CN101519422A - Method for preparing mono-ammonium glycyrrhizinate - Google Patents
Method for preparing mono-ammonium glycyrrhizinate Download PDFInfo
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- CN101519422A CN101519422A CN200810072825A CN200810072825A CN101519422A CN 101519422 A CN101519422 A CN 101519422A CN 200810072825 A CN200810072825 A CN 200810072825A CN 200810072825 A CN200810072825 A CN 200810072825A CN 101519422 A CN101519422 A CN 101519422A
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Abstract
The invention discloses a method for preparing mono-ammonium glycyrrhizinate, consisting essentially of the following processing steps of: dissolving glycyrrhizic acid powder into organic solvent solution for refluxing extraction; adding ammonia or ammonia water; and obtaining the mono-ammonium glycyrrhizinate after filtering and drying. The preparation method takes the glycyrrhizic acid powder as raw material to directly prepare mono-ammonium glycyrrhizinate, the operation is simple and convenient, the time is saved, the cost is reduced, and the product content is high, thus avoiding the drawbacks in the existing preparation process of the mono-ammonium glycyrrhizinate such as long steps, high cost, use of a large amount of organic solvent, not being beneficial to environmental protection, low product content, and the like.
Description
Technical field
The present invention relates to the preparation method of monoammonium glycyrrhizinate.
Technical background
Monoammonium glycyrrhizinate is the third generation substituent of Chinese medicine effective liquorice; and stronger anti-inflammatory is arranged, protect liver plasma membrane and improve the effect of liver function; the synthetic method of monoammonium glycyrrhizinate generally is to prepare the Potenlini powder from Radix Glycyrrhizae earlier at present, and earlier by synthetic Triammonium glycyrrhizinate, adds acetic acid then and prepare monoammonium glycyrrhizinate; process is many; complex process, the production cost height, and need to use a large amount of solvents; solvent for use is unfavorable for environmental protection, and the product content that obtains is lower.
Summary of the invention:
In order to overcome the deficiency of prior art, it is a kind of easy and simple to handle that the object of the invention is to provide, and saves time, reduce cost, and the higher method for preparing monoammonium glycyrrhizinate of product content.
Characteristics of the present invention are mainly to be made of following processing step:
The Potenlini powder is dissolved in alcohols more than 85% of 5～15 times of weight, concentration, the organic solvent of ketone refluxes 1～4 time, each 1～5 hour extracting solution; The gained extracting solution is added ammonia or ammoniacal liquor, to pH value between 5～6 and stir 30min～1h, leave standstill 8～24h then; Cross 10～300um filter cloth or sieve, be dried to moisture below 8%, promptly get monoammonium glycyrrhizinate.
Above-mentioned organic solvent can be the mixed solvent of ethanol, methyl alcohol, enol, acetone or alcohol and acetone, also can be other alcohols.
As further improvement, the most handy 4 times～6 times of above-mentioned filtration gained throw out, the alcoholic solvent recrystallization of concentration more than 70% 1～5 time, described alcoholic solvent can be pressed arbitrary proportion in ethanol, methyl alcohol, the enol one or more and mix.
Preparation method of the present invention is that raw material directly prepares monoammonium glycyrrhizinate with the Potenlini powder, easy and simple to handle, promptly save time, reduced cost again, and product content height, thereby avoid drawbacks such as step is long in the existing monoammonium glycyrrhizinate preparation process, cost is high, use a large amount of organic solvents, be unfavorable for environmental protection, product content is low.
Embodiment:
Embodiment 1: extracting liquorice acid powder 1Kg, add 50 ℃ of refluxing extraction 2h of 6Kg 95% ethanol for the first time, and filtration adds 95% ethanol 8Kg again, refluxing extraction 2h filters, and adds 6Kg 95% ethanol again, refluxing extraction 2h merges above-mentioned filtrate, feeds ammonia, to pH value be between 5～6, stir 1h, leave standstill 24h, suction filtration, get the monoammonium glycyrrhizinate crude product, monoammonium glycyrrhizinate is added 5Kg85% ethanol heating for dissolving, treat that solution is limpid after, add the 25g gac, refluxing extraction 1h, pour out, leave standstill 12h, suction filtration, vacuum-drying promptly gets the monoammonium glycyrrhizinate finished product to moisture 8%.
