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采用超临界流体萃取结合高速逆流色谱法从辣椒中制备分离和纯化辣椒素和二氢辣椒素

Preparative isolation and purification of capsaicin and dihydrocapsaicin from Capsici Fructus using supercritical fluid extraction combined with high speed countercurrent chromatography.

作者信息

Yan Rongwei, Zhao Leilei, Tao Junfei, Zou Yong, Xu Xinjun

机构信息

School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou, China.

Zhongshan WanYuan New Drug R&D Co., Ltd., Zhongshan, China.

出版信息

J Sci Food Agric. 2018 May;98(7):2498-2506. doi: 10.1002/jsfa.8736. Epub 2017 Nov 24.

Abstract

BACKGROUND

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.

RESULTS

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.

CONCLUSIONS

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.

摘要

背景

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。

结果

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。

结论

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。

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