人体毛发中硝甲西泮的HPLC-MS/MS检测

目的建立测定涉毒人员毛发样本中硝甲西泮的液相色谱-质谱/质谱(HPLC-MS/MS)分析方法。方法对质谱主要参数进行优化,采用电喷雾多反应监测模式(MRM)测定不同浓度标准样品并建立标准曲线,通过准确度、灵敏度和实际案例检材的检验对方法进行评价。结果标准溶液最低检出限0.1ng/mL,线性范围宽,R²>0.999,空白毛发外添加标样回收率>80%。结论优化后的毛发样本中硝甲西泮的HPLC-MS/MS操作简便快捷,灵敏度高,重现性好,具备定性定量的适用性和可靠性。

HPLC-MS/MS Identifying Nimetazepam in Human Hair

Objective To develop a HPLC-MS/MS method for identifying the nimetazepam in human hair sampled from drugger.Methods The sampling hair was cleaned and then ground into powder that was spiked(for the blank sample)or extracted(for the drugger’s)of nimetazepam,with the received solution potentially containing nimetazepam subjected to HPLC-MS/MS analysis whose main mass spectrometric parameters were previously optimized.The standard samples were determined through electrospray plus multiple reaction monitoring(MRM)so that the standard curve was established.The method was evaluated from the items of accuracy and sensitivity,having been verified with the samples of actual cases.Results The standard solution was of minimum detection limit as 0.1ng/mL,showing wide linear range and the coefficient of determination being R²>0.999.The standard sample recovery rate was>80%for the blank hair.Positive result of nimetazepam was obtained from the samples of actual case.Conclusion HPLC-MS/MS is simple,sensitive and reproducible,demonstrating its applicability and reliability for qualitative and quantitative detection of nimetazepam.