基质固相分散-液相色谱-质谱法测定蔬菜中的邻苯二甲酸酯

Determination of Phthalates in Vegetables by Liquid Chromatography-Electrospray Ionization Mass Spectrometry with Matrix Solid Phase Dispersion

采用基质固相分散-液相色谱-质谱法测定保护地蔬菜中邻苯二甲酸酯（PAEs）含量，并分析了蔬菜中PAEs污染状况，研究了水和洗涤液浸泡对蔬菜中PAEs的消除效果。蔬菜样品经弗罗里硅土和石墨化碳黑研磨均匀后，用乙酸乙酯淋洗净化，再用液相色谱／电喷雾质谱法测定。PAEs的添加回收率为82．7％～105．7％；RSD为1．7％～6．1％；检出限为邻苯二甲酸二甲酯（DMP）：0．99ng；邻苯二甲酸二乙酯（DEP）：0．75ng；邻苯二甲酸二丁酯（DBP）：0．70ng；邻苯二甲酸二异辛酯（DEHP）：1．9ng。本方法前处理简单，具有较高的准确度和灵敏度。黄瓜、番茄、西葫芦中4种PAEs总量分别为2．02、1．26、0．91mg／kg；洗涤实验结果表明，水和洗涤液浸泡可显著降低蔬菜中的PAEs含量。

The contents of phthalates （PAEs） in vegetables were studied by liquid chromatography-electrospray ionization mass spectrometry with matrix solid phase dispersion. The contents of PAEs in vegetables were detected, and the reduced ratio of PAEs in vegetables after washed by water or surfactant was studied. The samples required Florisil as dispersant sorbent, graphitizand carbon black as purificant and ethyl acetate as eluting solvent, and then the samples were analyzed by liquid chromatography-electrospray ionization mass spectrometry. The result showed that the recoveries were from 82.7% to 105.7%, RSD was from 1.7% to 6. 1%, limit of detection was 0. 988 ng for dimethyl-phthalate （ DMP）, 0. 749 ng for diethyl-phthalate （ DEP）, 0. 702 ng for di-n-butyl phthalate （DBP） and 1. 920 ng for di （2-ethylhexyl） phthalate （DEHP）. The washing experiments show that after washing by water and surfactant, the contents of PAEs in vegetables are reduced remarkably.