HPLC-MS/MS测定头发中的甲基苯丙胺和N-异丙基苄胺

Determination of methamphetamine and N-isopropylbenzylamine in hair by HPLC-MS/MS

目的建立了高效液相色谱-串联质谱法同时检测头发中甲基苯丙胺和N-异丙基苄胺的方法。方法头发样品经前处理后,通过Agilent ZORBAX SB-C18(4.6 mm×150 mm,5μm)色谱柱分离,以甲醇和乙酸铵/甲酸水溶液(乙酸铵5 mmol/L,0.1%(v/v)甲酸)作为流动相,等度洗脱,采用电喷雾离子源正离子(ESI+)多反应监测(MRM)模式进行质谱分析。结果甲基苯丙胺和N-异丙基苄胺在4~200 ng/mL浓度范围内线性关系良好;在4 ng/mL、50 ng/mL、200 ng/mL三组添加样本下,添加回收率范围在90%~102%;甲基苯丙胺和N-异丙基苄胺的检出限(LOD)和定量限(LOQ)均分别为0.20 ng/mL和4 ng/mL。结论本方法对甲基苯丙胺和N-异丙基苄胺的分离具有快速、简单、准确等特点,适用于头发中二者的检验。

Objective To establish a method for simultaneous determination of methamphetamine and N-isopropylbenzylamine in hair by high performance liquid chromatography-tandem mass spectrometry.Methods The research of hair samples were separated on an Agilent ZORBAX SB-C18(4.6 mm×150 mm,5μm)column with methanol and an amine acetate/formic acid solution(acetic acid amine 5 mmol/L,0.1%(v/v))as the mobile phase by isocratic elution.Mass spectrometry was performed using an electrospray ion source positive ion(ESI+)multiple reaction monitoring(MRM)mode.Results The linear relationship was established between methamphetamine and N-isopropylbenzylamine in the concentration range of 4~200 ng/mL.The recovery was in the range 90%~102%;the detection limit(LOD)and limit of quantitation(LOQ)of methamphetamine and N-isopropylbenzylamine were 0.2 ng/mL and 4 ng/mL,respectively.Conclusion The method is fast,simple and accurate for the separation of methamphetamine and N-isopropylbenzylamine.It is suitable for the test of both in hair.