气相色谱-质谱联用测定食品中的邻苯二甲酸酯  

Determination of Phthalate Esters in Food Samples by Gas Chromatography-Mass Spectrometry

作　　者：卢春山[1] 李玮[2] 屠海云 周敏[2] 韩里明 

机构地区：[1]浙江工业大学绿色化学合成技术国家重点实验室培育基地,浙江杭州310014 [2]杭州市质量技术监督检测院,浙江杭州310019

出　　处：《分析测试学报》2010年第10期1036-1040,1047,共6页Journal of Instrumental Analysis

摘　　要：建立了食品中15种邻苯二甲酸酯类增塑剂的超声提取-固相萃取净化/GC-MS分析方法。考察了不同类食品的提取、净化方法,对检测的色谱条件进行优化,并通过基质加标校准曲线补偿邻苯二甲酸酯的基体效应。研究表明,净化后食品萃取液的基质去除率达到80%;15种邻苯二甲酸酯的方法线性范围为1～800μg/kg,相关系数大于0.998;加标样品的平均回收率为84%～115%,RSD(n=6)为5.3%～9.4%。含油脂食品的检出限为0.50～3.20μg/kg;不含油脂食品和液体食品的检出限为0.02～0.50μg/kg。该方法前处理过程简单、溶剂用量小、净化效果好,可用于不同种类食品中15种邻苯二甲酸酯类增塑剂的测定。A gas chromatography mass spectrometric（GC-MS）method was developed for the determination of 15 phthalate esters in food samples.The process of extraction and clean-up of different foods were investigated and the chromatography parameters were optimized.After extracted with hexane/acetone,the food samples without oil were directly analyzed without clean-up.The food samples with oil were prepared by ultrasonic-assisted extraction with methanol,and part of oil in the extract was removed by freezing at 4 ℃,and cleaned up with C18 and PSA SPE column.The analytes were analyzed by gas chromatography-mass spectrometry（GC-MS）.The matrix effect of phthalate esters was compensated by matrix spiked calibration.The entire clean-up process was simple and highly efficient,and the removal efficiency of soil matrix could be up to 80%.The calibration curves of 15 phthalate esters were linear in the range of 1-800 μg/kg with correlation coefficients more than 0.998.The average recoveries of the spiked samples were in the range of 84%-115% with RSDs（n=6）of 5.3%-9.4%.The detection limits of phthalate esters in food samples with or without oil were 0.50-3.20 μg/kg and 0.02-0.50 μg/kg,respectively.The method was simple,accurate,reproducible,and could be applied in the determination of phthalate esters in different kinds of food samples.

关 键 词：邻苯二甲酸酯 固相萃取 基体效应 食品 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学] TQ414.1[理学—化学]