顶空—气相色谱法测定食品接触材料中4-甲基-1-戊烯和1-癸烯迁移量
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1湖南省产商品质量检验研究院,湖南 长沙 410007;2湖南省产商品评审中心,湖南 长沙 410118

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陈然兵(1974—),男,本科。E-mail:316027885@qq.com

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湖南省市场监督管理局科技计划项目(编号:2024KJJH18);湖南省自然科学基金项目(编号:2024JJ8261)


Determination of migration level of 4-methyl-1-pentene and 1-decene from food contact materials using headspace-gas chromatography
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1Hunan Provincial Institute of Product and Goods Quality Inspection, Changsha, Hunan 410007, China;2Hunan Provincial Product Evaluation Center, Changsha, Hunan 410118, China

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    摘要:

    目的 探究食品接触材料中4-甲基-1-戊烯和1-癸烯单体在4%乙酸、10%乙醇、20%乙醇及50%乙醇4种食品模拟液中迁移量的测定方法。方法 对比不同极性与规格色谱柱分离效果以优选色谱柱;以峰面积为指标优化顶空平衡温度与时间;以4种食品模拟物阴性样品浸泡液为基质,进行低、中、高三水平加标试验,测定并计算目标物迁移量的回收率与相对标准偏差,进行方法学验证。结果 最佳试验条件为:HP-5毛细管色谱柱(30 m×0.25 mm,1 μm),空平衡温度80 ℃、空平衡时间40 min,氢火焰离子化检测器检测,外标法定量。两种目标物在0.01~0.1 mg/L质量浓度区间内线性良好(相关系数均在0.995以上);方法检出限(S/N=3)为0.000 1~0.002 mg/kg,定量限(S/N=10)为0.000 3~0.006 mg/kg;加标回收率为81.0%~109%,相对标准偏差(n=6)为1.3%~9.8%。结论 该方法具有便捷、灵敏的优势,且准确度与精密度良好,可满足食品接触用塑料材料中4-甲基-1-戊烯和1-癸烯单体迁移量的检测需求。

    Abstract:

    Objective This study aims to establish an analytical method for detecting the migration levels of 4-methyl-1-pentene and 1-decene monomers from food contact materials into four food simulants, including 4% acetic acid, 10% ethanol, 20% ethanol, and 50% ethanol.Methods Chromatographic columns of different polarities and specifications are compared to select the optimal column. The headspace equilibrium temperature and equilibrium time are optimized using peak area as the evaluation index. Methodological validation is performed by conducting recovery experiments at low, medium, and high spiking levels using the soaking solutions of the negative sample of the four food simulants as the matrix, and the recoveries and relative standard deviations of the migration levels of target analytes are determined and calculated.Results The optimal experimental conditions are as follows: HP-5 capillary chromatographic column (30 m×0.25 mm, 1 μm), headspace equilibrium temperature of 80 ℃, equilibrium time of 40 min, detection by flame ionization detector (FID), quantification by the external standard method. Both target compounds exhibit good linearity in the concentration range of 0.01~0.1 mg/L, with correlation coefficients all greater than 0.995. The limits of detection (LOD, S/N=3) range from 0.000 1 to 0.002 mg/kg, and the limits of quantification (LOQ, S/N=10) range from 0.000 3 to 0.006 mg/kg. The spiked average recoveries range from 81.0% to 109%, with relative standard deviations (RSD, n=6) of 1.3%~9.8%.Conclusion This method is convenient and sensitive, with satisfactory accuracy and precision. It is suitable for the determination of 4-methyl-1-pentene and 1-decene monomer migration levels in plastic materials for food contact.

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柳阿芳,陈然兵,李政,等.顶空—气相色谱法测定食品接触材料中4-甲基-1-戊烯和1-癸烯迁移量[J].食品与机械,2026,(7):83-89.
Liu Afang, Chen Ranbing, Li Zheng, et al. Determination of migration level of 4-methyl-1-pentene and 1-decene from food contact materials using headspace-gas chromatography[J]. Food & Machinery,2026,(7):83-89.

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  • 收稿日期:2026-04-10
  • 最后修改日期:2026-07-11
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  • 在线发布日期: 2026-07-25
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