for whole series</strong></h5><ul><li>Part 1: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Part_1_Data_Processing_My_Favorite_e29bfc0816.pdf">My Favorite Processing Mode in Freestyle</a></li><li>Part 1A: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Part_1_A_Data_Processing_Preferred_plus_Nearby_Precursors_33bc95778b.pdf">Using "Nearby Precursor" Enhanced Processing Mode in FreeStyle</a></li><li>Part 2: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Part_2_Data_Processing_Alternate_99a4b51fa6.pdf">Alternate Processing Modes in Freestyle</a></li><li>Part 3: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/part_3_improved_handout_d14f81cc32.pdf">Setup of Basic Settings in Freestyle and NIST Search</a></li><li>Part 4: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Part_4_NIST_search_type_demonstration_adb3cdc1c5.pdf">Different NIST MSMS Searches Demonstrated</a></li><li>Part 5: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Part_5_Elemental_Composition_demonstration_27e151914b.pdf">Elemental Processing within Thermo Freestyle</a></li></ul><h3><span><strong>Part 1: Data Processing for NIST MSMS Search Using Thermo Freestyle Software (My Favorite Approach)</strong></span></h3><p><span>This guide outlines my preferred method for processing data in <strong>Thermo Freestyle software</strong> for <strong>NIST MSMS searches</strong>. These steps streamline data parsing and ensure accurate mass spectral interpretation for <strong>LC-MS and MSMS analyses</strong>.</span></p><h4><span><strong>Equipment &amp; Software</strong></span></h4><ul data-spread="false"><li><span><strong>Thermo Orbitrap MSMS</strong></span></li><li><span><strong>Thermo Freestyle Software</strong></span></li><li><span><strong>NIST 2023 Tandem Library</strong></span></li></ul><h4><span><strong>Orbitrap Data One Acquisition</strong></span></h4><ul data-spread="false"><li>LC-MS and MSMS Analyses</li><li><span>Non-targeted acquisition of MSMS</span></li><li><span>Positive and Negative Mode</span></li><li><span>Photo Detector Array (PDA) and UV-VIS Analyses</span></li><li><span>Example compounds:</span><ul data-spread="false"><li><span><strong>Uvinul 3000</strong></span> <i><span>(MW 214)</span></i></li><li><span><strong>Tinuvin 234</strong></span> <i><span>(MW 447)</span></i></li></ul></li></ul><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/James_Little_NIST_2023_Tandem_Library_Great_Resource_for_Unknown_Identifications_f4fc13b103.jpg" alt="James Little: NIST 2023 Tandem Library Great Resource for Unknown Identifications" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_James_Little_NIST_2023_Tandem_Library_Great_Resource_for_Unknown_Identifications_f4fc13b103.jpg 245w," sizes="100vw" width="1384" height="854"></p><h4><span><strong>My Favorite Data Processing Workflow</strong></span></h4><ul><li>shared with me by colleague</li></ul><h5><span><strong>Step 1: Setting Up Freestyle Windows</strong></span></h5><p><span>To optimize the workspace for data processing:</span></p><ol data-spread="false"><li><span>Open <strong>three</strong> windows at the bottom of Freestyle:</span><ul data-spread="false"><li><span><strong>Top window:</strong> Positive ion MS1</span></li><li><span><strong>Second window:</strong> Negative ion MS2</span></li><li><span><strong>Bottom window:</strong> UV or PDA trace</span></li></ul></li><li><span>Save this layout in <strong>Workspace Options/Layouts</strong> to ensure automatic parsing when opening new files.</span></li><li><span>Add the <strong>Nearby Precursors</strong> feature to simplify MSMS selection (except for averaged MS spectra).</span></li></ol><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/James_Little_Step_1_Setting_Up_Freestyle_Windows_0dac4585f9.jpg" alt="James Little: Step 1 - Setting Up Freestyle Windows" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_James_Little_Step_1_Setting_Up_Freestyle_Windows_0dac4585f9.jpg 245w," sizes="100vw" width="1839" height="403"></p><h5><span><strong>Step 2: Adjusting the Window Layout</strong></span></h5><ol data-spread="false"><li><span>Use <strong>Select Filter</strong> to:</span><ul data-spread="false"><li><span>Change the top window to <strong>positive ion</strong></span></li><li><span>Change the second window to <strong>negative ion</strong></span></li><li><span>Choose <strong>PDA or UV</strong> for the bottom window</span></li></ul></li><li><span>The spectrum window will display the <strong>selected MS/MS data</strong> for further processing.