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Peak Shapes and Their Measurements: The Need and the Concept Behind Total Peak Shape AnalysisGaussian peak shapes in chromatography are indicative of a well-behaved system. Such peak shapes are highly desirable from the perspective of column packing technology. From an analyst’s point of view, Gaussian peaks provide improved sensitivity (lower detection limits) and allow ease of quantitation. In practice, one can obtain peaks that tail, front, or concurrently front and tail for reasons such as column packing issues, chemical and kinetic effects, and suboptimal high performance liquid chromatography (HPLC) system plumbing and detector settings. Here, we discuss a number of approaches for peak shape measurement that are available in modern chromatography software, along with their advantages and drawbacks. A new “total peak shape analysis” approach is suggested that facilitates detection and quantification of concurrent fronting and tailing in peaks. Several remediation approaches are proposed that can help chromatographers analyze and improve peak shapes.
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The Question of Chromatographic Integration in Data IntegrityThe topic of chromatographic integration and data interpretation raises a lot of questions about data integrity. Is it acceptable to integrate data? What are the limits?
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The Role of Mass Spectrometry in Biopharmaceutical Drug Discovery and DevelopmentThe discovery and development of biopharmaceuticals that target specific diseases can be transformative for people living with illness. However, bringing a new therapy to market is a prolonged and costly process mired in uncertainty. Ensuring safety, efficacy, and product quality is paramount. Biopharmaceuticals, by their nature, are highly complex. A myriad of heterogeneity can be intentionally functional, an unwanted consequence of manufacturing and storage, or generated by biological modification in vivo. Not all, but some post-translational modifications or biotransformations can impact development, manufacturing, safety, efficacy, and overall product quality. These critical quality attributes (CQAs) need to be identified, characterized, controlled, and monitored throughout the drug discovery and development cycle. Specialty measurement using mass spectrometry (MS) continues to play an ever‑increasing role across the continuum.
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Efficient Quantitation of Biotherapeutics in Biological Matrices Through the Application of LC–MS‑Related TechniquesBiotherapeutics must endure in-depth testing to validate their efficacy and safety before their release to the medical community. Characterization and quantitation of these large molecule medicines is traditionally performed with ligand binding assays or radiolabeling procedures. Issues with selectivity, accuracy, and unavailability of applicable assays for the characterization and quantitation of certain biotherapeutics means that liquid chromatography–mass spectrometry (LC–MS) is becoming an increasingly selected method for biotherapeutics testing. Typically used for small molecules, LC–MS can be adapted for larger molecule analysis with additional high throughput and multiplexing capabilities. New method development has turned LC–MS into a highly sensitive option for biotherapeutics validation.
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Empower 2 Method Validation Manager Software: A Tool for Rapid Method ValidationMethod validation is a demanding activity. It requires a large investment in personnel, materials, instruments, supervision, and, most of all, time.
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A Look at Matrix EffectsIn the environmental analytical chemistry literature, the topic of matrix interferences and matrix effects has not been addressed in a fundamental way. Here, we examine which methods appear to have a tendency for matrix interference and suggest ways to reduce the problem.
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Biolayer Interferometry as an Alternative to HPLC for Measuring Product Concentration in Fermentation BrothSeveral key applications of biolayer interferometry in pharmaceutical development have emerged recently. Here, we evaluate its use for easuring product titer from fermentation, and compare the strengths and weaknesses of the technique to those of HPLC.
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Recent Advances in Comprehensive Chromatographic Analysis of Emerging DrugsThis article discusses the use of emerging technologies that are complementary to established techniques, to significantly reduce these shortcomings for both synthetic cannabinoids and synthetic cathinones. In this vein, the utility of recently reported approaches including ultrahigh performance supercritical fluid chromatography (UHPSFC)–photodiode array (PDA) ultraviolet (UV)–MS, and GC–vacuum UV is discussed. To increase the specificity of analysis, multiple chromatographic techniques are commonly used. For the analysis of emerging drugs, a combination of GC and UHPSFC is recommended. The utility of a previously unreported coupled-columns approach for UHPSFC to significantly enhance resolution of synthetic cathinones is presented.
Latest:
Recent Advances in Comprehensive Chromatographic Analysis of Emerging DrugsThis article discusses the use of emerging technologies that are complementary to established techniques, to significantly reduce these shortcomings for both synthetic cannabinoids and synthetic cathinones. In this vein, the utility of recently reported approaches including ultrahigh performance supercritical fluid chromatography (UHPSFC)–photodiode array (PDA) ultraviolet (UV)–MS, and GC–vacuum UV is discussed. To increase the specificity of analysis, multiple chromatographic techniques are commonly used. For the analysis of emerging drugs, a combination of GC and UHPSFC is recommended. The utility of a previously unreported coupled-columns approach for UHPSFC to significantly enhance resolution of synthetic cathinones is presented.
