色谱

色谱

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聚丙烯食品接触材料中的成核剂迁移规律研究

何敏恒1,*, 岑建斌1,2, 周朗君1, 何婉莜1, 陈鑫2   

  1. 1.广州检验检测认证集团有限公司,国家加工食品质量检验检测中心(广东), 广东 广州 511447;
    2.广检检测技术(上海)有限公司, 上海 201616
  • 收稿日期:2026-03-18
  • 通讯作者: * E-mail：heminheng@foxmail.com.
  • 基金资助:
    广东省市场监督管理局科技项目(2022CS03).

Study on migration laws of nucleating agents in polypropylene food-contact materials

HE Minheng1,*, CEN Jianbin1,2, ZHOU Langjun1, HE Wanyou1, CHEN Xin2   

  1. 1. Guangzhou Inspection and Testing Certification Group Co., National Quality Inspection and Testing Center for Processed Foods Guangdong, Guangzhou 511447, China;
    2. GTTC Testing Technology (Shanghai) Co., Ltd, Shanghai 201616, China
  • Received:2026-03-18
  • Supported by:
    Science and Technology Project of Guangdong Administration for Market Regulation (No. 2022CS03).

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摘要： 为评估聚丙烯(polypropylene, PP)食品接触材料中成核剂的迁移风险,建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定PP食品接触材料中的9种成核剂的检测方法。针对PP食品接触材料中9种成核剂在水基食品模拟物(4%乙酸、10%乙醇、20%乙醇和50%乙醇)和油基食品模拟物(95%乙醇、正己烷和橄榄油)中的迁移行为开展了系统研究。以甲酸-乙酸铵-乙腈为流动相,采用梯度洗脱模式,9种成核剂可在Phenomenex Kinetex Biphenyl色谱柱(4.6 mm×100 mm,2.6 μm)上得到良好分离。9种成核剂在给定的范围内线性关系良好,相关系数r2均大于0.9902,橄榄油模拟物的方法检出限和定量限分别为0.10~20.0 μg/kg和0.30~50.0 μg/kg,其他模拟物方法检出限和定量限分别为0.06~10.0 μg/L和0.20~25.0 μg/L。加标回收率为81%~103%,相对标准偏差为2.5%~6.0%。针对阳性样品,本研究系统分析了食品模拟物类型、暴露温度及作用时间等因素对成核剂的迁移规律的影响。结果表明,目标化合物1,3:2,4-二(3,4-二甲基)苄叉山梨醇缩醛(1,3:2,4-bis(3,4-dimethylobenzylideno) sorbitol, DMDBS)在油基模拟体系中呈现较高迁移水平,其迁移量随温度升高呈递增趋势,当温度达到60 ℃左右时,迁移过程基本达到动态平衡。本研究建立的方法操作简便、灵敏度高,可准确测定PP材料中9种成核剂的迁移量;研究结果揭示了DMDBS在油脂及高温环境下的高风险迁移特征,为评估PP食品接触材料的安全性提供了关键实验数据与理论依据。

关键词: 超高效液相色谱-串联质谱, 聚丙烯, 食品接触材料, 成核剂, 迁移规律

Abstract: To assess migration risks of nucleating agents in polypropylene (PP) food contact materials, an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for simultaneous quantification of 9 target compounds. The migration behaviors of nine nucleating agents from polypropylene (PP) food contact materials were systematically investigated in aqueous food simulants (4% acetic acid, 10%, 20%, and 50% ethanol) and oil-based food simulants (95% ethanol, n-hexane, and olive oil). Nine nucleating agents were well separated on a Phenomenex Kinetex Biphenyl column (4.6 mm×100 mm, 2.6 μm) under gradient elution with a mobile phase composed of formic acid, ammonium acetate and acetonitrile. All 9 nucleating agents showed good linearity in the given ranges. Their coefficients of determination r2 were all greater than 0.9902. The method limits of detection (LOD) and quantification (LOQ) were determined. For olive oil simulant, LODs were 0.10-20.0 μg/kg and LOQs 0.30-50.0 μg/kg. For other simulants, LODs were 0.06-10.0 μg/L and LOQs 0.20-25.0 μg/L. The recoveries ranged from 81% to 103%, while the relative standard deviations (RSDs) were 2.5%-6.0%. The effects of food simulant type, exposure temperature and contact time on the migration behavior of nucleating agents were systematically investigated using positive samples in this study. The results showed that the target compound 1,3:2,4-bis (3,4-dimethyl) benzylideno sorbitol (DMDBS) exhibited a high migration level in oil-based food simulants. Moreover, the migration amount increased with increasing temperature. The migration process basically reached dynamic equilibrium, while the temperature reached about 60 ℃. The method is simple and highly sensitive. It accurately determines the migration levels of nine nucleating agents in PP materials. The results reveal high-risk migration characteristics of DMDBS in oil and at high temperatures. This study provides key experimental data. It also provides a theoretical basis for assessing the safety of PP food contact materials.

Key words: UPLC-MS/MS, polypropylene, food contact materials, nucleating agent, migration laws

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