Meatherall R
Department of Biochemistry, St. Boniface General Hospital, Winnipeg, Manitoba, Canada.
J Anal Toxicol. 1994 Nov-Dec;18(7):369-81. doi: 10.1093/jat/18.7.369.
A confirmatory method using gas chromatography-mass spectrometry (GC-MS) is described for benzodiazepine metabolites commonly encountered in urine. The targeted drugs are diazepam, nordiazepam, temazepam, oxazepam, lorazepam, alpha-hydroxyalprazolam, alpha-hydroxytriazolam, 2-hydroxyethyl-flurazepam, N-desalkyl-3-hydroxyflurazepam, and N-desalkylflurazepam. After enzymatic hydrolysis, the free benzodiazepines are recovered from the urine by liquid-liquid extraction. The organic solvent is evaporated to dryness. The residue is subjected to sequential derivatization involving propylation of the secondary amine in the lactam ring followed by propionylation of hydroxyl groups. The derivatives are separated on a methyl silicone capillary column and then identified and quantitated by full-scan GC-MS. Characteristic ion clusters are selected for quantitation. Four internal standards are used: oxazepam-d5, lorazepam-d4, alpha-hydroxyalprazolam-d5, and alpha-hydroxytriazolam-d4.
本文描述了一种使用气相色谱 - 质谱联用（GC-MS）的确证方法，用于检测尿液中常见的苯二氮䓬类代谢物。目标药物包括地西泮、去甲地西泮、替马西泮、奥沙西泮、劳拉西泮、α-羟基阿普唑仑、α-羟基三唑仑、2-羟乙基氟西泮、N-去烷基-3-羟基氟西泮和N-去烷基氟西泮。酶促水解后，通过液 - 液萃取从尿液中回收游离的苯二氮䓬类药物。将有机溶剂蒸发至干。残渣进行连续衍生化，包括对内酰胺环仲胺进行丙基化，然后对羟基进行丙酰化。衍生物在甲基硅氧烷毛细管柱上分离，然后通过全扫描GC-MS进行鉴定和定量。选择特征离子簇进行定量。使用四种内标：奥沙西泮 - d5、劳拉西泮 - d4、α-羟基阿普唑仑 - d5和α-羟基三唑仑 - d4。
