[关键词]
[摘要]
本研究建立了一种磁力搅拌辅助的超临界CO2萃取法,用于提取五味子中的8种木脂素类化合物,采用高效液相色谱对目标分析物进行分离和测定。本研究以超临界CO2作为萃取溶剂,采用乙醇溶液预先浸渍样品,通过磁力搅拌促进样品与超临界CO2的充分接触,以提高传质效率。本研究对影响木脂素类化合物提取率的各个因素进行了优化,并与传统方法进行了比较。实验结果表明,各目标分析物在线性范围内具有良好的线性关系(r>0.9998),检出限和定量限为21.30~990.20 ng/mL和60.80~2992.80 ng/mL,加标样品回收率在75.00%~97.78%之间,分析结果令人满意。与其他方法相比,虽然本法在提取时间和实验成本上并不占优势,但本法所获得的提取率明显高于微波提取法和热回流提取法,并与药典方法相似,尽管本法在萃取过程中使用了少量的有机溶剂,但料液比仅为1:2,是其他方法的1/25~1/50。本法具有样品处理量大、操作简单、绿色环保、萃取效率高等优点,在工业化生产应用方面具有一定潜质,可用于中药中木脂素类化合物的提取分离。
[Key word]
[Abstract]
In this study, a magnetic stirring assisted supercritical CO2 extraction method was established and applied to the extraction of eight lignans from the fruit of Schisandra chinensis. The target analytes were separated and determined by high performance liquid chromatography (HPLC). Specifically, supercritical CO2 was used as extraction solvent, the sample was pre-impregnated with ethanol solution, and the contact between samples and supercritical CO2 was promoted by magnetic stirring to improve mass transfer efficiency. Then, various factors affecting the extraction efficiency of lignans were optimized, and compared with the traditional methods. The experimental results showed that the good linear relationship for analytes was obtained in the linear range (r>0.9998). The limit of detection and limit of quantification were 21.30~990.20 ng/mL and 60.80~2992.80 ng/mL, respectively. The spiked recoveries were between 75.00% and 97.78%. The analysis results were satisfactory. Compared with other methods, the extraction yield obtained by this method was significantly higher than that obtained by microwave extraction and thermal reflux extraction, and comparable to that obtained by the pharmacopoeia method. Although a small amount of organic solvent was used in the extraction process, the ratio of solid to liquid was only 1:2, which is 1/25~1/50 of other methods. This method has the advantages of large sample handling capacity, simple operation, environmental protection and high extraction efficiency, and certain potential in industrial production and application. It can be used for the extraction and separation of lignans in traditional Chinese medicine.
[中图分类号]
[基金项目]
吉林省科技厅发展计划项目(20190304011YY)