Polydopamine(PDA)and MIL-53(Fe)modified Fe3O4particles(MIL-53(Fe)@PDA@ Fe3O4magnetic 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. Signifi-cant extraction parameters were optimized to improve the extraction efficiency. Under the opti-mum conditions(5 mL desorption solvent of acetone,4.5 min extraction time,60 mg adsor-bent 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 0.998 0. 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@Fe3O4magnetic composite is effi-cient and has good potential for the extraction of SUHs.%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.
展开▼
