毛发中地佐辛、杜冷丁的UPLC-MS/MS检测

Determination of dezocine and pethidine in human hair by UPLC-MS/MS

建立快速检测毛发中地佐辛和杜冷丁含量的超高效液相色谱-质谱(UPLC-MS/MS)法。将清洗后的毛发样品经甲醇研磨超声提取后进行UPLC-MS/MS分析。色谱柱为Waters Acquity BEH C18(2.1 mm×100 mm,1.7μm),流动相为0.1%甲酸水-甲醇,0.4 mL/min梯度洗脱。质谱采用ESI+离子源,MRM多反应监测,测定地佐辛和杜冷丁的定性离子对和定量离子对。地佐辛和杜冷丁在0.01~8 ng/mg范围内线性关系良好,检出限均为0.005 ng/mg,定量限均为0.01 ng/mg;准确度和精密度、基质效应和提取回收率以及稳定性均符合方法学要求。本研究建立的方法可简单、快速、准确地测定毛发中地佐辛和杜冷丁的含量,可应用于地佐辛和杜冷丁滥用的相关案件分析。

A rapid analytical method for the determination of dezocine and pethidine in hair samples using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.After cleaned hair was extracted by grinding with methanol and ultrasonic,the final solution was analyzed by UPLC-MS/MS.The targets were gradient eluted on a Waters Acquity BEH C_(18)(2.1 mm×100 mm,1.7μm)column with 0.1%formic acid-water and methanol as mobile phase at a flow rate of 0.4 mL/min.The ESI^(+) ion source and multiple reaction monitoring(MRM)were used to select the qualitative and quantitative ion pairs of dezocine and pethidine.Dezocine and pethidine showed good linearity in the range of 0.01-8 ng/mg,with the limit of detection of 0.005 ng/mg and the LOQs of 0.01 ng/mg.The accuracy,precision,matrix effect,extraction recovery,and stability all met the requirements.The established method is simple,rapid,and accurate for the qualitative and quantitative determination of dezocine and pethidine in hair,which can be applied in the case analysis of dezocine and/or pethidine abuse.