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Titolo:
Analytical methodology for the detection of beta(2)-agonists in urine by gas chromatography-mass spectrometry for application in doping control
Autore:
Ventura, R; Damasceno, L; Farre, M; Cardoso, J; Segura, J;
Indirizzi:
IMIM, Unitat Farmacol, Barcelona 08003, Spain IMIM Barcelona Spain 08003IMIM, Unitat Farmacol, Barcelona 08003, Spain Univ Pompeu Fabra, Barcelona, Spain Univ Pompeu Fabra Barcelona SpainUniv Pompeu Fabra, Barcelona, Spain Univ Fed Rio de Janeiro, Rio De Janeiro, Brazil Univ Fed Rio de Janeiro Rio De Janeiro Brazil o, Rio De Janeiro, Brazil Univ Autonoma Barcelona, E-08193 Barcelona, Spain Univ Autonoma BarcelonaBarcelona Spain E-08193 E-08193 Barcelona, Spain
Titolo Testata:
ANALYTICA CHIMICA ACTA
fascicolo: 1, volume: 418, anno: 2000,
pagine: 79 - 92
SICI:
0003-2670(20000801)418:1<79:AMFTDO>2.0.ZU;2-R
Fonte:
ISI
Lingua:
ENG
Soggetto:
BETA(2)-ADRENERGIC AGONIST RESIDUES; BETA-AGONISTS; CLINICAL PHARMACOKINETICS; CONFIRMATORY ANALYSIS; SCREENING-PROCEDURE; ADRENERGIC-DRUGS; BAMBUTEROL; METABOLITES; ANIMALS; LIVER;
Keywords:
beta(2)-agonists; gas chromatography-mass spectrometry; doping analysis;
Tipo documento:
Article
Natura:
Periodico
Settore Disciplinare:
Physical, Chemical & Earth Sciences
Citazioni:
29
Recensione:
Indirizzi per estratti:
Indirizzo: Ventura, R IMIM, Unitat Farmacol, Doctor Aiguder 80, Barcelona 08003, Spain IMIM Doctor Aiguder 80 Barcelona Spain 08003 lona 08003, Spain
Citazione:
R. Ventura et al., "Analytical methodology for the detection of beta(2)-agonists in urine by gas chromatography-mass spectrometry for application in doping control", ANALYT CHIM, 418(1), 2000, pp. 79-92

Abstract

A comprehensive gas chromatographic-mass spectrometric (GC-MS) procedure for detection in urine of beta(2)-agonists having different alkyl or phenylalkyl chains at the nitrogen atom is described. The method is based on an enzymatic hydrolysis with P-glucuronidase from Helix pomatia, followed by a solid-phase extraction procedure using Bond Elut Certify columns. The influence of urine pH in the extraction recovery has been studied and pH 9.5 was found to give best recovery and cleaner extracts. After pH adjustment, the sample was applied to the pre-conditioned cartridges and after a washing step, the Pz-agonists were eluted with a mixture of chloroform and isopropanol (80:20, v/v) containing 2% ammonia. The residues were derivatised with N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA), and analysed by GC-MS. A validation procedure for qualitative analysis of Pz-agonists in urine wasperformed. Selectivity of the method showed that no interfering peaks wereobserved for most of the compounds at the retention time of the Pz-agonists. Extraction recoveries ranged from 68.1 to 103.7% in urine samples. Detection limits from 0.5 to 5 ng ml(-1) were obtained using selected-ion monitoring. Intra-assay precision ranged between 2.3 and 13.8% for ail compounds except for fenoterol. The International Olympic Committee (IOC) criteria for compound identification were fulfilled for the compounds studied. The optimised method was successfully applied to analyse urine samples obtained from excretion studies in healthy volunteers. (C) 2000 Elsevier Science B.V. All rights reserved.

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Documento generato il 06/04/20 alle ore 01:43:28