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A kind of industrial production method of diosgenin secondary glycoside

A technology of diosgenin and a production method is applied in the fields of medicinal chemical engineering and natural products, and can solve the problems of difficulty in separation, consumption, and high cost of column chromatography separation

Active Publication Date: 2017-03-22
十堰赟天生物科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, this process produces a large amount of acidic wastewater, and on the other hand, the target product diosgenin secondary glycosides is mixed with residual diosgenin and sugar esters and other by-products, which is difficult to separate, and column chromatography separation is expensive and consumes a large amount of solvent. polluted environment

Method used

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  • A kind of industrial production method of diosgenin secondary glycoside

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] like figure 1 As shown, a device used in the industrial production reaction system of diosgenin secondary glycosides, including an acid-resistant reaction tank 1, a stirring motor 2, a stirring rod 3, a stirring screw 4, an acid aqueous phase suspension 5, and a n-butanol phase 6 , Suction tube / filling tube 7, feed port cover 8, discharge port cover 9 and heating layer 10.

[0026] The inner wall of the acid-resistant reaction tank, the stirring rod 3 and the stirring spiral piece 4 are all ceramic coating or tetrafluoroethylene coating.

[0027] The inner layer of the discharge port cover and the inner and outer layers of the suction pipe are both ceramic coating or tetrafluoroethylene coating.

[0028] The acid water suspension phase 5 may be sulfuric acid water, hydrochloric acid water, nitric acid water, sulfurous acid water, nitrous acid water, etc.

Embodiment 2

[0030] A kind of industrialized production method of diosgenin secondary glycoside is as follows:

[0031] (1) 15 tons of fresh yam rhizomes are smashed, soaked with 70-95v / v% ethanol, then filtered to obtain an ethanol extract, and dried and crushed to obtain 1 ton of ethanol extract, then extracted with water-saturated n-butanol Ethanol extract powder, concentrate n-butanol extract to obtain n-butanol extract, i.e. dioscin extract, or extract ethanol extract powder with water-saturated ethyl acetate, and then concentrate to obtain ethyl acetate extract, i.e. dioscin extract liquid;

[0032](2) Preparation of acidic water phase: 98wt% vitriol oil or 37wt% concentrated hydrochloric acid are added to pure water or common tap water to obtain acidic water phase; the volume ratio of 98wt% vitriol oil or 37wt% concentrated hydrochloric acid to pure water or common tap water is 0.2:10, prepare 5-8 tons of acidic aqueous phase;

[0033] (3) Add the acidic aqueous phase prepared in ...

Embodiment 3

[0039] A kind of industrialized production method of diosgenin secondary glycoside is as follows:

[0040] (1) 28 tons of fresh yam rhizomes are added with water-saturated n-butanol to make a pulp, and the pulp residue is added in a sufficient amount of water in the sedimentation tank to make n-butanol layered, and then the n-butanol in the upper layer is extracted to obtain n-butanol of dioscin Alcohol extract, the main component of which is diosgenin;

[0041] (2) Preparation of acidic water phase: 98wt% vitriol oil or 37wt% concentrated hydrochloric acid are added to pure water or common tap water to obtain acidic water phase; the volume ratio of 98wt% vitriol oil or 37wt% concentrated hydrochloric acid to pure water or common tap water is 0.1:10, prepare 5-8 tons of acidic aqueous phase;

[0042] (3) Add the acid water phase prepared in step (2) into a reaction tank with a capacity of 20 tons, and add the n-butanol extract of dioscin prepared in step 1) in the reaction ta...

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Abstract

The invention discloses an industrial production method of secondary glycoside of dioscin. The industrial production method comprises the following steps: (1) preparing raw materials of secondary glycoside of dioscin; (2) preparing an acidic water phase; (3) adding the acidic water phase into a reaction tank, and adding the raw materials of the secondary glycoside of dioscin to form a two-phase reaction system with the acidic water phase; (4) heating and stirring the materials; (5) after the reaction system in the reaction tank is divided into a black n-butyl alcohol phase on the upper layer, a bronzing acidic water phase on the middle layer and a white precipitate phase on the bottom layer from top to bottom, abandoning the black n-butyl alcohol phase on the upper layer and the bronzing acidic water phase on the middle layer, and collecting the white precipitate phase on the bottom layer; (6) stirring and washing the white precipitate phase on the bottom layer respectively with pure water and water saturated n-butyl alcohol, and drying after stewing filtration to obtain the secondary glycoside of the dioscin; or stirring and washing the white precipitate phase on the bottom layer with the pure water and n-butyl alcohol, filtering and drying to obtain the secondary glycoside of the dioscin. The industrial production method has the advantages that high-purity secondary glycoside of the dioscin can be quickly obtained, and no wastewater is discharged.

Description

technical field [0001] The invention belongs to the fields of medicinal chemical engineering and natural products, and relates to an industrial production method of dioscin secondary glycosides, in particular to a dioscin secondary glycoside suitable for large-scale production of highly active dioscin secondary glycosides without any sewage discharge The industrial production method of the secondary glycoside of primary glycoside. Background technique [0002] Dioscin is an important medicinal raw material. The secondary glycoside of dioscin is glucoside without rhamnose. Due to its stronger polarity and special structure, it has stronger physiological activity than dioscin, and has more advantages in the fields of cardiovascular and cerebrovascular and other steroid hormones. important medical value. Dioscin is present in the rhizomes of plants of the genus Dioscorea. Dioscorea scutellaria is mainly cultivated in my country, and the rhizomes of diosgenus scutellaria are ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J71/00
CPCC07J71/0005
Inventor 董静洲艾训儒姚兰
Owner 十堰赟天生物科技发展有限公司
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