血和尿中7-氨基硝西泮的GC-ECD检测

 目的　建立血、尿中硝西泮的代谢物 7-氨基硝西泮GC-ECD检测方法。方法　碱性条件下用苯-异戊醇(98.8∶1.5)提取,七氟丁酸酐为酰化试剂,室温无水条件下进行酰化,GC-ECD法检测。结果　血、尿中7-氨基硝西泮浓度在5～300ng·mL^-1范围内呈良好的线性关系,血、尿中的提取率分别为(86.9±4.5)%(n=5)和(96.9±3.9)%(n=5),检出限分别为2.8及1.4ng·mL^-1。结论　该方法灵敏度高,线性范围宽,将建立的方法应用于人口服药物后的血、尿检测,结果满意。

Determination of 7-aminonitrazepam in plasma and urine by GC-ECD

OBJECTIVE To determine the contents of 7-aminonitrazepam, the metabolite of nitrazepam in plasma and urine by GC-ECD.METHODS The metabolite was extracted from plasma and urine with benzene-isopentyl alcohol (98.5∶1.5) at pH 10.8, and then derived with heptfluorobutanic acid anhydride. The analysis was performed on a HP-5 column with electron capture detection. RESULTS The linearity was obtained over the range of 5～300 ng·mL^-1, and the detection limits were 2.8 ng·mL^-1 and 1.4 ng·mL^-1 for 7-aminonitrazepam in plasma and urine respectively. The extraction recoveries were (86.9±4.5)%(n=5) and (96.9±3.9)%(n=5) respectively. The method was applied to determine 7-aminonitrazepam in plasma and urine after a single dose nitrazepam in 3 healthy subjectes.CONCLUSION The method was simple, specific and sensitive.