色谱

色谱 ›› 2018, Vol. 36 ›› Issue (7): 659-664.DOI: 10.3724/SP.J.1123.2018.01010

• 研究论文 • 上一篇    下一篇

分子印迹固相萃取-高效液相色谱法同时检测烟叶中磺酰脲类农药残留

郑亚丽1, 顾丽莉1, 师君丽2, 张梦晓1, 孔光辉2, 李志君1, 韩毅1, 彭健1   

  1. 1. 昆明理工大学化学工程学院, 云南 昆明 650500;
    2. 云南省烟草农业科学研究院, 云南 玉溪 653100
  • 收稿日期:2018-01-08 出版日期:2018-07-08 发布日期:2014-06-03
  • 通讯作者: 顾丽莉,E-mail:liligu001@163.com
  • 基金资助:

    中国烟草总公司云南省公司科技计划项目（2017YN11）.

Determination of sulfonylurea herbicide residues in tobacco leaves by molecularly imprinted-solid phase extraction-high performance liquid chromatography

ZHENG Yali1, GU Lili1, SHI Junli2, ZHANG Mengxiao1, KONG Guanghui2, LI Zhijun1, HAN Yi1, PENG Jian1   

  1. 1. School of Chemical Engineering, Kunming University of Science and Technology, Kunming 650500, China;
    2. Yunnan Academy of Tobacco Agricultural Science, Yuxi 653100, China
  • Received:2018-01-08 Online:2018-07-08 Published:2014-06-03
  • Supported by:

    Science and Technology Planning Project of Yunnan Province Company of China National Tobacco Corporation(No. 2017YN11).

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摘要：

以氯磺隆（CS）为模板分子，甲基丙烯酸为功能单体，三羟甲基丙烷三甲基丙烯酸酯为交联剂，在二氯甲烷氛围中，经沉淀聚合制备氯磺隆分子印迹聚合物（CS-MIP）微球。将该聚合物微球作为填料制得分子印迹固相萃取柱用于样品前处理，建立了分子印迹固相萃取-高效液相色谱（MIP-SPE-HPLC）同时检测烟叶中6种磺酰脲类除草剂残留的分析方法。针对氯磺隆、甲磺隆、苄嘧磺隆、苯磺隆、胺苯磺隆和烟嘧磺隆6种磺酰脲类除草剂，在烟叶中加标0.50~50 μg/g，经氯磺隆分子印迹固相萃取柱（CS-MIP-SPE）净化和富集，高效液相色谱（HPLC）检测，其平均回收率为77.60%~102.05%，相对标准偏差为0.16%~7.07%，检出限为0.08~0.46 μg/g。将MIP-SPE-HPLC方法用于实际农药残留检测，结果表明可同时满足烟叶中多种磺酰脲类除草剂残留量的检测要求。

关键词: 多农药残留分析, 分子印迹聚合物, 高效液相色谱, 固相萃取, 磺酰脲类除草剂, 烟叶

Abstract:

Molecularly imprinted polymer (MIP) micro-particles were prepared in dichloromethane (DCM) by precipitation polymerization using chlorsulfuron (CS) as a template molecule, α -methacrylic acid (MAA) as a functional monomer, and trimethylolpropane trimethacrylate (TRIM) as a cross-linker. The pretreatment process of the tobacco sample spiked with chlorsulfuron, metsulfuron-methyl, bensulfuron-methyl, tribenuron-methyl, ethametsulfuron, and nicosulfuron, was performed using a chlorsulfuron molecularly imprinted polymer solid phase extraction (CS-MIP-SPE) column prepared with CS-MIP as the sorbent. High performance liquid chromatography (HPLC) was subsequently used for quantitative analysis. In this way, a detection technique for sulfonylurea herbicide residues in tobacco leaves was developed using CS-MIP-SPE as a pretreatment method and HPLC as an analytical tool. The results showed that the methods can be applied to the determination of the six sulfonylurea herbicides in tobacco samples. At spiking contents ranging from 0.50 to 50 μg/g, the recoveries for the six sulfonylurea herbicides in tobacco samples were 77.60%-102.05%, with relative standard deviations of 0.16% to 7.07%, and detection limits of 0.08-0.46 μg/g. With its unique advantages, the MIP-SPE-HPLC method provides a multi-residue analytical platform that can meet the requirements of simultaneous determination of sulfonylurea herbicides in tobacco samples.

Key words: high performance liquid chromatography(HPLC), molecularly imprinted polymers(MIP), multi-pesticide residue analysis, solid phase extraction(SPE), sulfonylurea herbicides, tobacco leaves

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