CN103554212A - Method for preparing licorice extracts serving as bulk drug for veterinary use - Google Patents
Method for preparing licorice extracts serving as bulk drug for veterinary use Download PDFInfo
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- CN103554212A CN103554212A CN201310534997.4A CN201310534997A CN103554212A CN 103554212 A CN103554212 A CN 103554212A CN 201310534997 A CN201310534997 A CN 201310534997A CN 103554212 A CN103554212 A CN 103554212A
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Abstract
The invention relates to a method for preparing glycyrrhetinic acid which is medicine bulk drug for veterinary use, in particular to a method for preparing a bulk drug for veterinary use by extracting effective constituents from plant drugs, and the bulk drug is used to prevent and control diseases of birds and beasts. Specifically, the invention relates to a method for extracting purified glycyrrhetinic acid from liquorice. The method for preparing the glycyrrhetinic acid serving as a bulk drug for veterinary use is feasible in actual production, ensures high purity of the glycyrrhetinic acid, can be widely applied to pollution-free breeding industry, promotes the production of pollution-free food, and ensures food safety. The method is reasonable in technology and is economical and practical, the product purity can reach more than 91%, the production operability is high, the practical application value is high, and the method can bring good economic and social benefits.
Description
Technical field
The present invention relates to a kind of bulk drug that is widely used in the brutish disease of control, be applied to non-nuisance industry, ensure food safety, is the method that extracting effective components makes veterinary drug bulk drug from plant amedica specifically, is used for preventing and treating brutish disease.Particularly from Radix Glycyrrhizae, extract the preparation method of purifying liquorice hypo acid.
Background technology
In Radix Glycyrrhizae, be the root and rhizome of glycyrrhizic legume, glycyrrhiza inflate bat or glycyrrhiza glabra, have invigorate the spleen and benefit qi, the effect such as expelling phlegm for arresting cough, clearing heat and detoxicating, relieving spasm to stop pain, the mediation property of medicine.Be the long and conventional Chinese medicine the most widely of applicating history, for fields such as medicine, tobacco, food, in addition, the powder of Radix Glycyrrhizae and extract thereof are also as once using with feed.Modern pharmacology research shows, glycyrrhetinic acid (GA) is one of effective constituent of Radix Glycyrrhizae, have anti-inflammatory, antianaphylaxis, antiviral, protect the liver, the effect such as immunomodulatory.Its molecular structure is similar to hydrocortisone, and by suppressing the activity of 11-hydroxyl sterol desaturase-2 type in animal body, the conversion of the hydrocortisone that can slow down, improves action intensity; Documents and materials show, the surrogate of glycyrrhetinic acid Chang Zuowei hydrocortisone use clinically, and glycyrrhetinic acid has the effect of adrenocortical hormone sample and many-sided pharmacologically active.But the Radix Glycyrrhizae suitability for industrialized production aspect as veterinary drug bulk drug has no report.The present invention, from the feasibility of actual production, develops preparation and the method thereof of bulk drug for livestock glycyrrhetinic acid, and its purity is high, is widely used in non-nuisance industry, promotes the production of pollution-free food, and then ensures food safety.
Summary of the invention
The object of the invention is to: a kind of method of extracting purifying liquorice hypo acid from Radix Glycyrrhizae for animals is provided, can be used as in bulk drug and use.Its technique is reasonable, economical and practical, and product purity can reach 91%, and production operation is strong, and the value of practical application is large, is expected to bring good economic and social benefit.
The present invention is achieved in that middle extraction Potenlini makes Glycyrrhizinic acid monopotassium salt, then obtains glycyrrhetinic acid by Glycyrrhizinic acid monopotassium salt hydrolysis, has obtained the higher glycyrrhetinic acid of purity, reaches the purity requirement of bulk drug.
embodiment
1, the preparation of Glycyrrhizinic acid monopotassium salt
Sweet single meal soaks 3 times with 0.5% ammoniacal liquor of 1 ~ 15 times of amount, spends the night first; Filtered liquid is concentrated into original volume 1/5, and filtrate adds the vitriol oil to pH2 ~ 3.5, standing, and precipitation is spent the night, and filters, and precipitation is washed 3 times, 60 ℃ of following dry thick Potenlinis that to obtain; Add 4 ~ l0 and doubly measure dehydrated alcohol, reflux 3 times, 3h for the first time, rear twice 2h, filters, merging filtrate, cooling, filtrate is adjusted pH7 ~ 8 with 20%KOH, and the standing precipitation of separating out, spends the night, and filters, and precipitation is washed with a little alcohol, and drying at room temperature obtains GLYCYRRHIZIC ACID POTASSIUM; With Glacial acetic acid, dissolve and separate crystallization twice again, spend the night at every turn, filter to obtain yellowish bag Potenlini list bait salt, then obtain the crystallization of faint yellow yellow Potenlini list signature salt with 75% alcohol recrystallization.
2, the preparation of glycyrrhetinic acid
Glycyrrhizinic acid monopotassium salt, adds 5 ~ l0 times of water gaging heating for dissolving, then adds 3 ~ l0 and doubly measure ethanol, drip l ~ l0 and doubly measure concentrated hydrochloric acid, stirring and refluxing reaction 6h, cold putting, the solids that filtration is separated out, water washing, solids dissolves with chloroform, filters, twice of the NaOH aqueous solution extraction of chloroform solution use lmol/L, merge water, with hydrochloric acid, be neutralized to pH2 ~ 3, then use twice of chloroform extraction water.Chloroform is washed mutually, and concentrated, excess ethyl alcohol recrystallization, obtains glycyrrhetinic acid product.Purity 91%.
