目的 建立气相色谱-质谱(GC-MS)法测定食品接触材料及制品中2-甲基-2-丙烯酸-1,2-乙二醇酯(EGDMA)、1,4-丁二醇二甲基丙烯酸酯(BDDMA)和2,6-萘二甲酸二甲酯(NDC)共三种酯类单体迁移量的方法,为食品接触材料及制品中相关物质的风险监控提供技术支持。方法 食品接触材料样品经迁移试验后,所得水基模拟物浸泡液和橄榄油模拟物浸泡液分别经二氯甲烷和乙腈萃取后测定,95%乙醇食品模拟物的浸泡液直接进样。结果 三种酯类单体的分离效果良好,EGDMA和BDDMA在水基模拟物、95%乙醇模拟物、橄榄油模拟物中的检出限为0.005~0.007 mg/kg,定量限为0.015~0.020 mg/kg,线性范围为0.01~0.50 mg/kg。NDC在水基模拟物、95%乙醇模拟物、橄榄油模拟物中的检出限为0.003~0.005 mg/kg,定量限为0.010~0.015 mg/kg,线性范围为0.01~0.50 mg/kg。三个浓度水平下的加标回收率结果为82.5%~110.7%,相对标准偏差(RSD)为2.3%~7.8%。结论 该方法具有较好的准确度和精密度,适用于食品接触材料及制品中三种酯类单体的测定。
Abstract
The work aims to establish a gas chromatography-mass spectrometry (GC-MS) method for simultaneously determining the migration of three ester monomers, namely ethylene glycol dimethacrylate (EGDMA), 1,4-butanediol dimethacrylate (BDDMA) and dimethyl-2,6-naphthalenedicarboxylate (NDC) in food contact materials and articles, so as to provide technical support for effectively controlling the risks of relevant substances in plastic food contact materials and articles. After the migration test on food contact materials, the aqueous food simulant and olive oil simulant extracts were extracted with dichloromethane and acetonitrile, respectively, for subsequent analysis. The 95% ethanol food simulant was directly injected for quantification. Under optimized experimental conditions, the separation efficiency of the three ester monomers was excellent. The limits of detection (LODs) and quantification (LOQs) for EGDMA and BDDMA in aqueous, 95% ethanol, and olive oil simulants were 0.005-0.007 mg/kg and 0.015-0.020 mg/kg, respectively, with a linear range of 0.01-0.50 mg/kg. For NDC, the LODs and LOQs in the aqueous, 95% ethanol, and olive oil simulants were 0.003-0.005 mg/kg and 0.010-0.015 mg/kg, respectively, with a linear range of 0.01-0.50 mg/kg. The average spiked recoveries at three concentration were in the range of 82.5%-110.7%, and the relative standard deviations (RSDs)were 2.3%-7.8%. The method demonstrates good accuracy and precision, making it suitable for detecting the migration levels of three ester monomers in food contact materials and articles.
关键词
食品接触材料及制品 /
酯类单体 /
2-甲基-2-丙烯酸-1,2-乙二醇酯(EGDMA) /
1,4-丁二醇二甲基丙烯酸酯(BDDMA) /
2,6-萘二甲酸二甲酯(NDC) /
气相色谱-质谱法 /
迁移量
Key words
food contact materials and articles /
ester monomers /
ethylene glycol dimethacrylate (EGDMA) /
1,4-butanediol dimethacrylate (BDDMA) /
dimethyl-2,6-naphthalene dicarboxylate (NDC) /
gas chromatography-mass spectrometry (GC-MS) /
migration
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基金
广州市市场监督管理局科技项目(2025KJ05); 广州市科技项目(2023B04J0407); 广州市院士专家工作站(2024-D012)