GC-EI-MS内标法分析鱼肉中邻苯二甲酸酯

鱼肉样品以Florisil硅藻土层析柱净化后, 经气相色谱-电子轰击离子源-质谱法(GC-EI-MS)分析其中8种邻苯二甲酸酯(PAEs)含量: 邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丙酯(DPrP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二戊酯(DPeP)、邻苯二甲酸二环己基酯(DCHP)、邻苯二甲酸二己酯(DHP)、邻苯二甲酸二(2-乙基己基)酯(DEHP). 比较了外标和内标法定量, 并确定苯甲酸苄基酯为内标物; 优化了提取剂、吸附剂和洗脱剂的种类, 以及洗脱体积等样品前处理方法; 尤其对分析空白的控制问题进行了详细讨论; 准确分析了5种鱼样品中此类物质含量. 该方法的线性范围为50.0～800 μg•L^－1, 相关系数(R)大于0.99986, 相对标准偏差(Relative standard deviation, RSD)均小于12.7%, 检测限(Limit of detection, LOD)低于3.66 μg•L^－1, 样品的加标回收率为74.0%～113%. 其线性范围、相关系数、准确度、精密度和LOD等指标均满足鱼肉中多种PAEs同时分析的要求.

GC-EI-MS Internal Standard Analysis of Phthalic Acid Esters in Fish

The fish samples were cleaned up by Florisil, then analyzed by GC-EI-MS to determine eight phthalic acid esters, diethyl phthalate (DEP), dipropyl phthalate (DPrP), dibutyl phthalate (DBP), butyl benzyl phthalate (BBP), dipentyl phthalate (DPeP), dicyclohexyl phthalate (DCHP), dihexyl phthalate (DHP) and diethyl hexyl phthalate (DEHP). The external standard and internal standard method were compared, and the pretreatment method was optimized. Especially, the problem of analytical blank control in this experiment was discussed carefully. The linear range of the method was 50.0～800 μg•L^－1, and the linear correlation coefficient (R) was higher than 0.99986. The relative standard deviation of the method was less than 12.7% with the recovery values ranging from 74% to 113%. The limit of detection was lower than 3.66 μg•L^－1. The linear range, accuracy, precision and limit of detection of this method can satisfy the request of simultaneous analysis of PAEs in fish by GC-EI-MS.