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

Author:
Yan, Rongwei, Zhao, Leilei, Tao, Junfei, Zou, Yong, Xu, Xinjun
Source:
Journal of the science of food and agriculture 2018 v.98 no.7 pp. 2498-2506
ISSN:
0022-5142
Subject:
Capsicum, acid deposition, alkali treatment, capsaicin, carbon dioxide, countercurrent chromatography, crystallization, methanol, response surface methodology, solvents, supercritical fluid extraction, temperature
Abstract:
BACKGROUND: Supercritical fluid extraction with CO₂ (SFE‐CO₂) 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‐CO₂ 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‐CO₂ 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‐CO₂, 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
Agid:
5927889