Department of Applied Chemistry, China Agricultural University, Beijing 100193, PR China.
Anal Chim Acta. 2012 Oct 17;747:29-35. doi: 10.1016/j.aca.2012.08.015. Epub 2012 Aug 27.
A magnetic solid phase extraction (MSPE) method coupled with high-performance liquid chromatography (HPLC) was proposed for the determination of five sulfonylurea herbicides (bensulfuron-methyl, prosulfuron, pyrazosulfuron-ethyl, chlorimuron-ethyl and triflusulfuron-methyl) in environmental water samples. The magnetic adsorbent was prepared by incorporating Fe(3)O(4) nanoparticles and surfactant into a silica matrix according to a sol-gel procedure, which can provide surfactant free extracts during the eluting step to avoid chromatographic interference. The prepared adsorbent was used to extract the sulfonylurea herbicides in several kinds of water samples. The main factors affecting the extraction efficiency, including desorption conditions, extraction time, sample volume, and sample solution pH were optimized. Under the optimum conditions, good linearity was obtained within the range of 0.2-50.0 μg L(-1) for all analytes, with correlation coefficients ranging from 0.9993 to 0.9999. The enrichment factors were between 1200 and 1410, and the limits of detection were between 0.078 and 0.10 μg L(-1). The proposed method was successfully applied in the analysis of sulfonylurea herbicides in environmental samples (tap, reservoir, river, and rice field). The recoveries of the method ranged between 80.4% and 107.1%. This study reported for the first time the use of MSPE procedure in the preconcentration of sulfonylurea herbicides in environmental samples. The procedure proved to be efficient, environmentally friendly, and fast.
一种磁性固相萃取(MSPE)方法与高效液相色谱(HPLC)相结合,用于测定环境水样中的五种磺酰脲类除草剂(苄嘧磺隆、砜嘧磺隆、吡嘧磺隆-乙基、氯嘧磺隆-乙基和三氟啶磺隆-甲基)。磁性吸附剂是通过将 Fe(3)O(4)纳米粒子和表面活性剂掺入硅基质中,根据溶胶-凝胶法制备的,它可以在洗脱步骤中提供无表面活性剂的提取物,以避免色谱干扰。所制备的吸附剂用于提取几种水样中的磺酰脲类除草剂。优化了影响萃取效率的主要因素,包括解吸条件、萃取时间、样品体积和样品溶液 pH 值。在最佳条件下,所有分析物在 0.2-50.0 μg L(-1)范围内均获得良好的线性,相关系数在 0.9993 到 0.9999 之间。富集因子在 1200 到 1410 之间,检测限在 0.078 到 0.10 μg L(-1)之间。该方法成功应用于环境样品(自来水、水库、河流和稻田)中磺酰脲类除草剂的分析。该方法的回收率在 80.4%到 107.1%之间。本研究首次报道了 MSPE 程序在环境样品中磺酰脲类除草剂预浓缩中的应用。该程序证明是高效、环保和快速的。