Zhang Yuchi, Liu Chunming, Qi Yanjuan, Li Yuchun, Li Sainan, Wang Yuqi, Ren Junqi, Tang Ying
Central Laboratory, Changchun Normal University, No. 677 North Changji Road, Erdao District, Changchun, 130032, China.
Traditional Chinese Medicine Academy of Science of Jilin Province, No. 1745 Gongnong Road, Chaoyang District, Changchun, 130021, China.
Phytochem Anal. 2015 Sep-Oct;26(5):301-9. doi: 10.1002/pca.2564. Epub 2015 Apr 22.
Sample preparation is a crucial step in medicinal herb analysis because the desired chemical components need to be extracted from the herbal materials for further separation and characterisation. Thus, the development of " modern" sample preparation techniques with significant advantages over conventional methods is very important.
The aim of this study was the development of a new preparation method using circulating ultrasonic-assisted extraction (CUAE) coupled with centrifugal partition chromatography (CPC) for continuous extraction and on-line isolation of chemical constituents from Stellera chamaejasme L.
The stationary or mobile phase was used as the extraction solvent. Extraction parameters, including the ultrasound power, extraction time, temperature, and liquid:solid ratio, were optimised using a response surface methodology.
The extraction time, temperature, and power considerably affected the extraction yield. The optimised extraction parameters were an ultrasound power of 800 W, extraction time of 30 min, extraction temperature of 70 °C, and liquid:solid ratio of 8 mL/g. The solvent system for CUAE and CPC was optimised using mathematical equations, and the two-phase solvent system of n-hexane:ethyl acetate:methanol:water at a volume ratio of 3:5:4:6 was calculated. Four target compounds (daphnoretin, chamaechromone, neochamaejasmin A, and isochamaejasmin) with purities above 96% were successfully extracted and isolated on-line via CUAE/CPC.
Compared with the reference extraction methods, the instrumental setup achieved a scientific and systematic extraction and isolation of natural products and has great potential for industrial application.
样品制备是草药分析中的关键步骤，因为需要从草药材料中提取所需的化学成分，以便进一步分离和表征。因此，开发比传统方法具有显著优势的“现代”样品制备技术非常重要。
本研究的目的是开发一种新的制备方法，该方法采用循环超声辅助萃取（CUAE）与离心分配色谱（CPC）相结合，用于狼毒中化学成分的连续萃取和在线分离。
使用固定相或流动相作为萃取溶剂。采用响应面法对超声功率、萃取时间、温度和液固比等萃取参数进行了优化。
萃取时间、温度和功率对萃取产率有显著影响。优化后的萃取参数为超声功率800W、萃取时间30分钟、萃取温度70℃和液固比8mL/g。利用数学方程对CUAE和CPC的溶剂体系进行了优化，计算出正己烷：乙酸乙酯：甲醇：水体积比为3:5:4:6的两相溶剂体系。通过CUAE/CPC成功地在线萃取和分离了四种纯度高于96%的目标化合物（瑞香素、狼毒素、新狼毒素A和异狼毒素）。
与参考萃取方法相比，该仪器装置实现了对天然产物的科学、系统的萃取和分离，具有很大的工业应用潜力。
