Zhang Yong, Mei Meng, Liu Yi, Yu Jie, Huang Xiaojia, Yuan Dongxing
Se Pu. 2014 Sep;32(9):981-7. doi: 10.3724/sp.j.1123.2014.07005.
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.
制备了一种新型硼酸酯亲和整体材料，并将其用作搅拌棒吸附萃取（SCSE）的萃取介质。通过3-丙烯酰胺基苯硼酸（APB）和二乙烯基苯（DVB）的原位共聚制备了多孔硼酸酯亲和吸附剂。为了实现对苯甲酰脲类农药的最佳萃取性能，详细研究了几个参数，包括解吸溶剂、pH值、样品基质中的离子强度、萃取和解吸时间。同时，将SCSE-APBDVB与配备二极管阵列检测器的HPLC相结合，建立了一种简单、灵敏且环境友好的测定水和果汁样品中苯甲酰脲类农药的方法。在优化的实验条件下，目标分析物在水中的检测限（S/N = 3）为0.055 - 0.11 μg/L，在果汁中为0.095 - 0.31 μg/L。该方法的精密度通过以相对标准偏差（RSD）计算的批内和批间重复性进行评估，发现RSD均低于9.0%。所建立的方法成功应用于水和果汁样品中苯甲酰脲类农药残留的测定，加标目标化合物的回收率令人满意，在75.6% - 109%范围内。结果充分表明，新型吸附剂能够通过吸附剂与分析物之间的硼 - 氮配位、氢键和疏水相互作用等多种相互作用有效地萃取苯甲酰脲类农药。
