低共熔溶剂液相微萃取技术测定5种杀菌剂农药残留分析方法

A Liquid-phase Microextraction Method Based on Deep Eutectic Solvents Determination for Five Kinds of Fungicides Residues

摘要:

本文建立了低共熔溶剂液相微萃取高效液相色谱法测定5种杀菌剂（三唑醇、嘧霉胺、三唑酮、烯唑醇、嘧菌环胺）的农药残留分析方法，以苯酚作为氢键给体，氯化胆碱作为氢键受体组合而成的低共熔溶剂作为提取溶剂，THF作为分散剂，形成浑浊小液滴，目标分析物被萃取到微量的DESs相中，经过离心，吸取DESs相进高效液相色谱分析。对影响萃取效率的重要因素进行选择和优化。研究表明，氯化胆碱与苯酚在1:2的比率形成的低共熔溶剂萃取效果最好，同时，在最佳的萃取条件（样品容量为5 mL，DES2为150 μL，THF为150 μL，超声时间为20 min，离心时间为10 min）下进行添加回收率实验，回收率在73.7%~102.3%之间，相对标准偏差（RSD）为0.7%~7.1%，最小检出限（LOD）0.026~0.052 μg/L。为实际检测残留农药提供安全可靠的提取和分离技术，减少有机溶剂的使用对环境及人体健康构成的危害。

Abstract:

A method was developed for the determination of five fungicide residues (triadiconazole, pyrimethanil, triadimefon, carbazole, and cyprodinil) by high performance liquid chromatography with deep eutectic solvent as extraction in liquid-phase microextraction. A DES containing phenol as a hydrogen bond donor and choline chloride as a hydrogen bond acceptor was used as the extraction solvent. THF was used as a dispersant solvent to form small droplets of turbidity. The target analyte was extracted into trace DESs phase. After centrifugation, the upper DESs phase was subjected to high-performance liquid chromatography for analysis. Various parameters affecting extraction efficiency were investigated and optimized. The results were shown that the DESa molar ratio of choline chloride and phenol 1:2 is the best extraction efficiency. Under the optimum conditions are as follows: sample volume 5 mL, DES2 150 μL, and THF 150 μL, ultrasonic time 20 min and centrifugation time 10 min. The recoveries were between 73.7%~102.3%, the relative standard deviations (RSDs) were between 0.7%~7.1%, and the low limits of detection (LOD) were 0.026~ 0.052 μg/L.