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顶空/气相色谱-质谱联用法测定食品接触材料中5-亚乙基-2-降冰片烯的迁移量 预览

Determination of 5-Ethylidene-2-norbornene Migration in Food Packaging Materials by Head-space/Gas Chromatography-Mass Spectrometry
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摘要 建立了顶空/气相色谱-质谱联用(HS/GC-MS)测定食品接触材料中5-亚乙基-2-降冰片烯(ENB)迁移量的方法,对前处理方法(溶剂提取-直接进样和气液平衡-顶空进样)、顶空平衡温度、顶空平衡时间进行了优化。以水、4%(体积分数)乙酸、50%(体积分数)乙醇和橄榄油作为食品模拟物,样品经食品模拟物浸泡,于顶空气液平衡后进样,经DB-5MS色谱柱(30m×0.25mm×0.25μm)分离后,采用选择离子模式进行检测,外标法定量。在优化实验条件下,ENB在0.1~10mg/L范围内呈良好的线性关系,相关系数(r)大于0.999,在0.1、1.0、10mg/L3个加标水平下,方法的回收率为92.0%~108%,相对标准偏差(RSD,n=5)为0.9%~4.0%,检出限(LOD)为0.01mg/kg,定量下限(LOQ)为0.03mg/kg。该方法准确、可靠、灵敏度高,适用于食品接触材料中ENB迁移量的测定。 A head-space/gas chromatography-mass spectrometric(HS/GC-MS)method was established for the determination of 5-ethylidene-2-norbornene migration in food packaging materials.Water,4%aqueous acetic acid solution,50%aqueous ethanol solution and olive oil were chosen as food stimulant.Samples were soaked with the food stimulant,followed by injection after gas-liquid equilibrium and separation with a DB-5 MS capillary(30 m×0.25 mm×0.25μm)column.The target was determined in selective ion mode and quantified by external standard method.The pretreatment methods(solvent extraction-direct injection and gas-liquid balance-head space injection),headspace balance temperature,and headspace balance time were optimized.Under the optimal conditions,there was a good linearity for 5-ethylidene-2-norbornene between its peak areas and concentrations in the range of 0.1-10 mg/L with correlation coefficients(r)more than 0.999.The spiked recoveries for 5-ethylidene-2-norbornene in fruits at three spiked levels of 0.1,1.0,10 mg/L ranged from 92.0%to 108%,with relative standard deviations(RSDs,n=5)of 0.9%-4.0%.The limits of detection(LOD)of this method were 0.01 mg/kg,and the limits of quantitation(LOQ)were 0.03 mg/kg.With the advantages of accuracy,reliability and high sensitivity,this method was suitable for the determination of 5-ethylidene-2-norbornene migration in food packaging materials.
作者 李少飞 熊小婷 佘文勋 陈意光 刘德云 杨培 谭建华 李慧勇 席绍峰 LI Shao-fei;XIONG Xiao-ting;SHE Wen-xun;CHEN Yi-guang;LIU De-yun;YANG Pei;TAN Jian-hua;LI Hui-yong;XI Shao-feng(Guangzhou Quality Supervision and Testing Institute,Guangzhou 510000,China)
出处 《分析测试学报》 CSCD 北大核心 2018年第11期1344-1348,共5页 Journal of Instrumental Analysis
基金 湖南省高校产业化培育项目(13CY030) 湖南省高校创新平台开放基金项目(15K066) 湖南人文科技学院产学研合作引导项目(2013CXY04) 湖南省2017年研究生创新科研项目(CX2017B779)。
关键词 5-亚乙基-2-降冰片烯(ENB) 食品模拟物 食品接触材料 顶空/气相色谱-质谱联用法(HS/GC-MS) 5-ethylidene-2-norbornene(ENB) food simulant food packaging materials head-space/gas chromatography-mass spectrometry(HS/GC-MS)
作者简介 通讯作者:谭建华,博士,高级工程师,研究方向:食品包装产品、日用化工产品检测以及色谱、质谱分析,E-mail:tanjianhua0734@aliyun.com。
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