title: 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 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.
authors.affiliation: Molecular Spectroscopy Laboratory, Department of Chemistry, Faculty of Sciences, Los Andes University, La Hechicera, Mérida 5101, Venezuela. Electronic address: brunetto@ula.ve.
authors.forename: María del Rosario
authors.initials: Mdel R
authors.lastname: Brunetto
authors.affiliation: Molecular Spectroscopy Laboratory, Department of Chemistry, Faculty of Sciences, Los Andes University, La Hechicera, Mérida 5101, Venezuela.
authors.forename: Sabrina
authors.initials: S
authors.lastname: Clavijo
authors.affiliation: Molecular Spectroscopy Laboratory, Department of Chemistry, Faculty of Sciences, Los Andes University, La Hechicera, Mérida 5101, Venezuela.
authors.forename: Yelitza
authors.initials: Y
authors.lastname: Delgado
authors.affiliation: Molecular Spectroscopy Laboratory, Department of Chemistry, Faculty of Sciences, Los Andes University, La Hechicera, Mérida 5101, Venezuela.
authors.forename: Wendy
authors.initials: W
authors.lastname: Orozco
authors.affiliation: Molecular Spectroscopy Laboratory, Department of Chemistry, Faculty of Sciences, Los Andes University, La Hechicera, Mérida 5101, Venezuela.
authors.forename: Máximo
authors.initials: M
authors.lastname: Gallignani
authors.affiliation: Molecular Spectroscopy Laboratory, Department of Chemistry, Faculty of Sciences, Los Andes University, La Hechicera, Mérida 5101, Venezuela.
authors.forename: Carlos
authors.initials: C
authors.lastname: Ayala
authors.affiliation: Laboratory of Environmental Analytical Chemistry-LQA2, University of the Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca, Spain.
authors.forename: Víctor
authors.initials: V
authors.lastname: Cerdà
mesh_terms: D000081:Acetamides / Q000737:chemistry; D001262:Atenolol / Q000097:blood*; D005163:Factor Analysis, Statistical; D017022:Flow Injection Analysis / Q000295:instrumentation / Q000379:methods*; D005463:Fluoroacetates / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006801:Humans; D008872:Microwaves; D011433:Propranolol / Q000097:blood*; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*; D014297:Trimethylsilyl Compounds / Q000737:chemistry
chemical_list: D000081:Acetamides; D005463:Fluoroacetates; D014297:Trimethylsilyl Compounds; C086665:N-methyl-N-(trimethylsilyl)trifluoroacetamide; D001262:Atenolol; C039293:trimethylchlorosilane; D011433:Propranolol
keywords: Atenolol; Gas chromatography–Mass spectrometry (GC–MS); Human plasma; Microwave assisted derivatisation; Multisyringe flow injection analysis (MSFIA); Propranolol; Solid-phase extraction (SPE)