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.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2001年第8期919-921,共3页
Chinese Journal of Analytical Chemistry
