食品科学 ›› 2023, Vol. 44 ›› Issue (10): 359-367.doi: 10.7506/spkx1002-6630-20220406-052

• 安全检测 • 上一篇    下一篇

食品接触用橡胶中18 种多环芳烃的测定及迁移分析

童星,曾莹,陈银卿,刘宜奇,曾少甫,商贵芹,李丹,胡长鹰,王志伟   

  1. (1.暨南大学包装工程学院,广东省普通高校产品包装与物流重点实验室,广东 珠海 519070;2.广州海关技术中心,广东 广州 510623;3.暨南大学理工学院食品科学与工程系,广东 广州 510632;4.暨南大学力学与建筑工程学院,广东 广州 510632;5.常州进出口工业及消费品安全检测中心,江苏 常州 213000)
  • 出版日期:2023-05-25 发布日期:2023-06-02
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFC1603205;2018YFC1603200); 广东省重点领域研发计划项目(B2019B020212002);2018年度食品安全国家标准立项计划项目(spaq-2018-031)

Determination and Migration Analysis of 18 Polycyclic Aromatic Hydrocarbons in Food Contact Rubber

TONG Xing, ZENG Ying, CHEN Yinqing, LIU Yiqi, ZENG Shaofu, SHANG Guiqin, LI Dan, HU Changying, WANG Zhiwei   

  1. (1. Key Laboratory of Product Packaging and Logistics of Guangdong Higher Education Institutes, College of Packaging Engineering, Jinan University, Zhuhai 519070, China; 2. Guangzhou Customs Technology Center, Guangzhou 510623, China; 3. Department of Food Science and Engineering, School of Science and Technology, Jinan University, Guangzhou 510632, China; 4. School of Mechanics and Construction Engineering, Jinan University, Guangzhou 510632, China; 5. Changzhou Safety Testing Center for Entry-Exit Industrial and Consumable Products, Changzhou 213000, China)
  • Online:2023-05-25 Published:2023-06-02

摘要: 建立气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)联用仪同时测定食品接触用橡胶中18 种多环芳烃(polycyclic aromatic hydrocarbons,PAHs)残留量和迁移量的方法。采用硅胶固相萃取柱对橡胶提取液净化;正己烷对迁移液进行提取,经DB-EUPAH(60 m×250 μm,0.25 μm)色谱柱分离,采用选择离子扫描模式进行检测,内标法定量。结果表明,18 种PAHs的色谱分离效果好,在0.05~0.5 mg/L质量浓度范围内线性关系良好,检出限均不高于0.01 mg/L,定量限均不高于0.05 mg/L,残留量和迁移量3 个水平回收率均在61.3%~102.2%之间,相对标准偏差(n=6)为0.5%~9.1%。对34 批食品接触用橡胶进行检测,在10 批样品中共检出16 种PAHs,总残留量在0.24~16.97 mg/kg之间。迁移结果表明:在不同实验温度下,均未检测到橡胶中PAHs向4%乙酸溶液和10%乙醇溶液中的迁移;当食品模拟物为50%乙醇溶液时,检出多种PAHs的迁移量,随着温度的升高,PAHs迁出数目增多,其迁移速率和迁移量显著增大。食品接触用橡胶中PAHs的残留及其可能向食品中迁移所带来的安全性问题不容忽视。

关键词: 气相色谱-质谱联用;食品接触用橡胶;多环芳烃;残留量;迁移;食品安全

Abstract: A method was developed for the simultaneous determination of the residues and migration of 18 polycyclic aromatic hydrocarbons (PAHs) in food contact rubber by gas chromatography-mass spectrometry (GC-MS). The rubber extract was cleaned up by solid phase extraction (SPE) with a silica gel column. The migration solution was extracted with hexane, separated on a DB-EUPAH column (60 m × 250 μm, 0.25 μm), detected in the selective ion monitoring (SIM) mode, and quantified by an internal standard method. The results showed that good chromatographic separation of the 18 PAHs was achieved. The calibration curves showed good linearity in the concentration range of 0.05–0.5 mg/L. The limits of detection (LOD) were less than 0.01 mg/L, and the limits of quantification (LOQ) were less than 0.05 mg/L. The average recoveries for PAHs residues and migration at three spiked levels ranged from 61.3% to 102.2%, and the relative standard deviations (RSDs, n = 6) were 0.5%–9.1%. A total of 16 PAHs were detected in 10 of the 34 batches of food contact rubber tested with total residues ranging from 0.24 to 16.97 mg/kg. No PAHs were found to be migrated from the rubber to 4% acetic acid and 10% ethanol at different experimental temperatures. Many PAHs were found to be migrated to 50% ethanol as a food simulant. The number of PAHs migrated increased with an increase in temperature, and the rate and amount of migration increased significantly. The safety problems caused by the residues of PAHs in food contact rubber and their migration to foods cannot be neglected.

Key words: gas chromatography-mass spectrometry; polycyclic aromatic hydrocarbons; food contact rubber; residues; migration; food safety

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