硼亲和吸附剂的制备及其对苯甲酰脲类农药的萃取性能

以3-丙烯酰胺苯硼酸（APB）为单体，二乙烯基苯（DVB）为交联剂，“原位”聚合制备了聚（3-丙烯酰胺苯硼酸-二乙烯基苯）多孔硼亲和整体材料并作为搅拌饼固相萃取（SCSE-APBDVB）的萃取介质。以5种苯甲酰脲农药为目标化合物，详细考察了萃取过程中解吸溶剂、样品基底中pH值以及离子强度、萃取和解吸时间等实验条件对萃取效率的影响。在此基础上，与高效液相色谱-二极管阵列检测器联用建立了环境水样和果汁样品中苯甲酰脲农药残留的测定方法。在最佳条件下，在水样和果汁样品中，5种目标化合物的检出限（LOD，S/N=3）分别在0.055~0.11 μg/L和0.095~0.31 μg/L之间，所建立的方法具有理想的日内和日间重现性（RSD值均小于9.0%）。在对实际环境水样和果汁样品的测定中，不同加标浓度苯甲酰脲的回收率为75.6%~109%。研究表明，由于所制备吸附剂与目标化合物存在B-N配位作用、氢键和疏水等多种作用力，因此SCSE-APBDVB可对苯甲酰脲农药进行有效萃取，所建立的分析方法具有简便、灵敏和环境友好等特点。

Preparation of boronate affinity sorbent and its extraction performance for benzoylurea pesticides

A new boronate affinity monolithic material was prepared and used as the extraction medium of stir cake sorptive extraction (SCSE). The porous boronate affinity sorbent was prepared by in situ copolymerization of 3-acrylamidophenylboronic acid (APB) and divinyl benzene (DVB). To achieve optimum extraction performance for benzoylurea pesticides, several parameters, including desorption solvent, pH value, ionic strength in sample matrix, extraction and desorption times, were investigated in detail. At the same time, a simple, sensitive and environment friendly method for the determination of benzoylurea pesticides in water and juice samples was developed by the combination of SCSE-APBDVB with HPLC equipped with a diode array detector. Under the optimized experimental conditions, the limits of detection (S/N=3) for target analytes were 0.055-0.11 μg/L in water and 0.095-0.31 μg/L in juice. The precision of the proposed method was evaluated in terms of intra- and inter-assay repeatability calculated as RSD, and it was found that the RSDs were all below 9.0%. The developed method was successfully applied to the determination of benzoylurea pesticide residues in water and juice samples and satisfactory recoveries of spiked target compounds were in the range of 75.6%-109%. The results well demonstrate that the new sorbent can extract benzoylurea pesticides effectively through multi-interactions including boron-nitrogen coordination, hydrogen-bond and hydrophobic interactions between sorbent and analytes.