OBJECTIVE: Screen seventeen benzodizepines and their metabolitesin urine by GC/ECD and GC/MS. METHODS: They were GC (GC/ECD, GC/MS) assay of benzodizepines and GC (GC/ECD, GC/MS) assay of benzophenones of acid-hydrolytic products of 1,4-benzodizepines. RESULTS: The methods were simple and sensitive. The recoverys were 60% to 90% of most benzodizepines, linear calibration curves were 20 ng/ml-200 ng/ml (r > 0.99), and detection limits were 0.5 ng/ml-10 ng/ml. CONCLUSION They methods were evaluated with human urine samples.
Anti-Anxiety Agents/urine* ; Benzodiazepines/urine* ; Benzophenones/urine* ; Chromatography, Gas ; Gas Chromatography-Mass Spectrometry ; Humans

AIMTo investigate the fragmentation behavior of triazolobenzodiazepines and to develop a specific, sensitive and rapid LC/MSn assay for simultaneous determination of estazolam, alprazolam and triazolam in human urine.

METHODSAfter oral administration of a single 4 mg dose of the drugs to each of three healthy volunteers, urine samples were purified by solid-phase extraction, and then injected into an ODS column (150 mm x 4.6 mm) with a mobile phase of methanol-water (8:2) for LC/MSn analysis. The structures of estazolam, alprazolam and triazolam in human urine were identified by direct comparison of the observed mass spectra and the chromatographic retention time with those of the reference substance. The mass spectrometer (Finnigan LCQ) was operated in positive mode and in two scan modes including SIM and full scan MS/MS mode. The obtained mass spectra was analyzed assisted with the software Mass Frontier 1.0 for their fragmentation pathways.

RESULTSThe full scan MS/MS spectra of each compound gave characteristic fragment ions of [M + H - N2]+ and [M + H - Cl]+. The detection limit was below 0.5 ng.mL-1 for estazolam, alprazolam and triazolam in human urine.

CONCLUSIONThe method is useful in forensic and clinical toxicology in which unequivocal identification of eatazolam, alprazolam and triazolam is desired.

Alprazolam ; urine ; Anti-Anxiety Agents ; urine ; Chromatography, Liquid ; Estazolam ; urine ; Humans ; Male ; Spectrometry, Mass, Electrospray Ionization ; Triazolam ; urine