Method for preparing albiflorin and paeoniflorin

Abstract

The invention relates to a method for preparing albiflorin and / or paeoniflorin. The method is characterized by comprising the following steps of: refining alumina with white peony total glucoside extract, wherein the white peony total glucoside extract is dissolved with water, and alumina is refined; refining the alumina refined solution with activated carbon; and refining the activated carbon refined substance with silica gel, wherein eluent which is 8 to 20 times that of activated carbon refined substance is added into the activated carbon refined substance for dissolving, passes through a silica gel column, and is eluted with eluent; fractions are collected and inspected by thin layers to collect fraction containing paeoniflorin, fraction containing paeoniflorin and albiflorin and fraction containing albiflorin respectively; all solvents are reclaimed; the extract is dissolved with appropriate water and filtered; and the filtrates are dried to respectively obtain the paeoniflorin, mixture of paeoniflorin and albiflorin, as well as the albiflorin. The mixture of paeoniflorin and albiflorin is refined repeatedly according to the performed method to obtain the paeoniflorin and the albiflorin. According to the product prepared by the method, the content of paeoniflorin is more than or equal to 95 percent, and the content of the paeoniflorin is more than or equal to 92 percent, which are in accordance with the standard of raw material drugs of the first type of new drug.

Description

technical field [0001] The invention relates to a preparation method of paeonifloride glycoside and paeoniflorin, belonging to the field of traditional Chinese medicine. technical background [0002] CN 101607975A discloses a preparation method of paeonifloride, which adopts: "Method for separating and preparing paeonifloride by simulated moving bed chromatography" uses total glucosides of paeony as raw material, and uses simulated moving bed chromatography to separate and prepare paeonifloride Esteroside, the stationary phase of simulated moving bed chromatography adopts C 18 Silica gel, the mobile phase is a mixed solution of methanol or acetonitrile, water, formic acid, and isopropanol. There are following problems in this patent: 1) used filler C 18 The price of silica gel is about 1,000 yuan / kg, which is high cost; 2) Its simulated moving bed chromatography is high-pressure chromatography, which requires special equipment such as high-pressure columns and high-pressur...

AI Technical Summary

Problems solved by technology

There are following problems in this patent: 1) used filler C 18 The price of silica gel is about 1,000 yuan / kg, which is high cost; 2) Its simulated moving bed chromatography is high-pressure chromatography, which requires special equipment such as high-pressure columns and high-pressure infusion pumps, and requires high production conditions; 3) In terms of solvents, the patent is anti- phase packing, eluting with water containing organic solvent

This method has the following difficulties in industrial production: ① The total glucosides of paeony extract contains many impurities. After the paeoniflorin and paeoniflorin are eluted, the impurities are adsorbed on the silica gel and are difficult to remove. The silica gel column cannot be reused and needs to be removed. Repack the column, because the column contains flammable and toxic chemical reagents, which is difficult and dangerous to operate; ②The total glucosides of paeony extract is added to silica gel and dried and packed into the column, which has strong adsorption capacity. Although the prepared product has high purity, the elution The process is slow (elution process takes 1 to 2 days), consumes a large amount of solvent, and 1 / 3 of paeonifloride and paeoniflorin are adsorbed on silica gel, which is difficult to elute, and the product yield is low

③The silica gel column is eluted with mobile phases of different polarities, and the recovered solvent is difficult to reuse; ④Because the silica gel column needs to be disassembled and assembled repeatedly, the recovered solvent needs to be mixed in proportion, so it is difficult to avoid open production, and the volatilization of organic solvents can lead to flammable, flammable Explosion, poisoning, pollution and other hazards

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