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    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

    • 摘要: 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0.1~5.0 mg·L-1(DBP、BBP、DEHP、DNOP)、0.5~25.0 mg·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0.01 mg·kg-1,DINP、DIDP为1.0 mg·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%.

       

      Abstract: 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·kg-1 for DBP,BBP,DEHP and DNOP,and 1.0 mg·kg-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%.

       

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