气相色谱电子捕获检测法测定人尿中氟硝西泮的代谢物7-氨基氟硝西泮  

Determination of 7-Aminoflunitrazepam, Main Metabolites of Flunitrazepam, in Human Urine by Gas Chromatography with Electron Capture Detector

作　　者：邢丽梅[1] 谭家镒[1] 李发美[2] 姜兆林[1] 

机构地区：[1]中国刑事警察学院法医系,沈阳110035 [2]沈阳药科大学,沈阳110015

出　　处：《分析化学》2001年第8期919-921,共3页Chinese Journal of Analytical Chemistry

摘　　要：采用气相色谱电子捕获检测法测定人尿中氟硝西泮的代谢物 7 氨基氟硝西泮。测定时尿中加入内标 7 氨基硝西泮 ,用β 葡萄糖醛酸苷酶水解及碱性液液萃取 ,再用七氟丁酸酐衍生化。尿中 7 氨基氟硝西泮提取率为 96.8% ;回收率为 98.6± 3 .4% (平均值±SD) ;检出限为 1 .2 μg L ,对口服治疗量氟硝西泮的人尿进行检测 ,可检出服药后 60h尿中的 7 氨基氟硝西泮。A gas chromatographic technique with electron capture detection procedure was developed for the determination of 7-aminoflunitrazepam (7-AFLNZ), main metabolite of flunitrazepam (FLNZ) in human urine. After adding 7-aminonitrazepam (7-ANITZ, internal standard), hydrolysis with beta -glucuronidase, liquid-liquid extraction at pH 10.8, and derivatization with heptfluorobutanic acid anhydride, the analysis was performed on a HP-5 capillary column with electron capture detection. The detection limit of 7-AFLNZ in urine was 1.2 mug/L. The extraction efficiency of 7-AFLNZ and 7-ANITZ in urine was 96.8% end 93.5% respectively. The recovery of 7-AFLNZ spiked in blank speciments at level of 50 mug/L was 98.6 +/-3.4% (Mean SD). The method was used for assaying urine speciments tram volunteers ingesting FLNZ. A single dose concentration-time study was performed and the time course of 7-AFLNZ concentration over 60 hours was determined.

关 键 词：氟硝西泮 7-氨基氟硝西泮 氟代酰基衍生化 人尿 气相色谱法 测定 麻醉案件 

分 类 号：O657.7[理学—分析化学]