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High Resolution-Magic Angle Spinning (HR-MAS) solid-state NMR spectroscopy is finding increasing application in the analysis of solid foods, bypassing the need for complicated solvent extraction procedures. In the present protocol, we report a simple analytical approach based on HR-MAS NMR spectroscopy for the phenolic profiling of olive fruits, flesh, or skin. This approach allows the facile characterization of phenolic compounds in olive fruits cultivated for extra-virgin olive oil production as a function of maturation and variety, in addition to processing technology for table olives.

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Two-Phase Extraction for Comprehensive Analysis of the Plant Metabolome by NMR.

Methods Mol Biol

January 2025

Grupo Metabolômica, Universidade Estadual do Norte Fluminense, Campos dos Goytacazes, RJ, Brazil.

Metabolomics is the area of research, which strives to obtain complete metabolic fingerprints, to detect differences between them and to provide hypothesis to explain those differences (Schripsema J, Dagnino D, Handbook of chemical and biological plant analytical methods. Wiley, New York, 2015). However, obtaining complete metabolic fingerprints is not an easy task.

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Analysis of Urinary Metanephrines Using Liquid Chromatography Tandem Mass Spectrometry.

Methods Mol Biol

January 2025

Analytic Biochemistry, Calculi and Manual Chemistry, Mass Spectrometry, ARUP Laboratories, Inc., Salt Lake City, UT, USA.

Metanephrines (metanephrine [MN] and normetanephrine [NMN]) are O-methylated metabolites derived from the catecholamines, epinephrine, and norepinephrine, respectively. High concentrations of metanephrines have been observed in individuals with pheochromocytoma, a neuroendocrine tumor. Measurement of metanephrines in urine is used to screen for the tumor.

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UHPLC-TIMS-PASEF-MS for Lipidomics: From Theory to Practice.

Methods Mol Biol

January 2025

Department of Medicine and Surgery, Proteomics and Metabolomics Unit, University of Milano-Bicocca, Vedano al Lambro, Italy.

Trapped ion mobility spectrometry (TIMS) using parallel accumulation serial fragmentation (PASEF) is an advanced analytical technique that offers several advantages in mass spectrometry (MS)-based lipidomics. TIMS provides an additional dimension of separation to mass spectrometry and accurate collision cross-section (CCS) measurements for ions, aiding in the structural characterization of molecules. This is especially valuable in lipidomics for identifying and distinguishing isomeric or structurally similar compounds.

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A Protocol for GC-MS Profiling of Chiral Secondary Amino Acids.

Methods Mol Biol

January 2025

Laboratory of Analytical Biochemistry & Metabolomics, Biology Centre, Czech Academy of Sciences, České Budějovice, Czech Republic.

A simple analytical workflow is described for gas chromatographic-mass spectrometric (GC-MS)-based chiral profiling of secondary amino acids (AAs) in biological matrices. The sample preparation is carried out directly in aqueous biological sample extracts and involves in situ heptafluorobutyl chloroformate (HFBCF) derivatization-liquid-liquid microextraction of nonpolar products into hexane phase followed by subsequent formation of the corresponding methylamides from the HFB esters by direct treatment with methylamine reagent solution. The (O, N) HFB-butoxycarbonyl-methylamide AA products (HFBOC-MA) are separated on a Chirasil-L-Val capillary column and quantitatively measured by GC-MS operated in selected ion monitoring (SIM) mode.

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