Key Laboratory of Bioinorganic Chemistry, College of Science, Agricultural University of Hebei, Baoding 071001, Hebei, China.
Anal Chim Acta. 2010 Oct 29;679(1-2):56-62. doi: 10.1016/j.aca.2010.09.009. Epub 2010 Sep 16.
An ultrasound-assisted surfactant-enhanced emulsification microextraction (UASEME) was developed as a new approach for the extraction of organophosphorus pesticides (OPs) in water samples prior to high-performance liquid chromatography with diode array detection (HPLC-DAD). The use of a surfactant as an emulsifier in the UASEME method could enhance the dispersion of water-immiscible extraction solvent into aqueous phase and is favorable for the mass-transfer of the analytes from aqueous phase to the organic phase. Several variables that affect the extraction efficiency, including the kind and volume of the extraction solvent, the type and concentration of the surfactant, salt addition, ultrasound emulsification time and temperature, were investigated and optimized. Under the optimum experimental conditions, the calibration curve was linear in the concentration range from 1 to 200 ng mL(-1) for the seven OPs (isocarbophos, phosmet, parathion, parathion-methyl, fenitrothion, fonofos and phoxim), with the correlation coefficients (r) varying from 0.9973 to 0.9998. High enrichment factors were achieved ranging from 210 to 242. The established UASEME-HPLC-DAD method has been successfully applied for the determination of the OPs in real water samples. The limits of detection were in the range between 0.1 and 0.3 ng mL(-1). The recoveries of the target analytes over the three spiked concentration levels of the compounds (10, 50, and 100 ng mL(-1), respectively) in rain, reservoir and well water samples were between 83% and 106% with the relative standard deviations varying from 3.3% to 5.6%.
超声辅助表面活性剂增强乳化微萃取 (UASEME) 已被开发为一种新方法,用于在高效液相色谱-二极管阵列检测 (HPLC-DAD) 之前从水样中提取有机磷农药 (OPs)。在 UASEME 方法中使用表面活性剂作为乳化剂可以增强水不溶性萃取溶剂在水相中的分散,并有利于分析物从水相向有机相的传质。研究并优化了影响萃取效率的几个变量,包括萃取溶剂的种类和体积、表面活性剂的种类和浓度、加盐、超声乳化时间和温度。在最佳实验条件下,七种 OPs(异稻瘟净、甲拌磷、对硫磷、甲基对硫磷、杀扑磷、丰索磷和辛硫磷)的浓度范围为 1 至 200 ng mL(-1) 时,校准曲线呈线性,相关系数 (r) 变化范围为 0.9973 至 0.9998。实现了高富集因子,范围为 210 至 242。所建立的 UASEME-HPLC-DAD 方法已成功应用于实际水样中 OPs 的测定。检测限范围在 0.1 至 0.3 ng mL(-1) 之间。在雨水、水库和井水样品中,目标分析物在三个加标浓度水平(分别为 10、50 和 100 ng mL(-1)) 的回收率在 83%至 106%之间,相对标准偏差在 3.3%至 5.6%之间。