Embodiment 2: extracting liquorice acid powder 1Kg, add 50 ℃ of refluxing extraction 2h of 8Kg methyl alcohol for the first time, and filtration adds methyl alcohol 5Kg again, refluxing extraction 2h filters, and adds 5Kg methyl alcohol again, refluxing extraction 2h, merging filtrate feeds ammonia, to pH value be between 5～6, stir 1h, leave standstill 24h, suction filtration gets the monoammonium glycyrrhizinate crude product, monoammonium glycyrrhizinate is added the 6Kg85% dissolve with ethanol, after treating that solution is limpid, add the 30g gac, refluxing extraction 1h, leave standstill 12h, suction filtration, vacuum-drying get the monoammonium glycyrrhizinate finished product to moisture 6%.
Embodiment 3: Potenlini powder 1Kg is dissolved in the mixed solvent of the ethanol of 5Kg concentration 90% of weight and acetone and refluxes 4 times, each 1 hour extracting solution, ethanol and acetone be mixed into 1:1, mistake 180um filter cloth, merging filtrate, the gained extracting solution is added ammonia, to pH value between 5～6 and stir 30min, leave standstill 1h then, cross the 149um filter cloth, the ethyl alcohol recrystallization of gained throw out 4Kg, concentration 75% 3 times is dried to moisture below 8%, promptly gets monoammonium glycyrrhizinate.
Embodiment 4: Potenlini powder 1Kg is dissolved in the acetone solvent of 15Kg concentration 95% of weight and refluxes 2 times, got extracting solution in each 2 hours, cross the 100um filter cloth, merging filtrate adds ammonia with the gained extracting solution, to pH value between 5～6 and stir 30min, leave standstill 40min then, cross the 100um filter cloth, the ethyl alcohol recrystallization of gained throw out 5Kg, concentration 80% 2 times, be dried to moisture below 8%, promptly get monoammonium glycyrrhizinate.
Embodiment 5: Potenlini powder 1Kg is dissolved in the enol solvent of 10Kg concentration 80% of weight and refluxes 3 times, got extracting solution in each 1.5 hours, cross the 250um filter cloth, merging filtrate adds ammoniacal liquor with the gained extracting solution, to pH value between 5～6 and stir 40min, leave standstill 40min then, cross the 250um filter cloth, the enol recrystallization of gained throw out 6Kg, concentration 75% 2 times, be dried to moisture below 8%, promptly get monoammonium glycyrrhizinate.
Embodiment 6: Potenlini powder 1Kg is dissolved in the enol solvent of 8Kg concentration 85% of weight and refluxes 3 times, got extracting solution in each 5 hours, cross the 100um filter cloth, merging filtrate adds ammoniacal liquor with the gained extracting solution, to pH value between 5～6 and stir 50min, leave standstill 50min then, cross the 150um filter cloth, the enol recrystallization of gained throw out 5.5Kg, concentration 95% 4 times, be dried to moisture below 8%, promptly get monoammonium glycyrrhizinate.
Embodiment 7: Potenlini powder 1Kg is dissolved in the methanol solvate of 12Kg concentration 98% of weight and refluxes 3 times, got extracting solution in each 3 hours, cross the 250um filter cloth, merging filtrate adds ammoniacal liquor with the gained extracting solution, to pH value between 5～6 and stir 50min, leave standstill 50min then, cross the 150um filter cloth, the recrystallizing methanol of gained throw out 4.5Kg, concentration 85% 4 times, be dried to moisture 5%, promptly get monoammonium glycyrrhizinate.
Embodiment 8: Potenlini powder 1Kg is dissolved in the alcohol solvent of 7Kg concentration 90% of weight and refluxes 4 times, got extracting solution in each 1.5 hours, cross the 200um filter cloth, merging filtrate adds ammoniacal liquor with the gained extracting solution, to pH value between 5～6 and stir 30min, leave standstill 40min then, cross the 80um filter cloth, the recrystallizing methanol of gained throw out 4.5Kg, concentration 80% 3 times, be dried to moisture 6%, promptly get monoammonium glycyrrhizinate.
