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液相色谱-串联质谱法同时测定食品包装用复合膜袋中3种醇类物质迁移量
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黄晓钢,陈意光,刘德云,郭旭东,宋梓峰,熊小婷,谢文缄,李泽荣,凌光耀,饶璞 广州质量监督检测研究院国家包装产品质量监督检验中心(广州)广东 广州 511447 
基金项目:广州市市场监督管理局科技项目(2020kj05)
中文摘要:采用液相色谱-串联质谱(LC-MS/MS)建立了同时测定食品包装用复合膜袋中三羟甲基丙烷、四氢-2-呋喃甲醇和1,6-己二醇的方法。按相关标准对样品进行迁移试验后,对不同性质食品模拟液进行分类处理,其中水基、酸性和醇类(10%)模拟液直接过滤,醇类(10%以上)模拟液采用氮吹降低乙醇浓度,橄榄油模拟液采用10%甲醇溶液萃取后,上机测试。采用C18色谱柱,以0.01%甲酸-乙腈为流动相,梯度洗脱的方式进行分离,在电喷雾离子源正离子(ESI+)多反应监测(MRM)模式下进行检测,外标法定量。结果表明,3种醇类化合物的线性关系良好,相关系数(r)大于0.999。在3个加标浓度水平下,方法回收率为88.9%~116%,相对标准偏差(RSD)为0.70%~5.0%。在橄榄油食品模拟物中,三羟甲基丙烷的检出限(LOD,S/N ≥ 3)和定量下限(LOQ,S/N ≥ 10)分别为20 μg/kg和40 μg/kg,四氢-2-呋喃甲醇和1,6-己二醇的LOD和LOQ分别为4 μg/kg和10 μg/kg;在其他食品模拟物中,3种化合物的LOD和LOQ分别为4 μg/L和10 μg/L。该方法简便、可靠、灵敏、稳定,涉及的食品模拟物基本覆盖相关法规和标准中规定的类型,能满足食品包装用复合膜袋中3种醇类化合物迁移量的检测需求。
中文关键词:液相色谱-串联质谱法(LC-MS/MS)  食品包装用复合膜袋  三羟甲基丙烷  四氢-2-呋喃甲醇  1,6-己二醇  迁移量
 
Simultaneous Determination of Migration of Three Alcohols in Laminated Films and Pouches for Food Packaging
Abstract:Trimethylolpropane,tetrahydrofurfuryl alcohol and 1,6-hexanediol are the raw materials or additives used in the production of laminated films and pouches for food packaging.These three substances may remain in products and migrate into food,thus affecting human health.Specific migration limits(SML) for the above three substances are clearly stipulated in the relevant standards of China.Therefore,it is extremely necessary to establish a targeted detection method for the migration of the above three alcohols in laminated films and pouches for food packaging.A liquid chromatography-tandem mass spectrometry(LC-MS/MS) was established for the simultaneous determination of trimethylolpropane,tetrahydrofurfuryl alcohol and 1,6-hexanediol in laminated films and pouches for food packaging in this paper. Laminated films and pouches were treated with different simulants according to related regulations and standards. After soaking in food simulants, the simulated samples were pretreated with appropriate manners.Water-based,acid-based and part of alcohol-based(ethanol contents are equal to or less than 10% by volume) simulated samples were directly filtered.Other alcohol-based(ethanol contents are more than 10% by volume) simulated samples were adjusted to their original volume with water after removing most of alcohol by nitrogen blowing.The olive oil simulated sample was detected after extraction with 10% methanol solution.The separation was performed on an C18 column by gradient elution with formic acid(0.01%) and acetonitrile as mobile phases.The detection was performed with electrospray ion source in positive ion(ESI+) under multi reaction monitoring(MRM) mode.Meanwhile,external standard method was used for quantitative determination.Results indicated that this method exhibited perfect linear relationships for the 3 alcohols,with their correlation coefficients(r) more than 0.999.The recoveries at three spiked levels ranged from 88.9% to 116%,with relative standard deviations(RSD) of 0.70%-5.0%.The limits of detection(LODs,S/N ≥ 3) and limits of quantitation(LOQs,S/N ≥ 10) for trimethylolpropane in olive oil were 20 μg/kg and 40 μg/kg,respectively,and the LODs and LOQs for both tetrahydrofurfuryl alcohol and 1,6-hexanediol in olive oil were 4 μg/kg and 10 μg/kg,respectively.Meanwhile,the LODs and LOQs for the 3 alcohols in other food simulants were 4 μg/L and 10 μg/L,respectively.The method is simple,reliable,sensitive and stable.The food simulants included in the method basically covered the types specified in the regulations and standards.The LODs and LOQs of the method were lower than the specific migration limits(SML) specified in the regulations and standards.The method could meet the needs for migration determination of 3 alcohols in laminated films and pouches for food packaging.
Key Words:liquid chromatography-tandem mass spectrometry(LC-MS/MS)  laminated films and pouches for food packaging  trimethylolpropane  tetrahydrofurfuryl alcohol  1,6-hexanediol  migration
引用本文:黄晓钢,陈意光,刘德云,郭旭东,宋梓峰,熊小婷,谢文缄,李泽荣,凌光耀,饶璞.液相色谱-串联质谱法同时测定食品包装用复合膜袋中3种醇类物质迁移量[J].分析测试学报,2021,40(11):1651-1656.
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