塑料桶装食用油中邻苯二甲酸酯GC-MS的测定方法

Study on the Determination Method of Phthalic Acid Esters in Plastic Bottled Edible Oil by GC-MS

为了检测塑料桶装食用油中邻苯二甲酸酯污染程度,建立了气相色谱-质谱检测食用油中邻苯二甲酸酯含量的方法。样品经正己烷溶解,弗罗里硅土固相萃取柱净化,氮气吹干,二氯甲烷定容,气相色谱-质谱联用仪测定,外标法定量。在1.0~50.0 mg/L范围内具有良好的线性关系（r〉0.999 8）,最低检测限小于0.03 mg/L;在5、10、15 mg/kg的添加水平,邻苯二甲酸酯的加标回收率在88.85%~101.83%之间,相对标准偏差在1.44%~2.77%之间;在0~24 h内测定值的相对标准偏差在2.06%之内;标准品精密度实验的相对标准偏差在0.51%之内,样品精密度实验的相对标准偏差在1.37%之内。结果表明：该方法简便、快速、稳定、灵敏、准确,适合食用油中邻苯二甲酸酯定性和定量测定。

With the aim of control the pollution of phthalic acid esters in plastic bottled edible oil,the corresponding method for phthalic acid esters by GC-MS was developed in this manuscript.The sample was dissolved in hexane and purified by florisil solid-phase extraction column.Then it measured by GC-MS,using external standard method to quantitative analysis.In the 1.0~50.0 mg/L scope,it has the good linear relationship（r〉0.999 8）;lowest detectable limit smaller than 0.03 mg/L;the recovery rate of the phthalic acid esters at 5 mg/kg,10 mg/kg and 15 mg/kg addition were ranged from 88.85% to 101.83%,the relatively standard deviation is in1.44%~2.77%.When it measured between 0 to 24 hours,the relatives standard deviation is smaller than 2.06%.This method can effectively eliminate the interference of other matrix from edible oil.The relative standard deviation of standard and sample experimental precision are within 0.51% and 1.37%.The results shows that this method is simple,rapid,stable,sensitive and accurate for qualitative and quantitative determination of phthalic acid esters from edible oil.