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建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时检测乳制品中18种邻苯二甲酸酯的方法。采用正己烷提取样品中邻苯二甲酸酯,Waters Acquilty UPLC BEH Cl8色谱柱(2.1 mm×100mm,1.7μm),0.1%甲酸水和0.1%甲酸乙腈流动相梯度洗脱程序下分离,电喷雾正电离,多反应监测模式测定,采用Waters PFCs Isolator kit消除分析系统背景干扰。在该优化方法条件下,l8种邻苯二甲酸酯中DEHP、DNOP、DNP、DINP及DIDP线性范围50～2000μg/L,其余13种线性范围5～200μg/L之间,定量限范围为1～500μg/kg,三水平加标方法回收率范围65.4%～110%,相对标准偏差(RSD)为1.9%～21%。应用该方法分析了乳制品中18种邻苯二甲酯含量,与国标气质方法相比,方法操作简单、快速,系统响应信号稳定,可以作为乳制品中18种邻苯二甲酸酯类化合物的检测方法。
To establish a method for simultaneous determination of 18 phthalates in dairy products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). The samples were extracted with n-hexane, followed by a Waters Acquil UPLC BEH Cl8 column (2.1 mm × 100 mm, 1.7 μm), gradient elution with 0.1% formic acid and 0.1% formic acid in acetonitrile. The electrospray Positive ionization, multiple reaction monitoring mode determination, using Waters PFCs Isolator kit to eliminate background interference from the analytical system. Under the optimized conditions, the linear range of DEHP, DNOP, DNP, DINP and DIDP of l8 kinds of phthalates was 50-2000μg / L and the other 13 kinds of linear range of 5-200μg / L. The limits of quantitation The recoveries ranged from 65.4% to 110% and the relative standard deviations (RSDs) ranged from 1.9% to 21%. This method was used to analyze the content of 18 kinds of phthalate esters in dairy products. Compared with GB method, the method is simple, rapid and the system response signal is stable. It can be used as 18 kinds of phthalates in dairy products Detection method.