Simultaneous determination of eleven benzodiazepine hypnotics and eleven relevant metabolites in urine by column-switching liquid chromatography-mass spectrometry.
An automated column-switching liquid chromatographic-atmospheric pressure chemical ionization-mass spectrometric (LC-APCI-MS) method for the simultaneous determination of frequently encountered benzodiazepine hypnotics and their relevant metabolites in urine has been established. A column-switching online solid-phase extraction technique was employed to enhance sensitivity and eliminate tedious sample pretreatment. The combination of an N-vinylacetamide-containing hydrophilic polymer online extraction column and a C18 semi-micro LC column provided the successful separations and MS determinations of the 11 benzodiazepines and 11 relevant metabolites tested in this study. The detection limits ranged 2-10 ng/mL and 10-50 ng/mL in the SIM and full-scan modes, respectively, using 50 microL of urine. The calibration curves were linear up to 500 ng/mL for all these analytes in the SIM mode. The present method provided successful forensic applications for the proof of benzodiazepine administration.
Miki
Akihiro
A
Forensic Science Laboratory, Osaka Prefectural Police Headquarters, Japan. CZD13116@nifty.ne.jp
Tatsuno
Michiaki
M
Katagi
Munehiro
M
Nishikawa
Mayumi
M
Tsuchihashi
Hitoshi
H
D000927:Anticonvulsants / Q000032:analysis* / Q000652:urine; D001569:Benzodiazepines / Q000032:analysis* / Q000652:urine; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D005554:Forensic Medicine / Q000379:methods; D006801:Humans; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D015813:Substance Abuse Detection / Q000379:methods*
D000927:Anticonvulsants; D001569:Benzodiazepines