UPLC-MS/MS同时检测人体毛发中26种滥用药物

Simultaneous detection and quantification of 26 abuse drugs in human hair by UPLC-MS/MS

目的 建立了一种毛发中26种毒品及其代谢物的UPLC-MS/MS快速定性定量检测方法。方法 毛发经酸化甲醇(pH=3)水浴超声提取后,ACQUITY UPLC^(■)BEH C18色谱柱分离,乙腈(0.1%甲酸)-水(0.01%甲酸+0.05%氨水,体积比)梯度洗脱,电喷雾离子源正离子(ESI+)及选择反应监测模式(SRM)检测。结果 26种毒品及代谢物在0.1~40.0 ng/mg范围内线性关系良好,相关系数R^(2)均> 99.5%;方法检出限(S/N=3)在0.03~0.06ng/mg间、定量限(S/N=10)在0.1~0.2 ng/mg间;回收率(0.1 ng/mg,1.0 ng/mg,10.0 ng/mg)在68.3%~105.6%间;基质效应在84.0%~114.6%间;相对标准偏差(RSD%,n=6)在1.2%~8.3%之间;日间精密度为0.5%~8.9%。结论 本方法毛发使用量低、耗时短,与平行比较的其他提取溶剂具有更高的提取效果,现已应用于毛发检材量不足的实际案件的检验中。

Objective To establish a rapid qualitative and quantitative detection method based on UPLC-MS/MS for 26 drugs and their metabolites in human hair.Methods The hair was extracted with acidified methanol(pH = 3) in a water bath,separated on an ACQUITY UPLC^(■) BEH C18 column,gradient eluted with acetonitrile(0.1 % formic acid,volume ratio)-water(0.01 % formic acid+0.05 % ammonia,volume ratio),and detected with electrospray positive ionization and SRM mode.Results All the linear ranges for the 26 drugs and their metabolites were 0.1 ~ 40.0 ng/mg,and all the correlation coefficients were more than 0.995.The limits of detection(S/N = 3) were between 0.03 and 0.06 ng/mg and the limits of quantification(S/N = 10) were between 0.1 and 0.2 ng/mg.The recoveries(0.1 ng/mg,1.0 ng/mg,10.0 ng/mg)were in the range of 68.3 % to 105.6 %,and the matrix effects were in the range of 84.0 % to 114.6 %.The relative standard deviations(RSD,n=6) ranged from 1.2 % to 8.3 %,and the inter-day precision was ranged from 0.5 % to 8.9 %.Conclusion This method is low hair-consumption and short time-consuming,and has higher extraction effects compared with other parallel extraction methods.It has been widely used in the inspection of actual cases with insufficient hair samples.