高效液相色谱-串联质谱法测定食品中邻苯二甲酸酯

DETERMINATION OF PHTHALIC ACID ESTERS IN FOOD BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

[目的]建立液相色谱-串联质谱联用同时测定食品中5种邻苯二甲酸酯类(PAEs)残留的方法,调查这5种物质在食品中的污染情况。[方法]用正己烷浸泡,超声振荡对样品中PAEs进行提取并净化,采用高效液相色谱-串联质谱联用法测定其中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二异辛酯(DEHP)、邻苯二甲酸二正辛酯(DOP),离子源为ESI(+),定量检测方式为多反应监测(MRM)方式,利用保留时间和碎片信号比值判断定性结果。并用建立的方法分析实际样品。[结果]5种PAEs线性相关系数r﹥0.997,变异系数在1.2%～9.3%之间,高、中、低不同水平的加标回收率在80.9%～119.8%之间。测定256种食品样品,PAEs的检出率为32.6%。[结论]该方法简便快速,精密度较高,重现性较好,可应用于食品中5种邻苯二甲酸酯类的同时测定。调查结果显示,食品中邻苯二甲酸酯类环境激素的污染比较严重,应引起有关部门的重视。

[Objective] To establish a method that determinate 5 phthalic acid esters （PAEs） simultaneously, and to study the phthalate pollution in foods. [ Methods ] 256 foods from various super-markets and stores in Shenzhen were analyzed. Food samples were soaked in hexane and placed in a super-sonic instrument for one hour to extract the phthalates. High performance liquid chromatography-tandem mass spectrometric method was used to determinate the esters after proper preparation of the samples. [ Results] The correlation coefficients were above 0.997, the range of relative standard deviation （RSD） was from 1.2% to 9.3% and the recoveries were 80.9%-119.8%. 32.6% of the samples were proved to contain the esters. [Conclusion] The method is simple, effective and accurate. It can be applied to determinate 5 PAEs in foods simultancously. The phthalate pollution in food is serious. Relative departments should pay more attention to this situation.