Yan Rongwei, Zhao Leilei, Tao Junfei, Zou Yong, Xu Xinjun
School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou, China.
Zhongshan WanYuan New Drug R&D Co., Ltd., Zhongshan, China.
J Sci Food Agric. 2018 May;98(7):2498-2506. doi: 10.1002/jsfa.8736. Epub 2017 Nov 24.
Supercritical fluid extraction with CO (SFE-CO ) was utilized for extraction of capsaicin (CA) and dihydrocapsaicin (DHCA) from Capsici Fructus, and then a two-step enrichment method for separating capsaicinoids from SFE-CO extracts was developed. The process involved extraction with aqueous methanol and crystallization by alkali extraction and acid precipitation. Finally, a consecutive high-speed countercurrent chromatography (HSCCC) separation method was successfully applied in the purification of CA and DHCA from capsaicinoid crystal.
The extraction pressure, extraction temperature and volume of co-solvent were optimized at 33 MPa, 41 °C and 75 mL, respectively, using response surface methodology; the extraction rates of CA and DHCA were about 93.18% and 93.49%, respectively. 407.43 mg capsaicinoid crystal was isolated from the SFE-CO extracts obtained from 100 g capsicum powder by the two-step enrichment method. About 506 mg and 184 mg CA and DHCA with purities up to 98.31% and 96.68%, respectively, were obtained from 1 g capsaicinoid crystal in one HSCCC of three consecutive sample loadings without exchanging any solvent system.
This method comprising SFE-CO , a two-step enrichment and HSCCC was efficient, powerful and practical for the large-scale preparation of CA and DHCA from Capsici Fructus with high purity and high yield. © 2017 Society of Chemical Industry.
采用超临界CO₂流体萃取法(SFE-CO₂)从辣椒果实中提取辣椒素(CA)和二氢辣椒素(DHCA),并开发了一种从SFE-CO₂萃取物中分离辣椒素类化合物的两步富集方法。该过程包括用甲醇水溶液萃取以及通过碱萃取和酸沉淀进行结晶。最后,连续高速逆流色谱(HSCCC)分离方法成功应用于从辣椒素类化合物晶体中纯化CA和DHCA。
采用响应面法将萃取压力、萃取温度和共溶剂体积分别优化为33 MPa、41℃和75 mL;CA和DHCA的萃取率分别约为93.18%和93.49%。通过两步富集法从100 g辣椒粉末得到的SFE-CO₂萃取物中分离出407.43 mg辣椒素类化合物晶体。在不更换任何溶剂系统的情况下,通过连续三次进样的一次HSCCC操作,从1 g辣椒素类化合物晶体中分别获得了约分别为506 mg和184 mg、纯度高达98.31%和96.68%的CA和DHCA。
该方法包括SFE-CO₂、两步富集和HSCCC,对于从辣椒果实中大规模制备高纯度、高产量的CA和DHCA高效、强大且实用。© 2017化学工业协会。