基于离子液体原位泡腾萃取法在丹参及西洋参克百威残留分析中的应用

Application of Ionic Liquid In-situ Effervescent Extraction in the Analysis of Pesticide Residues of Salvia Miltiorrhiza and Panax Quinquefolium

本研究建立了一种新颖的基于酸性离子液体的原位泡腾萃取技术的前处理方法。酸性离子液体1-丁基-3-甲基咪唑硫酸氢盐呈酸性,能与碳酸氢盐反应产生二氧化碳,起到泡腾萃取的效果,它还能与六氟磷酸铵发生离子交换作用而置换成疏水性离子液体1-丁基-3-甲基咪唑六氟磷酸盐,使其与水相分离,通过离心获取萃取相,最后通过高效液相色谱仪测定萃取相中农药的含量。考察了酸性离子液体、碳酸氢钠和氯化钠用量对萃取效率的影响,最终所得最佳条件为200 mg酸性离子液体、0.4 g碳酸氢钠和1.0 g氯化钠。在最优条件下,克百威的线性范围为0.3~4.0μg/mL,日内和日间的相对偏差(RSD)为4.6%和10.2%,丹参和西洋参在4.0μg/mL加标水平下,加标回收率为94.7%(西洋参)和74.6%(丹参),将此方法可用于不同基质中药材和饮片中农药残留的处理。

In this study,a novel in-situ effervescent extraction technology based on acidic ionic liquids was established.The acidic ionic liquid 1-butyl-3-methylimidazole bisulfate is acidic and can react with bicarbonate to produce carbon dioxide,which plays the role of effervescent extraction.It can also be replaced by ion exchange with ammonium hexafluorophosphate to form hydrophobic ionic liquid 1-butyl-3-methylimidazole hexafluorophosphate,which can be separated from water phase by centrifugation to obtain the extraction phase.Finally,the pesticide content in the extraction phase was determined by high performance liquid chromatography.The effects of the dosage of acidic ionic liquid,sodium bicarbonate and sodium chloride on the extraction efficiency were investigated.The optimal extraction conditions were as follows:200 mg acid ionic liquid,0.4 g sodium bicarbonate and 1.0 g sodium chloride.Under the optimal conditions,the linear range of was 0.3~4.0μg/mL,and the relative deviation(RSD)of intra-day and inter-day was 4.6%and 10.2%,respectively.The recoveries were 94.7%(Panax quinquefolium)and 74.6%(Salvia miltiorrhiza)at the spiked level of 4.0μg/mL.The method could be used for the treatment of pesticide residues in different substrates of Chinese medicinal materials and decoction pieces.