食品科学 ›› 2021, Vol. 42 ›› Issue (12): 281-287.doi: 10.7506/spkx1002-6630-20201203-039

• 安全检测 • 上一篇    下一篇

三嗪类虚拟模板分子印迹聚合物的制备及其应用

巩碧钏,胡秋辉,苏安祥,徐辉,刘建辉,裴斐,杨文建   

  1. (南京财经大学食品科学与工程学院,江苏省现代粮食流通与安全协同创新中心,江苏高校粮油质量安全控制及深加工重点实验室,江苏 南京 210023)
  • 出版日期:2021-06-25 发布日期:2021-06-29
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFC1603406);江苏高校优势学科建设工程资助项目(PAPD)

Preparation and Application of Dummy Template Molecularly Imprinted Polymer in the Detection of Triazines in Fruits and Vegetables

GONG Bichuan, HU Qiuhui, SU Anxiang, XU Hui, LIU Jianhui, PEI Fei, YANG Wenjian   

  1. (Key Laboratory of Grains and Oils Quality Control and Processing, Collaborative Innovation Center for Modern Grain Circulation and Safety, College of Food Science and Engineering, Nanjing University of Finance and Economics, Nanjing 210023, China)
  • Online:2021-06-25 Published:2021-06-29

摘要: 以灭蝇胺为虚拟模板分子,甲基丙烯酸(methacrylic acid,MAA)为功能单体,三羟甲基丙烷三甲基丙烯酸酯(trimethylolpropane triacrylate,TRIM)为三元交联剂,乙腈为致孔剂,采用本体聚合法合成了三嗪类分子印迹聚合物(molecularly imprinted polymer,MIPs)。对MIPs制备工艺进行优化,灭蝇胺、MAA、TRIM的物质的量比为1∶4∶4时为最佳聚合体系。通过平衡吸附实验、红外光谱、扫描电镜等方法对聚合物进行测定和表征。吸附性能实验及Scatchard方程表明MIPs对扑草净的吸附性最好,存在2 类吸附位点,且最大表观结合量为3.13 mg/g。用MIPs制备分子印迹固相萃取柱并对洗脱条件进行优化,结合高效液相色谱法,建立了测定黄瓜、苹果和玉米中4 种三嗪类农药的检测方法。结果表明:体积分数为10%醋酸-甲醇溶液对目标农药的洗脱效果最好,该方法的检出限为0.01~0.03 ng/mL,平均回收率为81.5%~104.3%,相对标准偏差在1.3%~5.8%之间(n=3)。该方法符合检测要求,大幅提高了检测效率与精确度,为三嗪类农药残留的检测提供理论支持。

关键词: 三嗪类农药;分子印迹聚合物;虚拟模板;固相萃取

Abstract: Molecularly imprinted polymers (MIPs) were prepared by bulk polymerization with cyromazine as the virtual template molecule, methacrylic acid (MAA) as the functional monomer, trimethylolpropane trimethacrylate (TRIM) as the ternary crosslinking agent, and acetonitrile as the porogen. The optimum molar ratio of cyromazine to MAA to TRIM was determined to be 1:4:4. The as-prepared polymer was evaluated and characterized by equilibrium adsorption test, infrared spectroscopy, and scanning electron microscopy (SEM). The adsorption performance test and the Scatchard equation showed that the MIP had the best adsorption capacity toward prometryn. Two types of adsorption sites existed, and the maximum apparent binding capacity was 3.13 mg/g. A molecularly imprinted solid phase extraction (MISPE) column was prepared with the MIP, and the elution conditions were optimized. On this basis, a method for the determination of four triazine pesticides in cucumber, apple and corn was established by combining high performance liquid chromatography (HPLC). The results showed that 10% acetic acid-methanol was the best eluent for the target pesticides. The detection limits of this method were 0.01–0.03 ng/mL, and the average recoveries were 81.5%–104.3%, with relative standard deviations (RSDs) of 1.3%–5.8% (n = 3). The method could meets the requirements for the detection of pesticides with greatly improved efficiency and accuracy, which will provide theoretical support for the detection of triazine pesticide residues.

Key words: triazine pesticides; molecularly imprinted polymer; dummy template; solid phase extraction

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