GPC-GC-MS/MS同时测定含油食品中16种邻苯二甲酸酯

Determination of 16 Phthalate Esters in Oleaginous Food by GPC-GC-MS/MS

研究建立了含油食品中16种邻苯二甲酸酯含量的凝胶渗透色谱-气相色谱-串联质谱(GPC-GC-MS/MS)测定方法。含油食品经过提取后,提取液经凝胶渗透色谱分离纯化后进GC-MS/MS检测。系统优化了样品前处理方法,净化液在GC-MS/MS多反应检测(MRM)模式下进行检测,采用外标法定量分析。结果表明:该方法在0～16 mg·kg^(-1)范围内具有良好的线性关系,相关系数R^2在0.998 64～0.999 22。含油脂样品中16种邻苯二甲酸酯的加标回收率为84.85%～107.45%;方法检出限为100～200μg·kg^(-1),相对标准偏差(n=6)在2.0%～5.0%。本方法准确、稳定、简便、重复性较好,可应用于含油脂食品中16种邻苯二甲酸酯的实际检测分析。

The method for determining the contents of 16kinds of phthalate esters in oleaginous food by gel permeation chromatography(GPC)and gas chromatography-tandem mass spectrometry(GC-MS/MS)was studied and established.After extraction,the extract was purified by GPC and detected by GC-MS/MS.The method for each matrix was optimized,the extract was determined by GC-MS/MS in multi-reaction monitoring(MRM)mode,and external standard method was applied to quantitative analysis.The results of 16 phthalate esters showed good linearity in the range of 0~16 mg·kg^-1,with correlation coefficients(R2)between 0.998 64~0.999 22.The recoveries of 16 phthalate esters were 84.85%~107.45%,the detection limit of the method is 100~200μg·kg^-1,the relative standard deviation(n=6)between 2%~5%.This method is accurate,stable,simple and reproducible for monitoring the 16 phthalate esters in oleaginous food.