Study On The High Efficiency Preparation Of Chlorogenic Acid In Flos Lonicerae Japonicae

Chlorogenic acid is an main active constituent in Flos Lonicerae japonicae, and it has various biological activities. Methods of separating and purifying chlorogenic acid are based on column chromatography, which is comparatively complex and time-consumer. To find a simple and effective method for preparation of chlorogenic acid promoted us. A simple separation of chlorogenic acid was established on the base of selective extraction in our recently works.Extraction residue which from Flos Lonicerae japonicae with water-ethanol system was dispersed in water, and then extracted with a solvent (ethyl acetate:n-butyl alcohol=3:2, v/v) repeatedly. The light phase, the organic solution, then was extracted with polyacrylamide aqueous solution repeatedly. The crude chlorogenic acid was offered from the organic solution. The crude chlorogenic acid was crystallized in ethyl acetate-methanol (3:2, v/v) to give chlorogenic acid (98.43%), and he recovery of pure chlorogenic acid was27.42%.To improve the yield of chlorogenic acid, the method that solvent extraction combined adsorption of activated carbon for the separation and purification of chlorogenic acid was researched. Chlorogenic acid was enriched from the extractum of Flos Lonicerae japonicae with mixed solvent at ethanol-ethyl acetate (9:91, v/v), and then mixture solvent was applied on a short activated carbon column to remove pigment. The crude chlorogenic acid was obtained by concentration under vacuum from the organic solution. A high-purity (98.63%pure) chlorogenic acid was obtained from crude chlorogenic by recrystallization with solvent, acetate:methanol=3:2(v/v), and he recovery of pure chlorogenic acid was36.63%, the yield of product was improved.The extractum of Flos Lonicerae japonicae with water-ethanol was selectively by the mixed solvent:ethyl acetate:petroleum ether (1:1, v/v), then the extraction was washed with the sodium carbonate solution repeatedly. Compound I was isolated from organic phase directly. Compound II was obtained from aqueous phase by extraction after acidifying. Their structures were elucidated by means of physico-chemical properties, MS, IR and NMR evidences as3’,4’,5’,5,7-pentamethoxy flavone (Ⅰ), luteolin (Ⅱ)The method for separating and purifying chlorogenic acid3’,4’,5’,5,7-pentamethoxy flavone and luteolin has more advantages compared with the traditional column chromatograph, such as low cost, short production cycle, simple preparation, high-yield product.