GC-MS法建立血液、尿液中安定类药物的定性、定量检测方法及应用

The establishment of qualitative and quantitativedetermination method for the benzodiazepines in blood and urine by GC-MS method and its application

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SKF525a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2~50ng/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10~50ng/mL的范围内与峰面积呈良好的线性关系,R2>0.999 6,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0.34μg/mL和1.5μg/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 awas used as an internal standard,and GC-MS method which equipped with HP-5 MS 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 was0.28-10.13.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.