高效液相色谱-串联质谱法测定食品中邻苯二甲酸酯

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.

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

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 simultaneously.The phthalate pollution in food is serious.Relative departments should pay more attention to this situation.