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Enantiomeric Separation of Privileged Scaffold Derivatives in Early Drug Discovery Using Chiral SFCSuccessful therapeutic intervention often requires chiral medicines because of the intrinsic chirality of protein drug targets, which consist of L-amino acids. Potency, efficacy, and safety can be highly dependent on the precise stereochemical geometry of the molecules. Determining the biological profile of individual enantiomers in the early stages of drug discovery is important for successful optimization towards clinical candidates. Here we demonstrate the benefits of supercritical fluid chromatography (SFC) with three chiral stationary phases exemplified by high frequency resolution of 41 out of 50 chiral derivatives of eight commonly used drug discovery scaffolds including 1,3-thiazoles, 1,3-benzothiazoles, pyranoquinolones, indoles, and leucolines.
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Liquid Chromatography–Time-of-Flight Mass Spectrometry for Cannabinoid Profiling and Quantitation in Hemp Oil ExtractsA primary impediment to cannabinoid research is the fact that materials possessing psychoactive Δ-9-tetrathydrocannabinol are considered Schedule I drugs as defined in the U.S. Controlled Substances Act. An alternative source of cannabinoids may be found in hemp oil extracts. Hemp contains a low percentage of Δ-9-tetrathydrocannabinol (THC) by weight but relatively high amounts of non-psychoactive cannabinoids. The liquid chromatography-time of flight mass spectrometry (LC-TOF) method presented herein allows for the accurate, precise and robust speciation, profiling and quantification of cannabinoids in hemp oil extracts and commercial cannabinoid products for research and development laboratories. The method was determined to chromatographically separate 11 cannabinoids including differentiation of Δ-8-tetrahdrocannabinol and THC with excellent linear dynamic range, specificity and sensitivity.
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Testing the Limits of Ion Mobility Mass Spectrometry to Compare a Nonbiological Complex Drug Product and Purported Generics—A Case Study with CopaxoneThe analysis of oil samples containing many thousands of constituents best illustrates the benefits of ion mobility MS for complex samples. Here, we test the limits of ion mobility MS to discern differences between batches of Copaxone, a highly complex drug containing billions of peptides, and various purported generic versions of the drug.
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Comparison of Extracts from Dry and Alcohol-Steamed Root of Polygonatum kingianum (Huang Jing) by Sub-2-µm–LC–TOF-MSMost plants used in traditional Chinese medicine must be processed before their medicinal usage; hence the effective ingredients may differ from those in the freshly harvested plant extracts. In this work, we present a fast and generic approach using sub-2-?m liquid chromatography–time-of-flight–mass spectrometry (sub-2-?m-LC–TOF-MS) coupled with multivariate statistical data analysis to systematically profile ingredient changes between fresh and processed samples of huang jing.
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Analysis of PFAS in Locally Acquired Food ContainersThe combination of an untargeted approach using ultrahigh pressure liquid chromatography–quadrupole time-of-flight mass spectrometry (UHPLC–QTOF) and a targeted approach using UHPLC–tandem mass spectrometry (MS/MS) are presented as an ideal method for detecting per- and polyfluroalkyl substances (PFAS) in fast-food packaging.
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Analysis of PFAS in Locally Acquired Food ContainersThe combination of an untargeted approach using ultrahigh pressure liquid chromatography–quadrupole time-of-flight mass spectrometry (UHPLC–QTOF) and a targeted approach using UHPLC–tandem mass spectrometry (MS/MS) are presented as an ideal method for detecting per- and polyfluroalkyl substances (PFAS) in fast-food packaging.
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45th International Symposium on High Performance Liquid Phase Separations and Related Techniques (HPLC 2017) PreviewA preview of HPLC 2017, which will be held from 18 to 22 June 2017 at the Prague Congress Centre, Prague, Czech Republic.
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Detection of Novel “Designer Drugs” Using Full-Scan GC–HRAMNovel psychoactive substances pose a major challenge for forensic toxicology and drug-seizure laboratories because of the scale and speed at which these new “designer drugs” are entering the market. To keep pace with the threat, laboratories require robust full-scan detection techniques capable of both targeted drug screening and the identification of unexpected compounds too. Here, a full-scan gas chromatography (GC) coupled to high-resolution accurate mass (HRAM) approach for the profiling of known and unknown drugs of abuse is presented.
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High Performance Liquid Chromatography Analysis of Cinnamon from Different OriginQuantifying the content of coumarin and cinnamaldehyde in cinnamon products
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Considerations on Switching from Helium to HydrogenThe authors explain the operational considerations for switching from helium to hydrogen in the separations lab, as well as discussing options.
