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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
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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 广州质量监督检测研究院 
基金项目: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)
中文摘要: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-5 MS色谱柱(30 m×0.25 mm×0.25 μm)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0.1~10 mg/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、10 mg/L 3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0.01 mg/kg,定量下限(LOQ)为0.03 mg/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。
中文关键词: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)
 
Determination of 5 Ethylidene 2 norbornene Migration in Food Packaging Materials by Head space/Gas Chromatography-Mass Spectrometry
Abstract: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×0.25 μm) 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.
Key Words:5-ethylidene-2-norbornene(ENB)  food simulant  food packaging materials  head space/gas chromatography-mass spectrometry(HS/GC-MS)
引用本文: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.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[J].分析测试学报,2018,37(11):1344-1348.
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