特丁基二甲基硅烷衍生化-气相色谱-质谱联用法分析尿中硝西泮的代谢物7-氨基硝西泮

Determination of 7-Aminonitrazepam, Metabolite of Nitrazepam,in Urine by tert-Butyldimethylsilyl Derivatization-Gas Chromatography-Mass Spectrometry

建立了用特丁基二甲基硅烷 (TBDMS)衍生化 气相色谱 质谱联用分析尿中硝西泮的主要代谢物 7 氨基硝西泮 (7ANIZ)的高灵敏方法。方法的样品萃取率为 83.6 % ;线性范围为 10～ 5 0 0 μg L ;检出限 (LOD)为 1μg L ;定量限 (LOQ)为 3μg L ;RSD为 3.6 %～ 5 .8% ,回收率为 96 .3%～ 10 2 .6 %。对口服 10mg硝西泮者 96h内所排泄的尿液进行了 7ANIZ检测 ,结果表明 :本方法能满足司法鉴定的要求。

A highly sensitive method has been developed for the determination of urinary 7-aminonitrazepam (7ANIZ the major metabolite of nitrazepam, by tert-butyldimethylsilyl ( TBDMS) derivatization-gas chromatography-mass Spectrometry. The extraction. efficiency is 83.6%. The linear range is 10 similar to 500 mug/L. The limit of detection (LOD) is 1 mug/L and the limit of quantification (LOQ) is 3 mug/L. The RSD is 3.6% similar to 5.8%, and the recovery is 96.5% similar to 102.6%. 7-Aminonitrazepam in the urine sample excreted by the subject during 96 hours after oral administration of 10mg nitrazepam was measured. It has demonstrated that the method can be applied to the forensic identification.