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用于环境水中磺酰脲类除草剂磁性固相萃取的MIL-53(Fe)@聚多巴胺@FeO磁性复合材料的制备

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

作者信息

Deng Yulan, Li Aotian, Wang Yanfei, Sun Peng, Su Ping, Yang Yi

机构信息

College of Science, Beijing University of Chemical Technology, Beijing 100029, China.

Chinese Academy of Inspection and Quarantine, Beijing 100123, China.

出版信息

Se Pu. 2018 Mar 8;36(3):253-260. doi: 10.3724/SP.J.1123.2017.11041.

Abstract

Polydopamine (PDA) and MIL-53(Fe) modified FeO particles (MIL-53(Fe)@PDA@FeO 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 () no less than 0.9980. The limits of detection (LODs, =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@FeO magnetic composite is efficient and has good potential for the extraction of SUHs.

摘要

通过简单的一锅溶剂热法制备了聚多巴胺(PDA)和MIL-53(Fe)修饰的FeO颗粒(MIL-53(Fe)@PDA@FeO磁性复合材料)。将所得复合材料引入,通过磁性固相萃取(MSPE)从环境水样中快速萃取四种磺酰脲类除草剂(SUHs)。然后,通过配备光电二极管阵列检测器的高效液相色谱系统对除草剂进行分析。流动相为含有0.01%(v/v)三氟乙酸的乙腈和水的混合物,检测波长为233nm。优化了重要的萃取参数以提高萃取效率。在最佳条件下(5mL丙酮解吸溶剂、4.5min萃取时间、60mg吸附剂用量、0.5g NaCl和溶液pH 3),所建立的方法具有良好的线性,相关系数()不低于0.9980。四种SUHs的检测限(LODs,=3)为0.28 - 0.77μg/L。该方法成功用于测定三种环境水样中的四种SUHs,回收率令人满意,范围为78.8%至109.7%。因此,MIL-53(Fe)@PDA@FeO磁性复合材料高效,在萃取SUHs方面具有良好的潜力。

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