目的 运用气相色谱-质谱(GC-MS)法建立人体血液和尿液中安定类(苯二氮卓类,Benzodiazepines,BZDs)药物及其代谢物含量检测方法.方法 将无任何服用安定类药物史的志愿者尿样或血样中安定类药物,经碱性条件下水解后固相萃取(solid phase extraction,SPE)法提取,以SKF525 a作为内标,运用配有HP-5MS型弱极性色谱柱的GC-MS法并选择离子扫描模式(SIM)和全扫描模式(Full Scan)对14种安定类药物进行定性定量分析.结果 血液:14种安定类药物在2～50 ng/mL的范围内与峰面积呈良好的线性关系,R2＞0.999 0,平均回收率为96.63～103.06,标准偏差(Standard Deviation,SD)为0.04～6.92,相对标准偏差(relative standard deviation,RSD)为0.33～8.16％.尿样:14种安定类药物在10～50 ng/mL的范围内与峰面积呈良好的线性关系,R2＞0.9996,平均回收率为93.75～100.79,SD值0.04～3.56,RSD值为0.28％～10.13％.案件样品尿液中检测出地西泮及其代谢产物去甲地西泮成分,检出含量分别为0.34 μg/mL和1.5 μg/mL.结论 本方法精密度、准确度以及检测灵敏度高,准确定性定量,适合于安定类药物在血液、尿液中的定性定量.%Objective A content determination method for benzodiazepines (BZDs) and their metabolites in human blood and urine was established by gas chromatography-mass spectrometry (GC-MS) method.Methods Benzodiazepines in urine or blood samples were hydrolyzed under alkaline conditions and extracted by solid phase extraction method.SKF525 a was used as an internal standard,and GC-MS method which equipped with HP-5MS type weak polarity chromatographic column was used and ion scan mode and full scan mode were selected for qualitative and quantitative analysis of 14 kinds of benzodiazepines.Results Blood sample:The 14 kinds of benzodiazepines showed a good linear relationship with the peak area in the range of 2-50 ng/ml,R2＞0.999 0,the average recovery rate was 96.63-103.06;the standard deviation(SD)was 0.04-6.92;the relative standard deviation(RSD) was 0.33-8.16.Urine sample:The 14 kinds of benzodiazepines showed a good linear relationship with the peak area in the range of 10-50 ng/ml,R2＞0.999 6,the average recovery rate was 93.75-100.79;the SD value was 0.04-3.56;the RSD value was 0.28-10.13.Conclusion The method has high precision,accuracy and sensitivity,and can be accurately analyzed qualitatively and quantitatively,and it is suitable for qualitative and quantitative determination of benzodiazepines in blood and urine.
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