Embodiment 9: Potenlini powder 1Kg is dissolved in the propyl alcohol solvent of 10Kg concentration 85% of weight and refluxes 4 times, got extracting solution in each 1.5 hours, cross the 200um filter cloth, merging filtrate adds ammoniacal liquor with the gained extracting solution, to pH value between 5～6 and stir 30min, leave standstill 40min then, cross the 80um filter cloth, the ethyl alcohol recrystallization of gained throw out 4.5Kg, concentration 98% 3 times, be dried to moisture 6%, promptly get monoammonium glycyrrhizinate.
Embodiment 10: Potenlini powder 1Kg is dissolved in the propyl alcohol solvent of 7Kg concentration 94% of weight and refluxes 3 times, got extracting solution in each 2 hours, cross the 120um filter cloth, merging filtrate adds ammoniacal liquor with the gained extracting solution, to pH value between 5～6 and stir 55min, leave standstill 50min then, cross the 58um filter cloth, the ethyl alcohol recrystallization of gained throw out 5Kg, concentration 95% 4 times, be dried to moisture 6%, promptly get monoammonium glycyrrhizinate.
Embodiment 11: Potenlini powder 1Kg is dissolved in the propyl alcohol solvent of 5Kg concentration 94% of weight and refluxes 3 times, got extracting solution in each 3 hours, cross the 120um filter cloth, merging filtrate adds ammoniacal liquor with the gained extracting solution, to pH value between 5～6 and stir 35min, leave standstill 35min then, cross the 48um filter cloth, the enol recrystallization of gained throw out 4.5Kg, concentration 90% 2 times, be dried to moisture 6%, promptly get monoammonium glycyrrhizinate.
Embodiment 12: Potenlini powder 1Kg is dissolved in the enol solvent of 5Kg concentration 94% of weight and refluxes 4 times, got extracting solution in each 1.5 hours, cross the 250um filter cloth, merging filtrate adds ammoniacal liquor with the gained extracting solution, to pH value between 5～6 and stir 40min, leave standstill 40min then, cross the 106um filter cloth, the ethyl alcohol recrystallization of gained throw out 5Kg, concentration 96% 3 times, be dried to moisture 8%, promptly get monoammonium glycyrrhizinate.
Embodiment 13: Potenlini powder 1Kg is dissolved in the enol solvent of 7Kg concentration 95% of weight and refluxes 3 times, got extracting solution in each 3.5 hours, cross the 180um filter cloth, merging filtrate adds ammonia with the gained extracting solution, to pH value between 5～6 and stir 30min, leave standstill 40min then, cross the 120um filter cloth, the propyl alcohol recrystallization of gained throw out 5Kg, concentration 95% 3 times, be dried to moisture 7%, promptly get monoammonium glycyrrhizinate.
Embodiment 14: Potenlini powder 1Kg is dissolved in the methanol solvate of 6Kg concentration 90% of weight and refluxes 3 times, got extracting solution in each 3 hours, cross the 150um filter cloth, merging filtrate adds ammoniacal liquor with the gained extracting solution, to pH value between 5～6 and stir 40min, leave standstill 30min then, cross the 36um filter cloth, the ethyl alcohol recrystallization of gained throw out 5Kg, concentration 90% 3 times, be dried to moisture 7%, promptly get monoammonium glycyrrhizinate.
Embodiment 15: Potenlini powder 1Kg is dissolved in the methanol solvate of 10Kg concentration 92% of weight and refluxes 3 times, got extracting solution in each 2 hours, cross the 100um filter cloth, merging filtrate adds ammoniacal liquor with the gained extracting solution, to pH value between 5～6 and stir 40min, leave standstill 50min then, cross the 25um filter cloth, the recrystallizing methanol of gained throw out 5Kg, concentration 95% 3 times, be dried to moisture 7%, promptly get monoammonium glycyrrhizinate.
