Semi-industrial isolation of salicin and amygdalin from plant extracts using slow rotary counter-current chromatography.
Salicin in the bark extract of Salix alba and amygdalin in the fruit extract of Semen armeniacae were each separated by slow rotary counter-current chromatography (SRCCC). The apparatus was equipped with a 40-L column made of 17 mm i.d. convoluted Teflon tubing. A 500g amount of crude extract containing salicin at 13.5% was separated yielding 63.5 g of salicin at 95.3% purity in 20h using methyl tert-butyl ether-l-butanol (1:3) saturated by methanol-water (1:5) as a stationary phase and methanol-water (1:5) saturated by methyl tert-butyl ether-1-butanol (1:3) as a mobile phase. A 400g amount of crude extract containing amygdalin at 55.3% was isolated to yield 221.2g of amygdalin at 94.1% purity in 19h using ethyl acetate-1-butanol (1:2) saturated by water as a stationary phase and water saturated by ethyl acetate-1-butanol (1:2) as a mobile phase. The flow rate of the mobile phase was 50 ml/min. The results show that industrial SRCCC separation of salicin and amygdalin is feasible using a larger column at a higher flow rate of the mobile phase.
Du
Qizhen
Q
Institute of Food and Biological Engineering, Hangzhou University of Commerce, 149 Jiaogong Road, Hangzhou, Zhejiang 310035, China. qizhendu@mail.zjgsu.edu.cn
Jerz
Gerold
G
Ha
Yangchun
Y
Li
Lei
L
Xu
Yuanjin
Y
Zhang
Qi
Q
Zheng
Qunxiong
Q
Winterhalter
Peterb
P
Ito
Yoichiro
Y
D000678:Amygdalin / Q000302:isolation & purification*; D001592:Benzyl Alcohols / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid; D003377:Countercurrent Distribution / Q000379:methods; D004345:Drug Industry / Q000379:methods; D005960:Glucosides; D010936:Plant Extracts / Q000737:chemistry*
D001592:Benzyl Alcohols; D005960:Glucosides; D010936:Plant Extracts; D000678:Amygdalin; C005696:salicin