气相色谱-质谱法测定微波食品中17种邻苯二甲酸酯

建立了同时测定微波食品中17种邻苯二甲酸酯的气相色谱质谱(GC-MS)分析方法。本方法首次采用将微波食品按照不含油食品和含油食品进行分类前处理。不含油微波食品经正己烷提取GC-MS直接检测；含油微波食品经正己烷-乙腈提取，PSA/Silica复合玻璃固相萃取柱净化，浓缩定容后，GC-MS检测，外标法定量。17种邻苯二甲酸酯在0.02~1.00mg/L浓度范围内，线性相关良好，相关系数(R2)大于0.99。17种邻苯二甲酸酯的检出限为0.05mg/ kg。加标实验平均回收率为85.7%~105.1%，相对标准偏差(RSD)小于8.9%。在82份市售微波食品样品检测中，总体阳性检出率为17.1%，其中DBP的检出率为9.8%，污染水平在ND~3.51mg/kg之间；DEHP的检出率为11.0%，污染水平在ND~3.26mg/kg之间；有2份样品超过国家安全限量值要求，具有一定的潜在风险。该方法简便、准确、可靠，适用于微波食品中17种邻苯二甲酸酯类物质的测定。

Determination of 17 phthalates esters in microwave food by gas chromatography-mass spectrometry

A method for the simultaneous determination of 17 phthalates esters in microwave food by gas chromatography-mass spectrometry (GC-MS) was established. In this method, microwave food was firstly classified into oil-free food and oil-bearing food. Non oil containing food was extracted by n-hexane and detected directly by GC-MS; oil containing food was extracted by n-hexane and acetonitrile, purified by PSA / silica composite glass solid phase extraction column, concentrated and fixed volume, detected by GC-MS and quantified by external standard method. 17 phthalates esters in the concentration range of 0.02-1.00mg/L had good linear correlation, and the correlation coefficient (R2) was greater than 0.99. The quantitative limit of 17 phthalates esters was 0.05mg/kg. The average recovery was 85.9% ~ 105.1% and RSD was less than 8.9%. In 82 samples of microwave food sold in the market, the overall positive detection rate was 17.1%, of which the detection rate of DBP was 9.8%, and the pollution level was Nd~3.51mg/kg; the detection rate of DEHP was 11.0%, and the pollution level was Nd ~ 3.26mg/kg; 2 samples exceeded the national risk limit value requirements, with certain potential risks. The method is simple, accurate and reliable. It is suitable for the determination of 17 phthalate esters in microwave food.