硅胶固载离子液体基质固相分散法提取蜂房中的酚酸和黄酮类化合物

Extraction of Phenolic Acids and Flavonoids from Nidus Vespae Using Silica-supported Ionic Liquid-based Matrix Solid-phase Dispersion

摘要:

建立一种基于离子液体的基质固相分散-高效液相色谱法同时测定蜂房中的5种酚酸和黄酮类化合物。采用浸渍法制备硅胶固载离子液体吸附剂，并将其作为基质固相分散提取法的分散剂用于提取蜂房中的咖啡酸、阿魏酸、桑色素、白杨素和山奈素，通过高效液相色谱对目标化合物进行分离和测定。实验结果表明，硅胶固载离子液体-基质固相分散法的最佳提取条件为：以含10% [C6MIM]Cl的硅胶固载离子液体为分散剂，20 mL正己烷为淋洗剂，15 mL甲醇为洗脱剂，样品与分散剂质量比为1:4。各目标化合物在线性范围内呈现良好的线性关系（r>0.9995），检出限和定量限分别为0.05~0.18 μg/mL和0.17~0.59 μg/mL，日内和日间精密度(RSD)分别低于5.48%和6.60%，样品加标回收率在83.73~95.32%之间。本法结合了离子液体和基质固相分散提取法的优势，具有提取时间短，有机溶剂和样品用量少等优点，本法可广泛应用于药用动植物中酚酸和黄酮类化合物的提取分析。

Abstract:

In this study, a new kind of silica-supported ionic liquid (S-SIL) was prepared by impregnation and employed as the dispersion adsorbent for matrix solid-phase dispersion (MSPD). This system was used for the simultaneous extraction of caffeic acid, ferulic acid, morin, chrysin, and kaempferide from Nidus Vespae (honeycomb). High-performance liquid chromatography (HPLC) was used to separate and identify the analytes. The experimental conditions for S-SIL-based MSPD were optimized. S-SIL containing 10% [C6MIM]Cl was used as dispersant, 20 mL n-hexane was used as washing solvent, and 15 mL methanol was used as the eluent. The mass ratio of sample to S-SIL was set as 1:4. The calibration curve of each target compound showed a good linear relationship within the linear range (r > 0.9995). The limits of detection and quantification were in the range of 0.05 to 0.18 μg/mL and 0.17 to 0.59 μg/mL, respectively. The relative standard deviations (RSDs) of intra-day and inter-day precision were lower than 5.48% and 6.60%, respectively. The recoveries were between 83.73% and 95.32%. Thus, a novel method of S-SIL-based MSPD combined with HPLC was developed in this study, to identify five phenolic acids and flavonoids in Nidus Vespae. Compared with other extraction methods, this method required less extraction time, sample, and organic solvent, because it combined the advantages of ionic liquid and MSPD. This method could be widely applied for the extraction of phenolic acids and flavonoids from medicinal plants and animals.