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Screening method for benzodiazepines and hypnotics in hair at pg/mg level by liquid chromatography–mass spectrometry/mass spectrometry
Ist Teil von
Journal of chromatography. B, 2005-10, Vol.825 (1), p.72-78
Ort / Verlag
Amsterdam: Elsevier B.V
Erscheinungsjahr
2005
Quelle
Elsevier ScienceDirect Journals
Beschreibungen/Notizen
A procedure is presented for the screening of 16 benzodiazepines and hypnotics in human hair by LC–MS/MS (alprazolam, 7-aminoclonazepam, 7-aminoflunitrazepam, bromazepam, clobazam, diazepam, lorazepam, lormetazepam, midazolam, nordiazepam, oxazepam, temazepam, tetrazepam, triazolam, zaleplon and zolpidem). The method involves decontamination of hair with methylene chloride, hair cut into small pieces, incubation of 20
mg in phosphate buffer (pH 8.4) in the presence of 1
ng diazepam-d
5 used as internal standard, liquid–liquid extraction with diethyl ether/methylene chloride (10/90) and separation using liquid chromatography–tandem mass spectrometry. The limits of quantification for all benzodiazepines and hypnotics range from 0.5 to 5
pg/mg using a 20-mg hair sample. Linearity is observed from the limit of quantification of each compound to 200
pg/mg (
r
2
>
0.99). Coefficients of variation measured on six points and at two concentrations (10 and 50
pg/mg) range from 5 to 20% for all drugs but one. Extraction recovery, measured at the two same concentrations range from 32 to 76%. These results were found suitable to screen for 16 benzodiazepines in hair and detect them at very low concentrations, making this method suitable to monitor single dose.