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Titolo:
Simultaneous determination of fifteen low-dosed benzodiazepines in human urine by solid-phase extraction and gas chromatography-mass spectrometry
Autore:
Borrey, D; Meyer, E; Lambert, W; Van Peteghem, C; De Leenheer, AP;
Indirizzi:
State Univ Ghent, Toxicol Lab, B-9000 Ghent, Belgium State Univ Ghent Ghent Belgium B-9000 Toxicol Lab, B-9000 Ghent, Belgium State Univ Ghent, Lab Fysiol Biochem & Biometrie, B-9820 Merelbeke, Belgium State Univ Ghent Merelbeke Belgium B-9820 rie, B-9820 Merelbeke, Belgium
Titolo Testata:
JOURNAL OF CHROMATOGRAPHY B
fascicolo: 2, volume: 765, anno: 2001,
pagine: 187 - 197
SICI:
1387-2273(200112)765:2<187:SDOFLB>2.0.ZU;2-R
Fonte:
ISI
Lingua:
ENG
Soggetto:
PERFORMANCE LIQUID-CHROMATOGRAPHY; NITROGEN-PHOSPHORUS DETECTION; GC-MS; HUMAN PLASMA; WHOLE-BLOOD; HUMAN SERUM; FLUNITRAZEPAM; METABOLITES; HPLC; IDENTIFICATION;
Keywords:
benzodiazepines;
Tipo documento:
Article
Natura:
Periodico
Settore Disciplinare:
Life Sciences
Citazioni:
33
Recensione:
Indirizzi per estratti:
Indirizzo: De Leenheer, AP State Univ Ghent, Toxicol Lab, Harelbekestr 72, B-9000 Ghent, Belgium State Univ Ghent Harelbekestr 72 Ghent Belgium B-9000 ium
Citazione:
D. Borrey et al., "Simultaneous determination of fifteen low-dosed benzodiazepines in human urine by solid-phase extraction and gas chromatography-mass spectrometry", J CHROMAT B, 765(2), 2001, pp. 187-197

Abstract

A gas chromatographic-mass spectrometric method was developed for the simultaneous analysis of 15 low-dosed benzodiazepines, both parent compounds and their corresponding metabolites, in human urine. The target compounds arealprazolam, alpha -hydroxyalprazolam, 4-hydroxyalprazolam, flunitrazepam, 7-aminoflunitrazepam, desmethylflunitrazepam, flurazepam, hydroxyethylflurazepam, nitrogen-desalkylflurazepam, ketazolam, oxazepam, lormetazepam, lorazepam, triazolam and alpha -hydroxytriazolam. Nitrogen-methylclonazepam is used as the internal standard. The urine sample preparation involves enzymatic hydrolysis of the conjugated metabolites with Helix pomatia beta -glucuronidase for 1 h at 56 degreesC followed by solid-phase extraction on a phenyl-type column. The extracted benzodiazepines are subsequently analyzed ona polydimethylsiloxane column using on-column injection to enhance sensitivity. The extraction efficiency exceeded 80% for all compounds except for oxazepam, lorazepam and 4-hydroxyalprazolam which had recoveries of about 60%. The LODs ranged from 13 to 30 ng/ml in the scan mode and from 1.0 to 1.7ng/ml in the selected ion monitoring (SIM) mode. Linear calibration curveswere obtained in the concentration ranges from 50 to 1000 ng/ml in the scan mode and from 5 to 100 ng/ml in the SLM mode. The within-day and day-to-day relative standard deviations at three different concentrations never exceeded 15%. (C) 2001 Elsevier Science B.V. All rights reserved.

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Documento generato il 19/01/20 alle ore 15:03:56