QTRAP LC-MS/MS同时测定毛发中20种毒品及代谢物

目的建立了毛发中20种毒品及代谢物的液相色谱-四极杆/线性离子阱质谱(QTRAP LC-MS/MS)的检测方法。方法将洗净的毛发样品粉碎后经甲醇超声提取,离心取上清液过滤膜后,以含有5mM氟化铵的水溶液和乙腈作为流动相,经Phenomenex Kinetex®Biphenyl(100×3.0 mm,2.6μm)分离,采用多反应监测(MRM)、信息依赖性采集(IDA)、增强子离子扫描(EPI),结合20种毒品EPI谱库检索的多步模式进行分析。结果20种毒品及相关代谢物在浓度范围0.02ng/mg^2ng/mg内线性良好,线性相关系数均大于0.995;方法检出限(S/N=3)为0.10ng/g^1.00ng/g;在0.05、0.20、1.00ng/mg 3个添加水平的回收率为80.1%~110.3%,相对标准偏差1.05%~6.39%。结论本方法简便、快捷、可靠、灵敏度高,可满足鉴定工作需要。

Simultaneous determination of 20 illicit drugs and metabolites in hair by QTRAP LC-MS/MS

Objective To develop a method for simultaneous determination of 20 illicit drugs and metabolites in hair by using high performance liquid chromatography-tandem hybrid triple-quadrupole linear ion trap massspectrometry(QTRAP LC-MS/MS).Methods The supernatant of washed and pulverized hair samples were purified with membrane after ultrasonic extracted by methanol and centrifuged,then separated on a Phenomenex Kinetex®Biphenyl column(100×3.0 mm,2.6μm),which was eluted by the mobile phase of 5mM ammonium fluoride-acetonitrile.A multiple reaction monitoring(MRM)as survey scan and an enhanced product ion(EPI)scan as dependent scan were performed in an information dependent acquisition(IDA)experiment.Results The linearity of 20 illicit drugs and metabolites were pretty good when the concentration was from 0.02~2ng/mg.The correlation coefficients were all above 0.995.The limits of detection(LODs,S/N=3)were 0.10~1.00 ng/g.The mean recovery rate at 0.05、0.20、1.00 ng/mg were 80.1%~110.3%and the RSD were 1.05%~6.39%.Conclusion The established method is simple,rapid,sensitive and with high reliability,and is appropriate for the identification.