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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 an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) for the determination of 18 phthalates in oil samples. Methods The phthalates in the oil samples were extracted with acetonitrile and separated on a Waters Acquilty UPLC BEH Cl8 column. The mobile phases were eluted with 0.1% formic acid and 0.1% formic acid - acetonitrile. The mass spectra were analyzed by electrospray ionization - And multiple reaction monitoring mode determination, Waters PFCs Isolator kit eliminates background interference from the analytical system. Results The linear relationships of DEHP, DNOP, DNP, DINP and DIDP in the range of 50-2000 μg / L were good. The other 13 phthalates (DMP, DEP, DBP, DIBP, DMEP, BBP, DBEP, DCHP and DPh P) showed good linearity in the range of 5 ~ 200μg / L. The spiked recoveries ranged from 65.1% to 120% at high, middle and low levels with RSDs ranging from 1.0% to 9.3% The limit was 1.0 to 31 μg / kg (DIDP, DINP 125 μg / kg). Conclusion The method is simple, rapid and accurate and can be applied to the detection of 18 kinds of phthalates in oil samples.