King J W, King L J
Roche Biomedical Laboratories, Houston, Texas 77074, USA.
J Anal Toxicol. 1996 Jul-Aug;20(4):262-5. doi: 10.1093/jat/20.4.262.
Because of the increase in use of the newer benzodiazepines, we explored the opportunity to develop a gas chromatographic-mass spectrometric (GC-MS) method that encompasses most of the widely prescribed benzodiazepines in use today. The benzodiazepines included in our study are nordiazepam, oxazepam, temazepam, lorazepam, alpha-hydroxyalprazolam, alpha-hydroxytriazolam, desalkylflurazepam, and 2-hydroxyethylflurazepam. Using 1.0 mL of urine as the matrix, we added the enzyme Glusulase and incubated the specimens for 2 h to obtain the free drugs. The hydrolyzed samples were then loaded onto a Toxi-Lab Spec VC MP3 column containing a 15-mg disc. On-disc derivatization was accomplished by adding N-methyl-N-(t-butyldimethylsilyl) trifluroacetamide (MTBSTFA) with 1% TBDMSCI to the disc. The derivatives were then placed in a GC vial and analyzed by GC-MS in the selected ion monitoring mode. These results were then compared to confirmed positives by the traditional acid hydrolysis GC-MS method.
由于新型苯二氮䓬类药物的使用增加，我们探索了开发一种气相色谱-质谱联用（GC-MS）方法的机会，该方法涵盖了当今使用的大多数广泛处方的苯二氮䓬类药物。我们研究中包括的苯二氮䓬类药物有去甲西泮、奥沙西泮、替马西泮、劳拉西泮、α-羟基阿普唑仑、α-羟基三唑仑、去烷基氟西泮和2-羟乙基氟西泮。以1.0 mL尿液为基质，加入葡萄糖醛酸酶并将标本孵育2小时以获得游离药物。然后将水解后的样品加载到含有15 mg盘片的Toxi-Lab Spec VC MP3柱上。通过向盘片中加入含1%叔丁基二甲基硅烷基氯（TBDMSCI）的N-甲基-N-（叔丁基二甲基硅烷基）三氟乙酰胺（MTBSTFA）完成盘上衍生化。然后将衍生物放入GC小瓶中，并通过GC-MS在选择离子监测模式下进行分析。然后将这些结果与传统酸水解GC-MS方法确认的阳性结果进行比较。