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Novel C18 Stationary Phase Provides Exceptional Results for Metabolite ProfilingMetabolomics, the study of small molecule metabolites that are found within a biological sample, is an emerging field of study. Progress in this field depends upon technological advancement in the fields of LC–MS and separation technology.
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Affinity Capillary Electrophoresis— A Powerful Tool to Investigate Biomolecular InteractionsIn the biomedical research of molecular bases of both normal and pathological biological processes, it is currently necessary not only to detect, identify, and quantify individual compounds, but also to study their interactions with endo- and exogenous compounds. Obviously, for these purposes it is crucial to develop new advanced high‑performance analytical methods providing high sensitivity, high selectivity, and high throughput. These challenging requirements are well met by capillary electromigration (CE) methods. They have developed in the last three and half decades into high‑performance separation techniques suitable for the analysis of a wide spectrum of both low- and high‑molecular mass bioactive compounds.
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Analysis of Amphetamines and Synthetic Cathinones in Hair Samples Using LC–Tandem Mass Spectrometry and Solid-Phase ExtractionAn efficient method for forensic analysis of amphetamines and synthetic cathinones - the illicit drugs often called "bath salts" - in hair samples.
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The Benefits of Coupling Miniaturized Comprehensive 2D LC with Hybrid High-Resolution Mass SpectrometryComprehensive two-dimensional liquid chromatography (LC×LC) is evolving and becoming more commonly used in practice, but there are some specific problems still present that hamper the widespread use of this technology. One key aspect is the coupling of an on-line LC×LC system to a mass spectrometer. Generally, on-line LC×LC is based on a very fast second dimension separation to achieve low cycle times. This often results in flow rates that are far above the optimum for electrospray ionization mass spectrometry (ESI-MS). This month’s “Multidimensional Matters” looks at the benefits of miniaturization in the first and second dimension for coupling with a high-resolution mass spectrometer (HRMS) and describes an environmental analysis application.
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Recent Advances and Applications of Passive Sampling DevicesPassive samplers come in many forms and can be used in various fields. Here, we review multiple advances made to this sampling strategy.
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Advances in Chromatography for Charge Variant Profiling of BiopharmaceuticalsBiotherapeutic proteins, such as monoclonal antibodies (mAbs), are heterogeneous and exist as variant mixtures of structurally similar molecules. The heterogeneity of monoclonal antibodies is revealed by charge-sensitive methods, such as ion exchange chromatography (IEX). Changes in charge profile can significantly impact the structure, stability, binding affinity, and efficacy of the biotherapeutic drug. It is therefore necessary to understand the profile of the drug so that variants are identified and controlled. This article describes advances in ion exchange column chemistries, elution buffers, and ultrahigh-pressure liquid chromatography (UHPLC) instruments to meet the needs for modern, robust analysis of charge variants in monoclonal antibodies and therapeutic proteins.
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High-Throughput Structure-Based Profiling and Annotation of FlavonoidsA novel mass spectrometry-based flavonoid profiling workflow is applied to characterize and structurally annotate a large number of unknown flavonoids in fruit juice and vegetable juice samples.
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Host Cell Protein Analysis Using Mass SpectrometryAn increasing number of drugs coming onto the market are proteins rather than small molecules. A major portion of these are produced using a host cell system. Host cells express many of their own proteins that can easily contaminate the recombinant protein drug. Traditionally, these host cell proteins (HCPs) have been measured using immunoassays, but recently, orthogonal analytical methods, particularly mass spectrometry (MS), have started to be used. This article considers some of the current methods for HCP detection, with a focus on MS.
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Host Cell Protein Analysis Using Mass SpectrometryAn increasing number of drugs coming onto the market are proteins rather than small molecules. A major portion of these are produced using a host cell system. Host cells express many of their own proteins that can easily contaminate the recombinant protein drug. Traditionally, these host cell proteins (HCPs) have been measured using immunoassays, but recently, orthogonal analytical methods, particularly mass spectrometry (MS), have started to be used. This article considers some of the current methods for HCP detection, with a focus on MS.
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A Generic Workflow for Achiral SFC Purification of Complex Pharmaceutical MixturesThis process can improve efficiency in a drug discovery laboratory.
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Improving the Efficiency of Fatty Acid Methyl Ester Preparation Using Automated Sample Preparation TechniquesAn automated technique for esterifying fatty acids in canola oil compares favorably with a manual method.
