This procedure was developed as an overall benzodlazeplne confirmation scheme and Includes the detection of the most Important urinary analytes encountered by clinical toxicology laboratories in North America: α-hydroxyalprazolam, e(-hydroxytrlazolam, 2-hydroxyethylflurazepam, oxazepam, temazepam, and Iorazepam. Desmethyldlazepam (nordiazepam) was not targeted because it Is metabolized to oxazepam. This procedure takes advantage of β-glucuronldase hydrolysis for analysis of intact benzodlazepine molecules, oxazepam-2H5 as an internal standard, a newly developed extraction solvent, and a silylating moiety that may be more sensitive than trlmethylsilyl (-TMS) derivatives, the tert-butyldimethylsilyl (-TBDMS) derivative. For all compounds the extraction efficiency was greater than 90% and the limit of quantltatlon (LOQ at a S/N of 10) was less than 10 ng/mL. Coefficients of variation for a 200-ng/mL control were less than 5% and less than or equal to 11% for within-run and between-run trials, respectively. Of 13 human specimens screened by EMIT and most with self-reported histories, c(-hydroxyalprazolam was found In seven (range 49-1264 ng/mL), oxazepam was found in five (72-3897 ng/mL), and Iorazepam (476 ng/mL), 2-hydroxyethylflurazepam (2301 ng/mL), and (α-hydroxytrlazolam (106 ng/mL) In one each. © 1992, Oxford University Press. All rights reserved.