气相色谱-质谱法测定微波食品中17种邻苯二甲酸酯

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

中文关键词:  微波食品  气相色谱-质谱法  邻苯二甲酸酯类  污染水平

英文关键词:microwave food  gas chromatography-mass spectrometry  phthalates  pollution level

中文摘要:

      目的 建立气相色谱质谱法(gas chromatography-mass spectrometry, GC-MS)同时测定微波食品中17种邻苯二甲酸酯的分析方法。方法 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, 浓缩定容后经GC-MS检测, 外标法定量。结果 17种邻苯二甲酸酯在0.02~1.00 mg/L浓度范围内, 线性相关良好, 相关系数大于0.99。17种邻苯二甲酸酯的检出限为0.05 mg/kg。加标实验平均回收率为85.7%~105.2%, 相对标准偏差小于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%。结论 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同时测定。

英文摘要:

      Objective To establish a method for the determination of 17 kinds of phthalates in microwave food by gas chromatography-mass spectrometry (GC-MS). Methods Microwave food without oil was directly detected by GC-MS after hexane extraction. The oily microwave food was extracted with n-hexane acetonitrile, and purified with PSA/Silica composite glass solid-phase extraction column. After concentration and constant volume, it was detected by GC-MS and quantified by external standard method. Results The 17 kinds of phthalates had good linear correlation within the concentration range of 0.02?1.00 mg/L, and the correlation coefficient was greater than 0.99. The limits of detection 17 phthalate esters were 0.05 mg/kg. The average recovery rates of the spiked experiment were 85.7%?105.2%, and the relative standard deviations were less than 8.9%. Among 82 commercially available microwave food samples, the overall positive detection rate was 17.1%. Conclusion This method is simple, accurate and reliable, and is suitable for the simultaneous determination of 17 phthalates in microwave food.