CONFIRMATION OF LOW CONCENTRATIONS OF URINARY BENZODIAZEPINES, INCLUDING ALPRAZOLAM AND TRIAZOLAM, BY GC/MS - AN EXTRACTIVE ALKYLATION PROCEDURE

Urine samples containing diazolo- and triazolobenzo- diazepines and metabolites were hydrolyzed with β- glucuronidase and extracted with methylene chloride. The extracts were treated with methyl iodide, methylene chloride, and tetrahexylammonium hydrogen sulfate in basic solution to form the methyl derivatives of the drugs and metabolites. GC/MS analysis resulted in the following test characteristics: Day-to-day precision at 360 ng/mL (120 ng/mL for the trlazolobenzodiazepine metabolites) was 2.4 to 5.5% CV; calibration curves were linear to 6000 ng/mL (1000 ng/mL for the trlazolobenzodiazepine metabolites), and operational limits of quantitation were in the range 13-25 ng/mL. © 1992 Journal of Analytical Toxicology.