食品科学 ›› 2024, Vol. 45 ›› Issue (11): 285-292.doi: 10.7506/spkx1002-6630-20231010-068

• 安全检测 • 上一篇    下一篇

超高效合相色谱法快速测定食品复合包装袋中7 种异氰酸酯类化合物的残留量及迁移量

邱月,李根容,余秋玲,谭超兰,陆嘉莉,张清   

  1. (1.重庆市计量质量检测研究院,重庆 401123;2.重庆市九龙坡区疾病预防控制中心,重庆 400039)
  • 出版日期:2024-06-15 发布日期:2024-06-13
  • 基金资助:
    重庆市科技局科研院所绩效激励引导专项(cstc2022jxjl50001);重庆市市场监督管理局科研计划项目(CQSJKJ2022040); 重庆市市场监督管理局科研计划项目(CQSJKJDW2023003)

Rapid Determination of Residues and Migration of Seven Isocyanate Compounds in Food Composite Packaging Bags by Ultra-high Performance Convergence Chromatography

QIU Yue, LI Genrong, YU Qiuling, TAN Chaolan, LU Jiali, ZHANG Qing   

  1. (1. Chongqing Academy of Metrology and Quality Inspection, Chongqing 401123, China; 2. Jiulongpo District Center for Disease Control and Prevention, Chongqing 400039, China)
  • Online:2024-06-15 Published:2024-06-13

摘要: 目的:建立一种超高效合相色谱(ultra-high performance convergence chromatography,UPC2)法快速检测食品复合包装袋中7 种异氰酸酯类化合物的残留量和迁移量。方法:采用ACQUITY UPC2 HSS C18 SB色谱柱进行分离,流动相CO2-甲醇进行梯度洗脱,柱温40 ℃,系统背压13.10 MPa,二极管阵列检测器测定,外标法定量。结果:在最优条件下,7 种异氰酸酯类化合物可在2 min内实现基线分离,检出限为1.0~3.0 μg/kg,定量限为5.0~10.0 μg/kg。在10、125 μg/kg和625 μg/kg 3 个加标水平下,7 种异氰酸酯类化合物的加标回收率为85.1%~108.4%,相对标准偏差为0.7%~6.5%。采用本方法测定40 批次市售食品复合包装袋样品,在7 批次样品中发现有异氰酸酯类化合物残留,其中2,4-甲苯二异氰酸酯和2,6-二异丙基苯异氰酸酯的残留量相对较高,但这7 批次阳性样品中异氰酸酯类化合物的迁移量均未检出。结论:本方法的建立可为后续食品复合包装袋中异氰酸酯类化合物的残留量及迁移量测定提供技术支持。

关键词: 超高效合相色谱;食品复合包装袋;异氰酸酯类化合物;残留量;迁移量

Abstract: An ultra-high performance convergence chromatography (UPC2) method was developed to rapidly determine the residues and migration of seven isocyanate compounds in food composite packaging bags. The separation was performed on an ACQUITY UPC2 HSS C18 SB column using gradient elution with a mobile phase consisting of CO2 and methanol. The column temperature was 40 ℃, and the system back pressure was 13.10 MPa. The analytes were detected by a photo diode array (PDA) detector and quantified by an external standard method. The results showed that under the optimal conditions, baseline separation of the seven isocyanate compounds could be achieved within 2 min. The detection limits were in the range of 1.0–3.0 μg/kg, and the quantitation limits were in the ranged from 5.0 to 10.0 μg/kg. At spiked levels of 10, 125 and 625 μg/kg, the recoveries of the isocyanate compounds ranged from 85.1% to 108.4%, and the relative standard deviations (RSDs) ranged from 0.7% to 6.5%. The developed method was used to determine 40 batches of food composite packaging bag samples. Isocyanate compounds residues were found in 7 batches, among which the contents of TDI and DPI residues were relatively high, but no isocyanates were found to migrate from these positive samples. The establishment of this method can provide technical support for the determination of the residues and migration of isocyanate compounds in food composite packaging bags.

Key words: ultra-high performance convergence chromatography; food composite packaging bags; isocyanate compounds; residues; migration

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