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基于二元溶剂的离子液体辅助表面活性剂增敏乳状液微萃取测定苹果汁和苹果醋中的四种杀菌剂。

Binary-solvent-based ionic-liquid-assisted surfactant-enhanced emulsification microextraction for the determination of four fungicides in apple juice and apple vinegar.

机构信息

College of Science, China Agricultural University, Beijing, P.R. China.

出版信息

J Sep Sci. 2017 Feb;40(4):901-908. doi: 10.1002/jssc.201601001. Epub 2017 Jan 26.

Abstract

A binary-solvent-based ionic-liquid-assisted surfactant-enhanced emulsification microextraction method was developed for the separation/preconcentration and determination of four fungicides (pyrimethanil, fludioxonil, cyprodynil, pyraclostrobin) in apple juice and apple vinegar. A nonchlorinated solvent amyl acetate, which has a lower density than water, was used as the extraction solvent, and an ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate, which has a high density and low toxicity, was used as a secondary solvent mixed with the extraction solvent. After centrifugation, the binary solvent drop with a relatively high density was deposited on the bottom of the tube. Some parameters influencing the extraction efficiency of analytes such as type of extraction solvent, ratio of ionic liquid, volume of mixed solvent, type and concentration of surfactant, sample pH, NaCl concentration, and vortex time were investigated and optimized. Under the optimized conditions, the proposed method provided a good linearity in the range of 5-200 μg/L. The limits of quantification of the method were in the range of 2-5 μg/L. The relative standard deviations for interday assays were 1.7-11.9%. The method was applied to the determination of pyrimethanil, fludioxonil, cyprodynil, and pyraclostrobin in apple juice and apple vinegar samples, and the accuracy was evaluated through recovery experiments.

摘要

建立了一种基于双溶剂离子液体辅助表面活性剂增强乳状液微萃取方法,用于分离/预浓缩和测定苹果汁和苹果醋中的四种杀菌剂(嘧啶苯胺、氟啶胺、cyprodynil、吡唑醚菌酯)。使用非氯化溶剂乙酸戊酯作为萃取溶剂,密度高于水的离子液体 1-己基-3-甲基咪唑六氟磷酸盐作为与萃取溶剂混合的二次溶剂。离心后,相对密度较高的二元溶剂滴沉积在管底。考察并优化了影响分析物萃取效率的一些参数,如萃取溶剂的类型、离子液体的比例、混合溶剂的体积、表面活性剂的类型和浓度、样品 pH 值、NaCl 浓度和涡旋时间。在优化条件下,该方法在 5-200 μg/L 范围内具有良好的线性。方法的定量限在 2-5 μg/L 范围内。日内测定的相对标准偏差为 1.7-11.9%。该方法应用于苹果汁和苹果醋中嘧啶苯胺、氟啶胺、cyprodynil 和吡唑醚菌酯的测定,并通过回收率实验评估了准确性。

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