目的 建立一种使用气相色谱-氢火焰离子化检测器（GC-FID）测定食品接触用改性共聚酯产品中螺环乙二醇迁移量的分析方法。方法 通过食品模拟物或化学替代溶剂（如体积分数95%乙醇）进行迁移试验,并针对不同模拟物种类优化样品前处理流程：水及含乙醇类模拟物经甲醇稀释后直接测试;酸性模拟物经氢氧化钠中和后以二氯甲烷萃取后测试;油脂类模拟物（以玉米油为代表）则采用甲醇-乙腈混合溶液萃取后测试。气相色谱谱图采用保留时间定性,外标法定量。结果 螺环乙二醇在2.0~10 mg/kg范围内与峰面积呈现良好线性关系,检出限（以信噪比3∶1计）为1.0 mg/kg。通过加标回收试验验证了方法的准确性,回收率为83.5%~109.2%,7次平行测定的相对标准偏差（RSD）均低于2.5%,表明方法重现性良好。结论 本方法填补了现有标准中螺环乙二醇迁移量检测的空白,满足国家卫生健康委员会2025年第1号公告对聚环己烷二亚甲基萘二甲酸酯（PCN）材料中螺环乙二醇迁移限值（≤5 mg/kg）的合规性检测需求,为行业质量控制与政府监管提供了可靠的技术支撑。
Abstract
The work aims to establish an analytical method using gas chromatography with a flame ionization detector (GC-FID) for determining the migration level of spiroglycol in modified copolyester products for food contact. Food simulants or chemical alternative solvents (e.g., 95% ethanol) were used for migration testing, with optimized sample pretreatment procedures for different simulant types: water and ethanol-containing simulants were directly injected after methanol dilution, acidic simulants required neutralization with sodium hydroxide followed by dichloromethane extraction and fat-based simulants (represented by corn oil) were extracted with a methanol-acetonitrile mixed solution. Gas chromatography involved qualification by retention time and quantification by the external standard method. Spiroglycol exhibited a good linear relationship with peak area within the concentration range of 2.0-10 mg/L. The detection limit (based on a signal-to-noise ratio of 3∶1) was 1.0 mg/kg. Spike recovery tests demonstrated method accuracy, with recoveries ranging from 83.5% to 109.2%, and the relative standard deviations (RSD) for seven parallel determinations were all below 2.5%, indicating good reproducibility. This method addresses the gap in existing standards for detecting spiroglycol migration levels. It fully meets the compliance testing requirements specified in Announcement No.1 of 2025 by the National Health Commission for the migration limit of spiroglycol (≤5 mg/kg) in poly(cyclohexanedimethylene naphthalate) (PCN) materials, providing reliable technical support for industry quality control and government regulation.
关键词
气相色谱法 /
食品接触 /
改性共聚酯 /
螺环乙二醇 /
迁移量
Key words
gas chromatography /
food contact /
modified copolyester /
spiroglycol /
migration
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基金
上海市科学技术委员会研发公共服务平台建设项目（14DZ2293000）; 上海市质量监督检验技术研究院儿童和学生用品质量安全创新团队
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