超声辅助低共熔溶剂法提取葡萄皮中残留农药

A Green Ultrasound-assisted Dispersive Method Based on Deep Eutectic Solvent to Extract Pesticide in Grapeskin

建立超声辅助低共熔溶剂结合液液萃取技术提取葡萄皮中甲霜灵、吡虫啉、多菌灵3种农药的方法。采用ChCl-乙二醇(1∶2/mol∶mol)和ChCl-丙三醇(1∶4/mol∶mol)比例为体积比1∶1混合体系,用量2 mL,超声时间5 min,pH值为5,进行提取。色谱条件,色谱柱:Venusil MP C18(250 mm×4.6 mm,5μm);流速:1.0 mL/min;柱温:30℃;检测波长:280 nm和210 nm;进样量:20μL;流动相:甲醇(A)-0.05%磷酸水溶液(B);梯度洗脱。多菌灵、吡虫啉、甲霜灵的提取回收率分别为多菌灵91%,吡虫啉112%,甲霜灵85%。3种成分在线性范围内关系良好。超声辅助低共熔溶剂结合液液萃取方法能有效地提取出葡萄皮中甲霜灵、吡虫啉、多菌灵3种农药。

A kind of green ultrasound-assisted dispersive liquid-liquid microextraction method was established to extract the residues of metalaxyl,imidacloprid and carbendazim in grapeskin.The sample was extracted by a mixture of choline chloride and ethylene glycol(1∶2/mol∶mol)and choline chloride and glycerol(1∶4/mol∶mol)with the volume ratio of 1∶1 through ultrasonic for 5 min with volume of 2 mL and pH of 5.The chromatographic separation was performed on a Venusil MP C18(250 mm×4.6 mm,5μm)at 30℃with methanol(A)-0.05%phosphoric acid aqueous solution(B)as mobile phase in gradient elution mode.The wavelength of 280 nm and 210 nm were utilized.The extraction recovery rates of metalaxyl,imidacloprid and carbendazim were 91%,112%and 85%respectively.The three components showed good linear relationships and the recovery rates can meet the requirements of the method.The present experiment suggests that DESs are efficiently extract solvents in ultrasound-assisted dispersive liquid-liquid microextraction method for residual analysis of metalaxyl,imidacloprid and carbendazim in grapeskin.