Development of Manual Shaking and Ultrasound-Assisted Surfactant-Enhanced Emulsification Microextraction for Analysis of Organophosphorus Pesticides in Aqueous Samples

A novel, rapid and efficient manual shaking and ultrasound-assisted surfactant-enhanced emulsification microextraction (M-UASEME) combined with gas chromatography-flame photometric detection (GC-FPD) was developed for the extraction and determination of eight organophosphorus pesticides (OPPs) in tap water and honey samples. The main parameters that affected the extraction efficiency were investigated and optimized. Under the optimum conditions, the relative standard deviation (RSD, n = 6) ranged from 2.4 to 9.3%. Limits of detection (LOD) were varied between 0.005 and 0.05 µg L-1. Good linearity was obtained in a range of 0.5-50.0 µg L-1 for all analytes with the correlation coefficients (r) > 0.9964. Finally, the developed method was successfully applied to determine the eight pesticide residues in real samples. The recoveries of the target analytes in samples were between 82.4 and 96.7%.本研究开发了一种新颖、快速高效的手动振荡-超声辅助表面活性剂增强乳化微萃取（M-UASEME）结合气相色谱-火焰光度检测器（GC-FPD）的方法，用于自来水与蜂蜜样品中8种有机磷农药（OPPs）的萃取与测定。考察并优化了影响萃取效率的主要参数。在最优条件下，相对标准偏差（RSD，n = 6）为2.4%~9.3%，检出限（LOD）介于0.005~0.05 μg·L⁻¹之间。所有目标分析物在0.5~50.0 μg·L⁻¹范围内均表现出良好线性关系，相关系数（r）均大于0.9964。最后，所建立的方法被成功应用于实际样品中8种农药残留的测定，样品中目标分析物的加标回收率为82.4%~96.7%。