色谱

色谱 ›› 2018, Vol. 36 ›› Issue (3): 253-260.DOI: 10.3724/SP.J.1123.2017.11041

• 研究论文 • 上一篇    下一篇

MIL-53(Fe)@聚多巴胺@Fe3O4磁性复合材料的制备及其用于环境水样中磺酰脲类除草剂的磁固相萃取

邓玉兰1, 李傲天1, 王燕飞2, 孙鹏1, 苏萍1, 杨屹1   

  1. 1. 北京化工大学理学院, 北京 100029;
    2. 中国检验检疫科学研究院, 北京 100123
  • 收稿日期:2017-11-23 出版日期:2018-03-08 发布日期:2018-04-04
  • 通讯作者: 苏萍,Tel:(010)64441521,E-mail:suping@mail.buct.edu.cn;杨屹,Tel:(010)64441521,E-mail:yangyi@mail.buct.edu.cn
  • 基金资助:

    国家重点研发计划（2016YFF0204303）；国家自然科学基金（21675008）.

Preparation of MIL-53(Fe)@polydopamine@Fe3O4 magnetic composite for magnetic solid-phase extraction of sulfonylurea herbicides in environmental water

DENG Yulan1, LI Aotian1, WANG Yanfei2, SUN Peng1, SU Ping1, YANG Yi1   

  1. 1. College of Science, Beijing University of Chemical Technology, Beijing 100029, China;
    2. Chinese Academy of Inspection and Quarantine, Beijing 100123, China
  • Received:2017-11-23 Online:2018-03-08 Published:2018-04-04
  • Supported by:

    National Key Research and Development Program of China (No. 2016YFF0204303); National Natural Science Foundation of China (No. 21675008).

PDF

180

摘要：

制备了MIL-53（Fe）和聚多巴胺（PDA）修饰的磁性Fe3O4复合材料MIL-53（Fe）@PDA@Fe3O4，并将其作为吸附剂用于磁固相萃取-高效液相色谱法（MSPE-HPLC）检测环境水样中4种磺酰脲类除草剂（甲嘧磺隆、苄嘧磺隆、吡嘧磺隆和氯嘧磺隆）。实验优化了高效液相色谱条件（乙腈和含0.01%（体积分数）三氟乙酸的水溶液为流动相进行梯度洗脱，检测波长为233 nm）及磁固相萃取条件（洗脱剂为5 mL丙酮，萃取时间为4.5 min，吸附剂用量为60 mg，NaCl加入量为0.5 g，溶液pH值为3），在最佳条件下进行方法学考察，4种磺酰脲类除草剂均得到良好的线性关系，相关系数（r）≥0.9980。方法的检出限（LOD，S/N=3）为0.28~0.77 μg/L。将建立的方法用于3种环境水样中4种磺酰脲类除草剂的检测，其加标回收率为78.8%~109.7%。结果表明，制备的功能化复合材料结合了MIL-53（Fe）和Fe3O4的优点，可以简便快速地萃取分离环境水样中磺酰脲类除草剂。

关键词: 磁固相萃取, 高效液相色谱, 环境水样, 磺酰脲类除草剂, 金属-有机骨架, 聚多巴胺

Abstract:

Polydopamine (PDA) and MIL-53(Fe) modified Fe3O4 particles (MIL-53(Fe)@PDA@Fe3O4 magnetic composite) were prepared by simple one-pot solvothermal method. The obtained composite was introduced to rapidly extract four kinds of sulfonylurea herbicides (SUHs) from environmental water samples by magnetic solid-phase extraction (MSPE). Then the herbicides were analyzed by a high performance liquid chromatographic system equipped with a photodiode array detector. The mobile phase was a mixture of acetonitrile and water containing 0.01% (v/v) trifluoroacetic acid, and the detection wavelength was 233 nm. Significant extraction parameters were optimized to improve the extraction efficiency. Under the optimum conditions (5 mL desorption solvent of acetone, 4.5 min extraction time, 60 mg adsorbent dosage, 0.5 g NaCl and the pH 3 of the solution), the developed method showed good linearities with correlation coefficients (r) no less than 0.9980. The limits of detection (LODs, S/N=3) of the four SUHs were 0.28-0.77 μg/L. The method was successfully used to determine four SUHs in three kinds of environmental water samples with satisfactory recoveries ranging from 78.8% to 109.7%. Therefore, the MIL-53(Fe)@PDA@Fe3O4 magnetic composite is efficient and has good potential for the extraction of SUHs.

Key words: environmental water sample, high performance liquid chromatography (HPLC), magnetic solid-phase extraction (MSPE), metal-organic frameworks (MOFs), polydopamine (PDA), sulfonylurea herbicides (SUHs)

中图分类号: