气相色谱-质谱联用法测定食品接触材料及制品中19种邻苯二甲酸酯类化合物在橄榄油中的迁移量  

GC-MS Determination of Migration of Phthalate in Olive Oil from Food Contact Materials and Products by Gas Chromatography-Mass Spectrometry

作　　者：陈建国 陈洁如 刘在美 詹何珊 魏华[3] 保琦蓓 CHEN Jianguo;CHEN Jieru;LIU Zaimei(Ningbo Institute of Inspection and Quarantine Science and Technology,Ningbo 315200;Ningbo Joysun Product Testing Service Company,Ningbo 315000,China)

机构地区：[1]宁波检验检疫科学技术研究院,浙江宁波315200 [2]宁波中盛产品检测有限公司,浙江宁波315000 [3]宁波卫生职业技术学院,浙江宁波315100

出　　处：《浙江海洋大学学报（自然科学版）》2024年第3期234-242,共9页Journal of Zhejiang Ocean University：Natural Science

基　　金：宁波市科技计划项目(2021S195,202002N3114);浙江省基础公益研究计划项目(LGF20C090002)。

摘　　要：建立食品接触材料及制品中19种邻苯二甲酸酯在油性模拟物橄榄油中迁移量的气相色谱—质谱联用测试方法。迁移到油性模拟物中的邻苯二甲酸酯用乙腈提取,再用PSA-Silica混合填料的固相萃取小柱净化后,供仪器测定。17种邻苯二甲酸酯方法的检出限可以达到0.01 mg·kg^(-1),邻苯二甲酸二异壬酯(DINP)和邻苯二甲酸二异癸酯(DIDP)的检出限可以达到0.1 mg·kg^(-1)。17种目标物在0.02~2.00 mg·kg^(-1)、DINP和DIDP在0.20~20.0 mg·kg^(-1)线性范围内相关系数达到0.997以上,在食品模拟物试液中加入0.02,0.1,1.0 mg·kg^(-1)3个水平添加量,进行6次重复试验,结果显示回收率在88.8%~99.7%,同一水平RSD值在0.7%~6.9%之间,实验室间验证结果表明优化的方法具有较好的重复性和重现性。本方法准确、高效、简便,可用于检测油性模拟物橄榄油中邻苯二甲酸酯的迁移量。Simultaneous quantitative analytical method for determination of migration amount of 19 kinds of Phthalate in oily simulants of food contact materials and products by gas chromatography-mass spectrometry.Acetonitrile is used to extract the Phthalate migrated to the oily simulant,and then the solid phase extraction column with PSA Silica mixed packing is used for purification.Finally,gas chromatography-mass spectrometry is used for determination.The detection limits of 17 phthalate methods can reach 0.01 mg·kg^(-1),and the detection limits of DINP and DIDP can reach 0.1 mg·kg^(-1).The correlation coefficients of the targets reached more than 0.997 in the in the range of 0.20-20.0 mg·kg^(-1)for DINP and in the linear range of 0.02-2.00 mg·kg^(-1)for the other 18 targets.Three levels of 0.02,0.1,and 1.0 mg·kg^(-1)were added to the food simulant test solution and six replicates of the experiment were performed,which showed recoveries ranging from 88.8%to 99.7%,with RSDs ranging from 0.7%to 6.9%at the same level.Inter-laboratory validation results show that the optimized method has good repeatability and reproducibility.This method is accurate,efficient and simple,and can be used to detect the migration of Phthalate esters in oil-based simulants.

关 键 词：食品接触材料 气相色谱—质谱法 迁移量 邻苯二甲酸酯 

分 类 号：O656.31[理学—分析化学] TS206.4[理学—化学]