LLE-GC-MS/MS法快速检验血及尿液中尼美西泮

Rapid determination of nimetazepam in blood and urine by LLE-GC-MS/MS

目的建立一种三重串联四级杆气相色谱质谱联用仪(GC-MS/MS)快速检验血中和尿液中尼美西泮的方法。方法对吸毒人员的血液和尿液经过液液提取(LLE)后,利用配备有HP-5MS弹性石英毛细管柱(30 m×0.25 mm×0.25μm)的三重串联四级杆气相色谱质谱联用仪(GC-MS/MS)选择多反应监测(MRM)模式进行分析,使用优化的质谱参数对待测物进行定性、定量分析。结果尼美西泮的MS/MS的质谱图特征性强,定性准确;在1~1000 ng/mL的浓度范围内呈良好线性关系(r^(2)=0.9987,n=9),检出限为0.1 ng/mL,方法回收率大于80%。结论经验证,GC-MS/MS方法高效、简便易于操作,灵敏度高,可用于血液和尿液中尼美西泮的定性定量检验。

Objective To establish a method for rapid determination of nimetazepam in blood and urine by gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS).Methods After liquid-liquid extraction(LLE),the blood and urine of drug addicts were analyzed by gas chromatography tandem mass spectrometry(GC-MS/MS)equipped with HP-5MS elastic quartz capillary column(30 m×0.25 mm×0.25μm)in multiple reaction monitoring(MRM)mode,and the optimized mass spectrometry parameters were used for qualitative and quantitative analysis.Results In this method,the concentration range was 1~1000 ng/mL(r^(2)=0.9987,n=9),which was in a good linear relationship,the detection limit was 0.1 ng/ml,and the recovery rate was more than 80%.Conclusion After verification,the developed method is efficient,simple and easy to operate and high sensitivity,and it can be used in the qualitative and quantitative determination of nimetazepam in blood and urine.