Claims (4)
1, a kind of preparation method of monoammonium glycyrrhizinate is characterized in that mainly being made of following processing step:
The Potenlini powder is dissolved in alcohols more than 85% of 5～15 times of weight, concentration, the organic solvent of ketone refluxes 1～4 time, got extracting solution in each 1～5 hour, the gained extracting solution is added ammonia or ammoniacal liquor, to pH value between 5～6 and stir 30min～1h, leave standstill 8～24h then, cross 10～300um filter cloth or sieve, be dried to moisture below 8%, promptly get monoammonium glycyrrhizinate.
2, the preparation method of monoammonium glycyrrhizinate according to claim 1 is characterized in that described organic solvent is the mixed solvent of ethanol, methyl alcohol, enol, acetone or alcohol and acetone.
3, the preparation method of monoammonium glycyrrhizinate according to claim 1 and 2 is characterized in that described filtration gained throw out is with 4 times～6 times, the alcoholic solvent recrystallization of concentration more than 70% 1～5 time.
4, the preparation method of monoammonium glycyrrhizinate according to claim 3 is characterized in that described alcoholic solvent is that in ethanol, methyl alcohol, the enol one or more mix by arbitrary proportion.
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| CN200810072825A CN101519422A (en) | 2008-02-27 | 2008-02-27 | Method for preparing mono-ammonium glycyrrhizinate |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286058A (en) * | 2011-09-07 | 2011-12-21 | 西安瑞联近代电子材料有限责任公司 | Method for preparing glycyrrhizic acid with high purity |
| CN103193856A (en) * | 2013-04-10 | 2013-07-10 | 宁夏紫荆花制药有限公司 | Method for preparing mono-ammonium glycyrrhizinate |
| CN104592340A (en) * | 2014-08-15 | 2015-05-06 | 宝鸡金森制药有限公司 | Glycyrrhizinic acid monoammonium salt fine product preparation method |
| 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 |
| CN106478761A (en) * | 2016-08-30 | 2017-03-08 | 青海省青海湖药业有限公司 | A kind of preparation method of mono-ammonium glycyrrhizinate |
| CN106565815A (en) * | 2016-10-28 | 2017-04-19 | 新疆昆仑神农股份有限公司 | Monoammonium glycyrrhizinate purification method |
| CN107308177A (en) * | 2017-07-19 | 2017-11-03 | 辽宁华润本溪三药有限公司 | A kind of pharmaceutical composition of antalgic and inflammation relieving and preparation method thereof and purposes |
| CN114437167A (en) * | 2021-12-31 | 2022-05-06 | 江苏天晟药业股份有限公司 | Method for preparing licorzinc by using glycyrrhizic acid powder |
-
2008
- 2008-02-27 CN CN200810072825A patent/CN101519422A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286058A (en) * | 2011-09-07 | 2011-12-21 | 西安瑞联近代电子材料有限责任公司 | Method for preparing glycyrrhizic acid with high purity |
| CN103193856A (en) * | 2013-04-10 | 2013-07-10 | 宁夏紫荆花制药有限公司 | Method for preparing mono-ammonium glycyrrhizinate |
| CN104592340A (en) * | 2014-08-15 | 2015-05-06 | 宝鸡金森制药有限公司 | Glycyrrhizinic acid monoammonium salt fine product preparation method |
| 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 |
| CN106478761A (en) * | 2016-08-30 | 2017-03-08 | 青海省青海湖药业有限公司 | A kind of preparation method of mono-ammonium glycyrrhizinate |
| CN106565815A (en) * | 2016-10-28 | 2017-04-19 | 新疆昆仑神农股份有限公司 | Monoammonium glycyrrhizinate purification method |
| CN107308177A (en) * | 2017-07-19 | 2017-11-03 | 辽宁华润本溪三药有限公司 | A kind of pharmaceutical composition of antalgic and inflammation relieving and preparation method thereof and purposes |
| CN107308177B (en) * | 2017-07-19 | 2022-05-17 | 辽宁华润本溪三药有限公司 | Analgesic and anti-inflammatory pharmaceutical composition and preparation method and application thereof |
| CN114437167A (en) * | 2021-12-31 | 2022-05-06 | 江苏天晟药业股份有限公司 | Method for preparing licorzinc by using glycyrrhizic acid powder |
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Application publication date: 20090902 |