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

GC-MS Determination of Phthalates in Canned Food 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0．1～5．0mg·L^-1（DBP、BBP、DEHP、DNOP）、0．5～25．0mg·L^-1（DINP、DIDP）范围内呈线性关系，相关系数大于0．995。方法测定限（S／N=10）：DBP、BBP、DEHP、DNOP为0．01mg·kg^-1，DINP、DIDP为1.0mg·kg^-1以罐头食品为基体，加入3种不同浓度的6种邻苯二甲酸酯标准溶液做回收试验，测得回收率在85％～130％之间，相对标准偏差〈10％。

Six phthalates （PAEs）, namely dibutyl phthalate （DBP）, benzyl-n-butyl phthalate （BBP）, di-（2- ethyl hexyl）-phthalate （DEHP）, di-n-octyl phthalate （DNOP）, di-iso-nonyl phthalate （DINP） and di-iso-decyl phthalate （DIDP）, in canned food were determined simultaneously by GC-MS under selective ion monitoring mode after separation by dispersive solid phase extraction （DSPE）. Sample of canned food was extracted ultrasonically with 10. 0 mL of n-hexane with 2 mL of acetonitrile as dispersion agent. The extract obtained was purified by DSPE using ethylene diamine-N-propylsilane （PSA） as solid phase material. After centrifuging, the supernatant solution was used for GC-MS analysis. Linearity ranges found were in the range of 0. 1- 5. 0 mg · L^-1 for DBP, BBP, DEHP and DNOP, and in the range of 0. 5-25. 0 mg · L^-1 for DINP and DIDP, with correlation coefficients over 0. 995. Determination limits （S/N= 10） of the method obtained were 0. 01 mg · L^-1 for DBP, BBP, DEHP and DNOP, and 1.0 mg · L^-1 for DINP and DIDP. Tests for recovery and precision were made by addition of standard solutions of the 6 phthalates in 3 different concentrations to canned food sample which was then analyzed by the proposed method. Values of recovery obtained were in the range of 85%- 130% with values of RSD＇s less than 10%.