食品科学 ›› 2020, Vol. 41 ›› Issue (24): 287-294.doi: 10.7506/spkx1002-6630-20191113-164

• 安全检测 • 上一篇    下一篇

气相色谱-质谱联用法检测食品复合包装材料中17 种丙烯酸酯类单体的残留量及迁移量

张勤军,贝荣华,张泓,胡长鹰   

  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.国家食品安全风险评估中心,北京 100022;4.暨南大学理工学院,广东 广州 510632)
  • 出版日期:2020-12-25 发布日期:2020-12-28
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFC1603205;2018YFC1603200); 国家自然科学基金面上项目(31571762);广东省重点领域研发计划项目(2019B020212002)

Determination of Residues and Migration of 17 Acrylate Monomers in Food Composite Packaging Materials by Gas Chromatography-Mass Spectrometry

ZHANG Qinjun, BEI Ronghua, ZHANG Hong, HU Changying   

  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 Technical Center, Guangzhou 510623, China;3. China National Center for Food Safety Risk Assessment, Beijing 100022, China;4. College of Science and Technology, Jinan University, Guangzhou 510632, China)
  • Online:2020-12-25 Published:2020-12-28

摘要: 建立气相色谱-质谱联用同时测定食品复合包装材料中17 种丙烯酸酯类单体的残留量及向油性模拟物异辛烷迁移量的方法。胶黏剂样品经甲醇稀释,复合膜样品在25 ℃低温下经甲醇超声提取1 h,阳性复合膜样品经异辛烷(60 ℃、1 h或40 ℃、0.5 h)迁移后,经HP-INNOWax色谱柱分离,采用选择离子模式进行检测,外标法定量。在优化实验条件下,17 种单体的检出限和定量限分别在0.02~0.1 mg/L和0.05~0.50 mg/L之间,残留量和迁移量在0.1、0.5、1.0、2.0 mg/L 4 个加标水平下,回收率均为70.1%~109.2%,相对标准偏差(n=6)为0.8%~9.2%。该方法前处理简单,分离度较好,能在17 min内同时检测17 种丙烯酸酯类单体。用该方法测定6 种胶黏剂和35 种不同种类食品复合膜中丙烯酸酯单体的残留量及阳性复合膜样品向异辛烷的迁移量。其中,6 种胶黏剂中均检测出丙烯酸酯类单体,8 种复合膜样品检测出有丙烯酸酯类单体残留,但此8 种复合膜中的丙烯酸酯类单体的迁移量未检出。

关键词: 丙烯酸酯类单体;胶黏剂;食品复合包装材料;残留量;迁移量

Abstract: A gas chromatography-mass spectrometry (GC-MS) method was developed for simultaneous determination of 17 acrylate monomers in food composite packaging films and their migration to isooctane as an oily food simulant. The adhesive samples were diluted with methanol, and the composite film samples were extracted ultrasonically with methanol at 25 ℃ for 1 h. After the positive composite film samples were migrated to isooctane at 60 ℃ for 1 h or at 40 ℃ for 0.5 h, chromatographic separation was performed on an HP-INNOWax column prior to analysis in the selective ion monitoring (SIM) mode. An external standard method was used for quantitation. Under the optimized conditions, the limits of detection (LODs) and limits of quantitation (LOQs) for the 17 monomers were 0.02–0.1 and 0.05–0.50 mg/L, respectively. At four spiked concentration levels of 0.1, 0.5, 1.0 and 2.0 mg/L, the recoveries for acrylate monomer residues and migration were in the range of 70.1%–109.2%, with relative standard deviations (RSDs, n = 6) ranging from 0.8% to 9.2%. This method required simple sample pretreatment, exhibited good separation performance, and could simultaneously detect the 17 acrylate monomers within 17 minutes. When it was applied to determine the residual amounts of acrylate monomers in 6 kinds of adhesives and 35 kinds of food composite packaging films and the migration amounts of positive composite films to isooctane, acrylate monomers were detected in all the adhesives and in only eight of the food composite packaging films, from which no migration of acrylate monomers was found.

Key words: acrylate monomers; adhesives; food composite packaging materials; residues; migration amount

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