Below in conjunction with specific examples, further illustrate the present invention.
Embodiment
Potenlini list is forged the extracting method that salt hydrolysis obtains glycyrrhetinic acid
1, the preparation of Glycyrrhizinic acid monopotassium salt
Radix Glycyrrhizae meal 1000g soaks 3 times with 0.5% ammoniacal liquor of 14 times of amounts, spends the night first; Filtered liquid concentrates and is written to original volume 1/5, and filtrate adds the vitriol oil to pH2 ~ 3.5, standing, and precipitation is spent the night, and filters, and precipitation is washed 3 times, and 60 ℃ of following being dried to obtain thick Potenlini 60g; Add 4 ~ 10 times of amount dehydrated alcohols, reflux 3 times, 3h for the first time, rear twice 2h, filters, and closes well filtrate, and cooling, filtrate is adjusted pH7 ~ 8 with 20%KOH, and the standing precipitation of separating out, spends the night, and filters, and precipitation is washed with a little alcohol, and drying at room temperature obtains GLYCYRRHIZIC ACID POTASSIUM 40g; With Glacial acetic acid, dissolve crystallization twice again, spend the night at every turn, filter to obtain faint yellow Glycyrrhizinic acid monopotassium salt 12g, then obtain faint yellow yellow Glycyrrhizinic acid monopotassium salt crystallization 10g with 75% alcohol recrystallization.
2, the preparation of glycyrrhetinic acid
Glycyrrhizinic acid monopotassium salt 5g, adds 50ml water heating for dissolving, then adds 15ml ethanol, oil adds 7.5ml concentrated hydrochloric acid, the reverse 6h of stirring and refluxing, cold putting, the solids that filtration is separated out, water washing, solids dissolves with chloroform, filters, twice of the NaOH aqueous solution extraction of the pseudo-liquid use of chlorine lmol/L, merge water, with hydrochloric acid, be neutralized to pH2 ~ 3.5, then use twice of chloroform extraction water.Chloroform is washed mutually, and concentrated, excess ethyl alcohol recrystallization, obtains glycyrrhetinic acid product 1.5g.Purity 91%.
Claims (1)
1. the present invention relates to a kind of preparation of licorice extract of bulk drug for livestock, it is characterized in that: Glycyrrhizinic acid monopotassium salt hydrolysis obtains the extracting method kind of glycyrrhetinic acid, (1) relate to Glycyrrhizinic acid monopotassium salt system each, 0.5% ammoniacal liquor immersion 3 times for Radix Glycyrrhizae meal, spends the night: filtered liquid is concentrated into original volume 1/5 first, filtrate adds the vitriol oil to pH2 ~ 3.5, standing, precipitation is spent the night, and filters, precipitation washing 3 times, 60 ℃ of following being dried to obtain slightly Potenlini; Add 4 ~ l0 and doubly measure dehydrated alcohol, reflux 3 times, 3h for the first time, rear twice 2h, filters, merging filtrate, cooling, filtrate is adjusted pH7 ~ 8 with 20%KOH, and the standing precipitation of separating out, spends the night, and filters, and precipitation is washed with a little alcohol, and drying at room temperature obtains GLYCYRRHIZIC ACID POTASSIUM; With the intoxicated acid of ice, dissolve crystallization twice again, spend the night at every turn, filter to obtain faint yellow Glycyrrhizinic acid monopotassium salt, then obtain faint yellow yellow Glycyrrhizinic acid monopotassium salt crystallization with 75% alcohol recrystallization; (2) preparation of glycyrrhetinic acid, Glycyrrhizinic acid monopotassium salt, adds 5 ~ 10 times of water gaging heating for dissolving, add again 3 ~ 10 times of amount ethanol, drip l ~ l0 and doubly measure concentrated hydrochloric acid, stirring and refluxing reaction 6h, cold putting, filters the solids of separating out, water washing, solids dissolves with chloroform, filter, the NaOH aqueous solution extraction twice of lmol/L for chloroform solution, merges water, with hydrochloric acid, be neutralized to pH2 ~ 3.5, then use twice of chloroform extraction water; Chloroform is washed mutually, and concentrated, excess ethyl alcohol recrystallization, obtains glycyrrhetinic acid product; Purity 91%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310534997.4A CN103554212A (en) | 2013-11-04 | 2013-11-04 | Method for preparing licorice extracts serving as bulk drug for veterinary use |
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| CN201310534997.4A CN103554212A (en) | 2013-11-04 | 2013-11-04 | Method for preparing licorice extracts serving as bulk drug for veterinary use |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829681A (en) * | 2015-05-08 | 2015-08-12 | 江苏天晟药业有限公司 | Method for purifying glycyrrhetinic acid |
| CN106336446A (en) * | 2016-08-24 | 2017-01-18 | 江苏天晟药业股份有限公司 | Preparation method of potassium glycyrrhizate |
-
2013
- 2013-11-04 CN CN201310534997.4A patent/CN103554212A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829681A (en) * | 2015-05-08 | 2015-08-12 | 江苏天晟药业有限公司 | Method for purifying glycyrrhetinic acid |
| CN106336446A (en) * | 2016-08-24 | 2017-01-18 | 江苏天晟药业股份有限公司 | Preparation method of potassium glycyrrhizate |
| CN106336446B (en) * | 2016-08-24 | 2018-07-03 | 江苏天晟药业股份有限公司 | A kind of preparation method of potassium glycyrrhizana |
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Application publication date: 20140205 |