[关键词]
[摘要]
将超声辅助离子液体/阴离子表面活性剂双水相萃取和高效液相色谱法相结合,建立一种简单、绿色、高效的分析方法用于检测虎杖中的虎杖苷和白藜芦醇。本研究以水溶性离子液体为萃取剂,以阴离子表面活性剂为成相盐,在超声的辅助作用下,目标分析物被萃取于离子液体中。实验结果表明,最佳提取条件为:以400 μL 1-丁基-3-甲基咪唑四氟硼酸盐为萃取剂,0.16 g十二烷基苯磺酸钠为成相盐,样品溶液pH 7.0,超声时间20 min,超声功率160 W。各化合物在线性范围内都具有良好的线性关系(r>0.9995),日内和日间精密度分别低于3.27%和6.31%,检出限和定量限分别为2.8~12.3和9.4~41.1 ng/mL,样品加标回收率在86.88~94.13%之间。本研究采用离子液体代替传统的有机溶剂作为萃取剂,集提取、分离和纯化于一体,具有操作简单、溶剂用量少、提取时间短等优点,可广泛应用于中药活性成分的提取与分析。
[Key word]
[Abstract]
A simple, green and efficient method for the determination of polydatin and resveratrol in Polygonum Cuspidatum was established by the ultrasound-assisted ionic liquid / anionic surfactant aqueous two-phase extraction coupled with high performance liquid chromatography. In this study, the water-soluble ionic liquid was used as the extraction solvent and the anionic surfactant was used as the salt phase, and the target analyte was extracted into the sample solution with the aid of ultrasound. The experimental results showed that the optimum extraction conditions: 400 μL of [C4MIM][BF4] was used as extraction solvent, 0.16 g of sodium dodecylbenzenesulfonate (SDBS) was used as salt phase, the pH of sample solution was 7.0, and the analyte was extracted for 20 min at 160 W. All the compounds had good linearity in the linear range (r>0.9995), and the RSDs of intra-day and inter-day precision were lower than 3.27% and 6.31%, respectively. The limits of detection (LOD) and quantification (LOQ) were 2.8~12.3 and 9.4~41.1 ng/mL, respectively, and the spiked recoveries were between 86.88% and 94.13%. In this study, ionic liquid was used as an extraction agent (instead of traditional organic solvent), which combined extraction, concentration, purification and separation. The proposed method has the advantage of simple experiment operation, less solvent consumption and short extraction time, which could be widely used in the extraction and analysis of active components in traditional Chinese medicine in the future.
[中图分类号]
[基金项目]
国家自然科学基金青年科研基金项目(51703012);国家级大学生创新创业训练计划项目(201710190039)