Latest:
Recent Advances in Comprehensive Chromatographic Analysis of Emerging DrugsThis article discusses the use of emerging technologies that are complementary to established techniques, to significantly reduce these shortcomings for both synthetic cannabinoids and synthetic cathinones. In this vein, the utility of recently reported approaches including ultrahigh performance supercritical fluid chromatography (UHPSFC)–photodiode array (PDA) ultraviolet (UV)–MS, and GC–vacuum UV is discussed. To increase the specificity of analysis, multiple chromatographic techniques are commonly used. For the analysis of emerging drugs, a combination of GC and UHPSFC is recommended. The utility of a previously unreported coupled-columns approach for UHPSFC to significantly enhance resolution of synthetic cathinones is presented.
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Ultra-Fast Separations of Pharmaceutical Compounds with 10 mm Columns Packed with Sub-2 µm ParticlesVery short columns filled with 1.9 µm particles were evaluated for the ultra-fast analysis of pharmaceutical formulations. Local anæsthetic, mydriatic and anti-hypertensive agents were chosen as analytes and a method was developed and validated for each of these substances, according to ICH guidelines. Excellent quantitative performance was obtained using an optimized chromatographic system that reduces the importance of extra-column effects and cuts the analysis time to less than 15 s.
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Photodegradation and Photstability Studies of Bendroflumethiazide in Pharmaceutical Formulations and Urine Samples by Micellar Liquid ChromatographyA simple HPLC procedure is described for the determination of bendroflumethiazide (BMFT) in pharmaceutical formulations and urine samples. No interferences from common additives or other drugs frequently administered with BMFT or from endogenous compounds in urine samples were found. The lack of an organic solvent in the mobile phase reduces the risk of environmental contamination and human toxicity.
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Analysis of Omeprazole and Lansoprazole in Capsules by Capillary Zone ElectrophoresisA simple capillary zone electrophoresis method is discussed for the simultaneous analysis of omeprazole and lansoprazole. The aim is to provide an efficient assay for the quality control of both pharmaceuticals.
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Visual Presentation of Data by Means of Box PlotsThe authors explain how to construct box plots and how they can help you to learn more about your data.
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Analysis of Omeprazole and Lansoprazole in Capsules by Capillary Zone ElectrophoresisA simple capillary zone electrophoresis method is discussed for the simultaneous analysis of omeprazole and lansoprazole. The aim is to provide an efficient assay for the quality control of both pharmaceuticals.
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Accelerated and Automated Extraction of Hexavalent Chromium from Solid Waste Materials Coupled with Ion Chromatography DeterminationIn this article, the authors describe a method based on the accelerated and automated extraction of hexavalent chromium from solid samples followed by ion chromatography analysis using spectrophotometric detection. The experiments were performed on different samples of sludge and soil.
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Accelerated and Automated Extraction of Hexavalent Chromium from Solid Waste Materials Coupled with Ion Chromatography DeterminationIn this article, the authors describe a method based on the accelerated and automated extraction of hexavalent chromium from solid samples followed by ion chromatography analysis using spectrophotometric detection. The experiments were performed on different samples of sludge and soil.
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Visual Presentation of Data by Means of Box PlotsThe authors explain how to construct box plots and how they can help you to learn more about your data.
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CDS and LIMS IntegrationIn this article, Jo Webber tackles the problem of ensuring data integrity in pharmaceutical manufacturing. She shows how, by using modern technology and well integrated systems, quality can be improved.
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Preparative Chiral SFC as a Green Technology for Rapid Access to Enantiopurity in Pharmaceutical Process ResearchThis month’s column provides an overview of green chemistry issues relating to preparative chiral SFC chromatography in support of preclinical development in the pharmaceutical industry.
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Preparative Chiral SFC as a Green Technology for Rapid Access to Enantiopurity in Pharmaceutical Process ResearchThis month’s column provides an overview of green chemistry issues relating to preparative chiral SFC chromatography in support of preclinical development in the pharmaceutical industry.
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Separating Proteins by pI-Values — Can 2D LC Replace 2D GE?The authors address the specific separation problems of proteins and assess whether 2D liquid chromatography could possibly be considered as an alternative to traditional 2D gel electrophoresis in the future.
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Preparative Chiral SFC as a Green Technology for Rapid Access to Enantiopurity in Pharmaceutical Process ResearchThis month’s column provides an overview of green chemistry issues relating to preparative chiral SFC chromatography in support of preclinical development in the pharmaceutical industry.
Latest:
Accelerated and Automated Extraction of Hexavalent Chromium from Solid Waste Materials Coupled with Ion Chromatography DeterminationIn this article, the authors describe a method based on the accelerated and automated extraction of hexavalent chromium from solid samples followed by ion chromatography analysis using spectrophotometric detection. The experiments were performed on different samples of sludge and soil.
Latest:
Separating Proteins by pI-Values — Can 2D LC Replace 2D GE?The authors address the specific separation problems of proteins and assess whether 2D liquid chromatography could possibly be considered as an alternative to traditional 2D gel electrophoresis in the future.
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PeakMaster — A Freeware Simulator of Capillary Zone ElectrophoresisThe authors describe how this free downloadable software calculates and displays CZE separations after the user has entered sample and operations parameters. The underlying principles and mathematical basis are explained.
Latest:
PeakMaster — A Freeware Simulator of Capillary Zone ElectrophoresisThe authors describe how this free downloadable software calculates and displays CZE separations after the user has entered sample and operations parameters. The underlying principles and mathematical basis are explained.
