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建立了油脂中3种邻苯二甲酸酯的凝胶渗透色谱(GPC)-气质联用(GC-MS)的分析检测方法。油脂经乙酸乙酯-环己烷(体积比1∶1)溶解,GPC净化后用正己烷定容,HP-5MS毛细管色谱柱分离(30 m×0.25 mm,0.25μm),GC-MS选择离子监测模式(SIM)测定,外标法定量。分析结果表明,3种邻苯二甲酸酯在5~500 mg/kg的线性范围内,线性关系良好(R2>0.999),平均加标回收率为80.02%~103.09%,RSD为1.55%~5.02%。DBP和DEHP的检出限为0.1 mg/kg,DINP的检出限为3.0 mg/kg。该方法具有简便、高效和准确的特点。
The analytical method of gel permeation chromatography (GC-MS) was established for the determination of three kinds of phthalates in oils and fats. The crude product was dissolved in ethyl acetate-cyclohexane (1: 1 by volume). The crude product was purified by GPC and partitioned with HP-5MS capillary column (30 m × 0.25 mm, Monitoring mode (SIM) determination, external standard quantitative. The analytical results showed that the linearity of the three phthalates was good (R2> 0.999) in the linear range of 5 ~ 500 mg / kg, the average recoveries were 80.02% ~ 103.09% and the RSDs were 1.55% ~ 5.02%. The detection limit of DBP and DEHP was 0.1 mg / kg and the limit of detection of DINP was 3.0 mg / kg. The method is simple, efficient and accurate.