食用油中邻苯二甲酸酯的GC-MS测定方法研究

Determination of phthalic acid esters in edible oil by GC-MS

为了检测食用油中邻苯二甲酸酯污染程度,建立了气相色谱-质谱法检测食用油中邻苯二甲酸酯含量的方法。样品经环己烷-乙酸乙酯溶解,凝胶渗透色谱分离系统净化,减压浓缩至干,正己烷定容,气相色谱-质谱联用仪测定,外标法定量。在50μg/L^5000μg/L范围内具有良好的线性关系(R2>0.997),方法检测限小于40μg/kg;在100μg/kg^5000μg/kg的添加水平下,邻苯二甲酸酯的加标回收率在77.52%~103.10%之间,相对标准偏差在0.29%~4.68%之间;方法精密度实验的相对标准偏差在5%之内;基质加标校正曲线的定量优于标准品校正曲线。结果表明,该方法适用于食用油中邻苯二甲酸酯定性和定量测定。

In order to evaluate the pollution ofphthalic acid esters （PAEs） in edible oil, the method of determining PAEs in edible oil by GC-MS was set up. The sample was dissolved in cyclohexane-ethylacetate and purified by gel permeation chromatography （GPC）, which was trated to dry and dissolved by N-hexane. It was measured by gas chromatography-mass spectrometer （GC-MS） using external standard method. In a range of 50μg/L-5000μg/L, it had a good linear relationship （R2 〉0.997）. The detection limit of the method was lower than 40p, g/kg. Under a range of 1000μg/kg-5000p, g/kg, the recovery rate was in the range from 77.52% to 103.10%, and relative standard deviation （RSD） was between 0.29% and 4.86%. The relative standard deviation （RSD） of the precision experiment was within 5%. Quantitative results of matrix adding standard calibration curve were better than that of standard calibration curve. The results showed that this method was suitable for qualitative and quantitative determination of PAEs in edible oil.