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

作　　者：胡守江[1] 杨丹[1] 王胜杰 周耀斌[1] 葛宇[1] 周静[1] HU Shou-Jiang;YANG Dan;WANG Sheng-Jie;ZHOU Yao-Bin;GE Yu;ZHOU Jing(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233,China)

机构地区：[1]上海市质量监督检验技术研究院,上海200233

出　　处：《食品安全质量检测学报》2020年第20期7262-7268,共7页Journal of Food Safety and Quality

基　　金：上海市质量技术监督局科技项目(2018-12)。

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0.02~1.00mg/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0.05mg/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。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.

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 

分 类 号：TS207.3[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]