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Updated: Apr 19, 2026
Gas Chromatography-Mass Spectrometry Paired with Total Vaporization Solid-Phase Microextraction as a Forensic Tool
Published on: May 25, 2021
Development of a MSFIA sample treatment system as front end of GC-MS for atenolol and propranolol determination in
María del Rosario Brunetto1, Sabrina Clavijo1, Yelitza Delgado1
1Molecular Spectroscopy Laboratory, Department of Chemistry, Faculty of Sciences, Los Andes University, La Hechicera, Mérida 5101, Venezuela.
Abstract:
An on-line solid-phase extraction (SPE) method coupled to gas chromatography-mass spectrometry (GC-MS) has been developed for the determination of atenolol (ATN) and propranolol (PRO) in human plasma. The hyphenation of SPE with multisyringe flow injection analysis (MSFIA) allows the simultaneous GC-MS determination of ATN and PRO with high selectivity and sensitivity. On-line preconcentration and derivatisation of the analytes were carried out by means of using restricted access materials (RAM) and microwave (MW) assisted derivatisation reactions with N-methyl-N-(trimethylsilyl) trifluoroacetamide (MSTFA)+1% trimethylchlorosilane (TMCS). Multivariate optimization was applied to optimize experimental conditions. The whole procedure comprising sample pretreatment and analyte determination took about 15 min. However, the overlap of the automatic sample treatment with the GC separation increased the frequency to 7 samples h(-1). The validated method was successfully applied to direct ATN and PRO determination in human plasma.
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