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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

Yan, Rongwei, Zhao, Leilei, Tao, Junfei, Zou, Yong, Xu, Xinjun
Journal of the science of food and agriculture 2018 v.98 no.7 pp. 2498-2506
Capsicum, acid deposition, alkali treatment, capsaicin, carbon dioxide, countercurrent chromatography, crystallization, methanol, response surface methodology, solvents, supercritical fluid extraction, temperature
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