分散固相萃取—气相色谱—质谱法测定罐头食品中6种邻苯二甲酸酯

DETERMINATION OF SIX PHTHALATES IN CANNED FOOD BY GC-MS WITH DISPERSIVE SOLID-PHASE EXTRACTION

以正己烷为萃取溶剂,采用乙二胺-N-丙基硅烷(PSA)固相材料分散净化技术,以气相色谱-质谱(GC-MS)在选择离子监测模式下测定罐头食品中邻苯二甲酸二丁酯(DBP)、邻苯二甲酸苄基丁基酯(BBP)、邻苯二甲酸二乙基己基酯(DEHP)、邻苯二甲酸二辛酯(DNOP)、邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)。该方法在0.1～5.0μg/mL(DBP、BBP、DEHP、DNOP)、0.5～25.0μg/mL(DINP、DIDP)范围内线性关系良好,相关系数大于0.995。对6种罐头食品进行加标回收试验,在0.2～2.0mg/kg(DBP、BBP、DEHP、DNOP)、1.0～10.0mg/kg(DINP、DIDP)添加水平下,回收率为80%～130%,相对标准偏差<10%,方法检出限(S/N=10):DBP、BBP、DEHP、DNOP为0.01mg/kg,DINP、DIDP为1.0mg/kg。

A gas chromatography-mass spectrometry method （GC-MS） under selective ion monitoring mode was established for the simultaneous determination of six phthalates in canned food. Phthalates, namely, dibutyl phthalate（DBP）, benzyl-n-butyl phthalate（BBP）, di-（2-ethylhexyl） phthalate（DEHP）, di-n-octyl phthalate（DNOP）, diisononyl phthalate（DINP） and diisodecyl phthalate （DIDP） were extracted from samples with n-hexane and the extract was cleaned up by dispersive method with primary-secondary amine （PSA） sorbent. Good linear and lower limits of detection were obtained, the linears were between 0.1-5.0μg/mL （DBP, BBP, DEHP, DNOP）, 0.5-25.0μg/mL（DINP, DIDP）, correlation coefficients were larger than 0.995, and the detection limits （S/N=10） were 0.01 mg/kg （DBP, BBP, DEHP, DNOP）, 1.0mg/kg （DINP, DIDP）. Six common representative samples were selectedto validate the method by recovery and precision. On the spike level of 0.2-2.0mg/kg （DBP, BBP, DEHP, DNOP）, 1.0-10.0 mg/kg （DINP, DIDP）, the obtained recoveries were in the range of 80-130%, with RSDs less than 10%.