气相色谱-质谱法测定鱼油胶囊壳中22种邻苯二甲酸酯类含量及迁移量

为测定鱼油胶囊壳中22种邻苯二甲酸酯类(PAEs)的含量及迁移量,本文建立了气相色谱-质谱检测方法(GC-MS)。胶囊壳经热水溶解,正己烷超声萃取,萃取液经氮吹浓缩后,以PAH色谱柱分离,在SIM模式下进行检测。并将该方法应用于鱼油胶囊壳中邻苯二甲酸酯的迁移研究,以精制玉米油作为食品模拟物,测定了鱼油胶囊壳中邻苯二甲酸酯的迁移量。结果表明,22种PAEs在10~500μg/L浓度范围内线性关系良好,相关系数均大于0.9987,方法定量限为10~29μg/kg;阴性样品的3个添加水平的平均回收率在82.1%~112.1%之间,相对标准偏差(RSD,n=6)为2.1%~7.7%。结果显示胶囊壳中存在明显的迁移现象。本方法适用于鱼油胶囊壳及食品模拟物中邻苯二甲酸酯类的测定。

Determination of 22 Kinds of Phthalate Esters in Fishoil Capsule Shells and Their Migration by Gas Chromatography-mass Spectrometry

A method was established for the simultaneous determination of 22 phthalate esters(PAEs)in fishoil capsuleshells by gas chromatography-mass spectrometry(GC-MS). The capsule shells were dissolved in hot water,extracted with hexane,and concentrated by nitrogen gas blowing. A total of 22 targets were separated by PAH capillary chromatographic column and detected by selected ion monitoring(SIM)mode of GC-MS. The method was applied to the migration of phthalate in fish oil capsule shell. The migration of phthalate in fish oil capsule shell was measured with refined corn oil as food simulant.The results showed that,the calibration curves were linear with correlation coefficients higher than 0.9987. The LOQs of PAEs were in the range of 10~29 μg/kg. The average recoveries of negative samples at three spiked levels were between 82.1% and 112.1% with the relative standard deviation(RSD,n=6)was 2.1%~7.7%. The significant migration in fishoil capsule shells were observed using this method.This method was suitable for the determination of phthalates in fish oil capsule shell and food simulant.