West R E, Ritz D P
POISONLAB Inc., San Diego, CA 92111.
J Anal Toxicol. 1993 Mar-Apr;17(2):114-6. doi: 10.1093/jat/17.2.114.
A method for the GC/MS confirmation of oxazepam, nordiazepam, desalkylflurazepam, temazepam, and alpha-hydroxyalprazolam in urine is described. The method incorporates a solid phase extraction technique developed by Varian which was found to extract all five metabolites with recoveries exceeding 73%. The extracted metabolites were derivatized with N-methyl-N-(tert-butyldimethylsilyl)-trifluoroacetamide (MTBSTFA), resulting in the formation of stable tert-butyldimethylsilyl (TBDMS) derivatives. Quantitation was performed by GC/MS using oxazepam-D5, nordiazepam-D5, and alpha-hydroxyalprazolam-D5 as internal standards. The method was found to be linear over the range of 50-2000 ng/mL. Within-run precision, measured as the coefficient of variation at 100 ng/mL, was less than 3% for all analytes except temazepam which was 6% (N = 20).
本文描述了一种用于尿液中奥沙西泮、去甲西泮、去烷基氟西泮、替马西泮和α-羟基阿普唑仑的气相色谱/质谱（GC/MS）确证方法。该方法采用了Varian公司开发的固相萃取技术，发现该技术能提取所有五种代谢物，回收率超过73%。提取的代谢物用N-甲基-N-（叔丁基二甲基甲硅烷基）-三氟乙酰胺（MTBSTFA）进行衍生化，形成稳定的叔丁基二甲基甲硅烷基（TBDMS）衍生物。使用奥沙西泮-D5、去甲西泮-D5和α-羟基阿普唑仑-D5作为内标，通过GC/MS进行定量分析。该方法在50 - 2000 ng/mL范围内呈线性。批内精密度以100 ng/mL时的变异系数衡量，除替马西泮为6%（N = 20）外，所有分析物均小于3%。