</span></li></ol><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/James_Little_Step_2_Adjusting_the_Window_Layout_d18baf8c37.jpg" alt="James Little: Step 2 - Adjusting the Window Layout" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_James_Little_Step_2_Adjusting_the_Window_Layout_d18baf8c37.jpg 245w," sizes="100vw" width="1829" height="1042"></p><h5><span><strong>Step 3: Processing MSMS Data</strong></span></h5><ol data-spread="false"><li><span>Left-click in the <strong>top box</strong> for the <strong>positive ion chromatogram</strong>.</span></li><li><span>Right-click to <strong>average the spectrum</strong> in the Spectrum box.</span></li><li><span>Subtract background if necessary <strong>before averaging</strong>.</span></li><li><span>Populate the <strong>Avg Range</strong> box and select <strong>Range 1</strong>.</span></li><li><span>Go to <strong>Positive Ion Chromatogram</strong>, specify the range, and confirm.</span></li><li><span>Avoid averaging MS2 spectra when exporting to <strong>NIST search</strong>, as it will convert accurate mass to <strong>nominal mass</strong>.</span></li></ol><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/James_Little_Step_3_Processing_MSMS_Data_5a5e2b87b5.jpg" alt="James Little: Step 3 - Processing MSMS Data" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_James_Little_Step_3_Processing_MSMS_Data_5a5e2b87b5.jpg 245w," sizes="100vw" width="1878" height="1059"></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/James_Little_Step_3_Processing_MSMS_Data_1_131f4645ca.jpg" alt="James Little: Step 3 - Processing MSMS Data" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_James_Little_Step_3_Processing_MSMS_Data_1_131f4645ca.jpg 234w," sizes="100vw" width="1513" height="1011"></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/James_Little_Step_3_Processing_MSMS_Data_2_6ff9040f00.jpg" alt="James Little: Step 3 - Processing MSMS Data" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_James_Little_Step_3_Processing_MSMS_Data_2_6ff9040f00.jpg 245w," sizes="100vw" width="1738" height="1046"></p><h5><span><strong>Step 4: Selecting an MS2 Spectrum for NIST Search</strong></span></h5><ol data-spread="false"><li><span>Identify an <strong>m/z value of interest</strong> (e.g., <strong>m/z 215.0702</strong>).</span></li><li><span>Apply <strong>Chromatogram range filter</strong> to isolate the target ion.</span></li><li><span>The MS2 spectrum will replace the MS1 chromatogram in the top window.</span></li><li><span>Click on the peak of interest to generate an <strong>MS2 spectrum</strong>.</span></li><li><span>Repeat the process for <strong>Negative Ion MS2 (MSMS) spectrum</strong>.</span></li><li><span>Send spectra to <strong>NIST MS search</strong> for <strong>compound identification</strong>.</span></li></ol><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/James_Little_Step_4_Selecting_an_MS_2_Spectrum_for_NIST_Search_271afd5538.jpg" alt="James Little: Step 4 - Selecting an MS2 Spectrum for NIST Search" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_James_Little_Step_4_Selecting_an_MS_2_Spectrum_for_NIST_Search_271afd5538.jpg 245w," sizes="100vw" width="1849" height="1125"></p><h3><span><strong>Conclusion</strong></span></h3><p><span>Using this workflow, Thermo Freestyle software efficiently processes LC-MS/MS data for <strong>NIST searches</strong>, ensuring accurate identification of unknown compounds. By saving custom layouts and avoiding averaged MS2 spectra, this method maximizes precision and efficiency.</span></p>

 Data Processing for NIST MSMS Search Using Thermo Freestyle Software (My Favorite Approach)

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