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Development of an Ultrasensitive LC–MS-MS Method for Determination of 5-Fluorouracil in Mouse Plasma5-Fluorouracil (5-FU) is a low-molecular-weight anticancer drug in clinical use for several solid tumors in humans. Currently, the most widely used methodology for 5-FU quantitation is liquid chromatography–tandem mass spectrometry (LC–MS-MS) with either liquid–liquid extraction (LLE), protein precipitation, or a combination of both as sample cleanup procedures.
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Liquid Chromatography’s Complementary Role to Gas Chromatography in Cannabis TestingLiquid chromatography (LC) is proving to be a valuable complementary technique to gas chromatography (GC) in cannabis testing for the analysis of cannabinoids, mycotoxins, and pesticides.
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E-Liquid flavors by SBSE-TD-GC-MSVolatile flavor and aroma compounds are extracted and determined in e-liquids for regulatory compliance purposes using SBSE-TD-GC-MS, in an efficient solvent-free workflow.
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Radical Mass Spectrometry as a New Frontier for BioanalysisIn this article, we discuss radical MS, an increasingly important area of MS development and the application to bioanalysis. At the current stage, most of the research is performed by a small set of academic groups; it is likely that these types of fundamental studies will attract more attention and even be commercialized in the near future.
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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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Quantitative HPLC Analysis of Coumarin in Alcoholic Woodruff Extracts in May WineHow long should you perform an extraction of woodruff leaves so that you don’t end up with a harmful amount of coumarin, but still get the characteristic flavor of the finished May wine?
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Ultrahigh-Performance Liquid Chromatography–Mass Spectrometry in LipidomicsAn analytical method for the global profiling of molecular lipids in biological samples, with particular emphasis on the plasmalogen lipids, is described.
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Current Practices and Considerations for a Stability-Indicating Method in Pharmaceutical AnalysisWhat are the characteristics and relevant considerations for the development and validation of a stability-indicating method?
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Landmarks in the Evolution of Ion ChromatographyFrom the invention of eluent suppression to today's "just add water" concept, pivotal developments over the last 40 years are chronologically highlighted from a chemical and instrumental viewpoint.
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High-Resolution Mass Spectrometry: An Ideal Analytical Tool for Drug Metabolism StudiesA method using HR-MS systems to characterize the structures of metabolites is presented. The result is a general workflow for metabolism studies in drug discovery and development.
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*** TEST *** Estimation of the Main Sources of Uncertainty in Chromatographic Analysis: Determination of Biogenic Amines ***TEST ***This article establishes the estimation of the uncertainty associated with the chromatographic determination of biogenic amines. The authors identify and estimate each source of uncertainty to establish the accuracy of results and to obtain a better understanding of the method. Thus, measurement uncertainty was split into two sections: uncertainty related to the working conditions, which considers the equipment used, and inherent uncertainty, which includes the chemical stages indicated in the procedure as well as calibration sources, taking into account the existence of the matrix effect. Recovery studies also were made to quantify the contribution of bias to the overall uncertainty. This parameter was calculated for the determination of biogenic amines in different types of samples.
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Strategies for the Detection and Elimination of Matrix Effects in Quantitative LC–MS AnalysisWe assessed a simple method based on recovery for the detection of matrix effects and two alternative methods for the rectification of matrix effects in LC–MS: standard addition and the coeluting internal standard method.
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Application of Mass Spectrometry to Support Verification and Characterization of Counterfeit PharmaceuticalsThe production and sale of counterfeit drugs has risen sharply in recent years. The World Health Organization (WHO) estimates that counterfeit medicines account for approximately 1% of sales in developed countries and well over 10% in developing countries.
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The Next Step in Targeted Drug Imaging for Oncology: Combining Laser-Induced Post-Ionization with MALDI ImagingOver the last decade, matrix-assisted laser desorption–ionization (MALDI) imaging has become an indispensable tool for a broad range of applications, from studying plant metabolomics to discovering biomarkers of disease to developing new therapies. As such, MALDI imaging is revolutionizing preclinical drug discovery pipelines by providing direct distribution monitoring of therapeutic compounds and their metabolites along with untargeted pharmacodynamic information. A key application of MALDI imaging is tissue analysis for oncology, and recent developments in MALDI technology promise greater benefits to cancer research. The combination of MALDI with laser-induced post-ionization (PI) enhances the detection and imaging of pharmaceutical compounds and other classes of compounds, allowing for significant advances in the use of MALDI imaging for studying drug metabolism and pharmacodynamics in tumor tissues. This article describes the value of MALDI Imaging for oncology applications and examines the potential for laser-induced PI, including the ability to achieve up to three orders of magnitude higher sensitivity and to image metabolite classes previously undetectable with traditional MALDI.
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The Smell of Success: Using GC–MS–MS for Low Level Allergenic Fragrance DetectionThe regulatory and practical issues that surround allergenic fragrance use within cosmetics and cleaning products are explored in this article.
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A New Method for Quality by Design Robust Optimization in Liquid ChromatographyA new method to optimize liquid chromatography (LC) methods using a Quality by Design (QbD) approach is presented. This method is based on the use of design of experiments (DOE) and independent component analysis (ICA) to accurately estimate the modeled responses (that is, the retention times at the beginning, the apex, and the end) of each peak, even for coeluted peaks. This method was applied to the optimization of the separation of nine compounds in a mixture, yielding the design space and the demonstration of robustness of the method.
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The Misunderstood Laboratory Solvent: Reagent Water for HPLCA good pretreatment system combines reverse osmosis and electrodeionization technologies.
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Separation of AntiretroviralsAntiretrovirals have come back to the forefront of separation science at this moment in time, as they have found use in the fight against SARS-CoV-2.
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Analysis of Four Phthalate Monoesters in Human Urine Using Liquid Chromatography Tandem Mass SpectrometryA fast, sensitive and accurate quantitative method was developed using HPLC–MS–MS for analysis of phthalate metabolites in urine samples.
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How Reversed-Phase Liquid Chromatography WorksThis tutorial on reversed-phase LC explains the role of solvent, chain conformation, solute position, and retention dynamics.
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Helium Supply: The Search For AlternativeThis article provides an update on the search for an alternative to helium.
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Nontargeted Metabolite Profiling by UHPLC–MS: A Case Study in Beer Reveals Effect of Temperature on Nonvolatile Small Molecules During StorageThis analytical approach can be applied in many fields; the example illustrates its use in a food chemistry application.
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Determination of Fipronil and Its Metabolites in Eggs and Environmental Matrices by LC–MS/MSAn improved LC–MS/MS method that can rapidly detect fipronil, an insecticide harmful to human health, is presented here for chicken eggs, feed, and soil.
