Simultaneous determination of eleven benzodiazepine hypnotics and eleven relevant metabolites in urine by column-switching liquid chromatography-mass spectrometry

J Anal Toxicol. 2002 Mar;26(2):87-93. doi: 10.1093/jat/26.2.87.

Abstract

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.

MeSH terms

  • Anticonvulsants / analysis*
  • Anticonvulsants / urine
  • Benzodiazepines / analysis*
  • Benzodiazepines / urine
  • Chromatography, High Pressure Liquid / instrumentation
  • Chromatography, High Pressure Liquid / methods*
  • Forensic Medicine / methods
  • Humans
  • Sensitivity and Specificity
  • Spectrometry, Mass, Electrospray Ionization / methods*
  • Substance Abuse Detection / methods*

Substances

  • Anticonvulsants
  • Benzodiazepines