食品科学 ›› 2022, Vol. 43 ›› Issue (4): 305-314.doi: 10.7506/spkx1002-6630-20201114-153

• 安全检测 • 上一篇    下一篇

磺酰脲类除草剂分子印迹聚合物制备及其应用

冯格格,王猛强,李壮,佘永新,王淼,曹振,王珊珊,郑鹭飞,金茂俊,王静,邵华,金芬   

  1. (中国农业科学院农业质量标准与检测技术研究所,北京 100081)
  • 出版日期:2022-02-25 发布日期:2022-03-08
  • 基金资助:
    国家大麦青稞产业技术体系项目(CARS-05-05A-03)

Preparation and Application of Molecularly Imprinted Polymer for the Detection of Sulfonylurea Herbicides

FENG Gege, WANG Mengqiang, LI Zhuang, SHE Yongxin, WANG Miao, CAO Zhen, WANG Shanshan, ZHENG Lufei, JIN Maojun, WANG Jing, SHAO Hua, JIN Fen   

  1. (Institute of Quality Standard and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, Beijing 100081, China)
  • Online:2022-02-25 Published:2022-03-08

摘要: 采用沉淀聚合法,以甲磺隆和氯磺隆为双模板分子,4-乙烯基吡啶为功能单体,二乙烯基苯为交联剂,乙腈为致孔剂,合成对29 种磺酰脲类农药具有高选择性的分子印迹聚合物。通过扫描电镜、平衡吸附实验等对制备的印迹聚合物进行表征和测定。结果表明:分子印迹聚合物对29 种磺酰脲类农药具有特异性吸附作用,其最大表观结合量为13.21 mg/g。以此合成的聚合物作为吸附材料制备固相萃取柱,进一步建立了分子印迹固相萃取-高效液相色谱-串联质谱法,用于测定农产品中29 种磺酰脲类农药残留。该方法在2~100 μg/L 范围内,磺酰脲类除草剂峰面积与质量浓度呈良好的线性关系,相关系数(R2)大于0.999,定量限为10 μg/kg。在不同添加水平下,样品中磺酰脲类除草剂的加标回收率在74.8%~110.5%之间,相对标准偏差不高于5.3%。

关键词: 磺酰脲类除草剂;分子印迹聚合物;固相萃取;应用

Abstract: Molecularly imprinted polymers (MIPs) with high selectivity to 29 sulfonylurea pesticides were synthesized by precipitation polymerization, using metsulfuron methyl and chlorsulfuron methyl as the template molecules, 4-vinylpyridine as the function monomer, divinylbenzene as the cross-linking agent and acetonitrile as the porogen, and they were characterized by scanning electron microscopy (SEM) and equilibrium adsorption experiments. The results showed that the MIPs exhibited specific adsorption for the 29 sulfonylurea pesticides, and the maximum apparent binding capacity was 13.21 mg/g. The synthesized polymers were used as solid phase extraction sorbents to develop a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of the 29 sulfonylurea residues in agricultural products. In this method, the peak area of sulfonylurea herbicides had a good linear relationship with their concentration in the range of 2–100 μg/L with a correlation coefficient (R2) of more than 0.999, and the limit of quantitation (LOQ) was 10 μg/kg. At different spiked levels, the recoveries of sulfonylurea herbicides in samples ranged from 74.8% to 110.5% with a relative standard deviation (RSD) of not more than 5.3%.

Key words: sulfonylurea herbicides; molecularly imprinted polymer; solid phase extraction; application

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