Development of a MSFIA sample treatment system as front end of GC–MS for atenolol and propranolol determination in human plasma

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 15min. However, the overlap of the automatic sample treatment with the GC separation increased the frequency to 7samplesh−1. The validated method was successfully applied to direct ATN and PRO determination in human plasma.