超高效液相色谱—串联质谱法检测油脂样品中18种邻苯二甲酸酯含量

Determination of 18 kinds of phthalic acid esters in fat samples by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法（ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS）检测油脂样品中18种邻苯二甲酸酯的含量。方法采用乙腈提取油脂样品中的邻苯二甲酸酯,经Waters Acquilty UPLC BEH Cl8色谱柱分离,以0.1%甲酸和0.1%甲酸-乙腈为流动相进行梯度洗脱;质谱采用电喷雾正电离-和多反应监测模式测定,Waters PFCs Isolator kit消除分析系统背景干扰。结果DEHP、DNOP、DNP、DINP及DIDP在50-2000μg/L范围内线性关系良好,其余13种邻苯二甲酸酯（DMP、DEP、DBP、DIBP、DMEP、BMPP、DEEP、DPP、DHXP、BBP、DBEP、DCHP和DPh P）在5-200μg/L范围内线性关系良好,高、中、低3水平加标回收率在65.1%-120%范围内,RSD为1.0%-9.3%,检出限为1.0-31μg/kg（DIDP、DINP为125μg/kg）。结论本方法操作简单、快速、准确,可适用于油脂样品中18种邻苯二甲酸酯的检测。

Objective To establish a method for determination of 18 kinds of phthalic acid esters（PAEs） in fat samples by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. Methods PAEs in samples were extracted by acetonitrile, and separated by Acquilty UPLC BEH C（18） column with the mobile phase of acetonitrile with 0.1% formic acid（A）-0.1% formic acid solution（B） for gradient elution. Mass was used electrospray ionization mode（ESI＋） and multiple reactions monitoring mode（MRM） for determination, and mass Waters PFCs Isolator kit was used to eliminate the interference in background. Results Eighteen kinds of PAEs had good linear relationships in the range of 50-2000 μg/L for DEHP, DNOP, DNP, DINP and DIDP, and 5-200 μg/L for the others 13 kinds of PAEs（DMP, DEP, DBP, DIBP, DMEP, BMPP, DEEP, DPP, DHXP BBP, DBEP, DCHP, and DPh P）, respectively. The overall recoveries spiked at low, middle and high levers were 65.1%-120%, and the relative standard deviations（RSDs） were 1.0%-9.3%. The limits of detection（LODs） were 1.0-31 μg/kg（DIDP, DINP were 125 μg/kg）. Conclusions The method is simple, rapid, and accurate, which is suitable to determine PAEs in fat samples.