CN103193856A - Method for preparing mono-ammonium glycyrrhizinate - Google Patents
Method for preparing mono-ammonium glycyrrhizinate Download PDFInfo
- Publication number
- CN103193856A CN103193856A CN2013101211823A CN201310121182A CN103193856A CN 103193856 A CN103193856 A CN 103193856A CN 2013101211823 A CN2013101211823 A CN 2013101211823A CN 201310121182 A CN201310121182 A CN 201310121182A CN 103193856 A CN103193856 A CN 103193856A
- Authority
- CN
- China
- Prior art keywords
- monoammonium glycyrrhizinate
- certain
- preparation
- glycyrrhizinate
- alcohols material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a method for preparing mono-ammonium glycyrrhizinate. The method comprises the following steps of: extracting the raw material glycyrrhizic acid by using an acidic alcohol material, adding ammonia water to adjust the PH, adding glacial acetic acid to form thin paste, standing, centrifuging to obtain a crude product of mono-ammonium glycyrrhizinate, and adding ethanol and active carbon for recrystallization, thereby obtaining the quality goods of mono-ammonium glycyrrhizinate. The technical method is simple, low in cost, good in product properties and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of monoammonium glycyrrhizinate.
Background technology
Monoammonium glycyrrhizinate (Glycyrrhizic acid ammonium salt) belongs to the Triterpenes triterpenes, and molecular formula is C
42H
61O
16NH
4, molecular weight is 839.97, for white or faint yellow crystal type powder, special sweet taste is arranged.Find that after deliberation monoammonium glycyrrhizinate has anti-liver poisoning, hormonelike activity, prevents liver cirrhosis etc.Monoammonium glycyrrhizinate not only has significant curative effect to respiratory system diseases such as trachitis, bronchitis, cough, asthma, and digestive tract infection, hepatitis B, stomatocace, stomach ulcer etc. are also had good therapeutic action.For multiple toxin such as diphtheria toxin, tetanus toxin and snake venom etc. stronger detoxicating functions is arranged, also have the effect of similar adrenocortical hormone simultaneously.Chinese medicine has the many target spots of body, many organs, and multisystem produces the advantage of comprehensive action.The effect of research monoammonium glycyrrhizinate salt pair toad isolated heart is observed the convergent force of finding monoammonium glycyrrhizinate salt pair isolated heart and is weakened, and cardiac output reduces, and heart rate slightly slows down.Ammonium glycyrrhizinate has been widely used in medicine, healthcare products, food service industry.
Summary of the invention
The objective of the invention is for a kind of preparation method of monoammonium glycyrrhizinate is provided.
A kind of preparation method of monoammonium glycyrrhizinate, concrete steps are as follows:
(1) the Potenlini acid alcohols material that adds its 5 times amounts, 3 times of amounts extracts 2 times at a certain temperature and is respectively 4h, 3h, filters united extraction liquid;
(2) add ammoniacal liquor and transfer certain PH, centrifugal after the sedimentation, wet product add organic solvent furnishing scattered paste shape, the static centrifugal monoammonium glycyrrhizinate crude product that gets;
(3) the monoammonium glycyrrhizinate crude product adds certain density alcohols material, gac and stirs, reflux decolour at a certain temperature, sedimentation filter the wet product of monoammonium glycyrrhizinate;
(4) 50～60 ℃ of down oven dry, pulverize, sieve the monoammonium glycyrrhizinate elaboration.
Described acid alcohols material is acidic ethanol, and PH is 3.5～4.0; Certain temperature is 40～50 ℃.
Described certain PH is 7.2～7.5; Organic solvent is glacial acetic acid.
Described certain density alcohols material is 75%～80% ethanol; Certain temperature is 40～50 ℃.
The present invention has the following advantages:
(1) product purity height: calculate with dry product, gained monoammonium glycyrrhizinate purity salt can reach more than 98%, has broken through currently available products purity.
(2) proterties is good: adopt extraction, crystallization, centrifugal, make product color good, the crystal homogeneous.
(4) prescription is reasonable, practical: the present invention has utilized monoammonium glycyrrhizinate to be soluble in the character of organic solvent, and is both scientific and reasonable, practical, can guarantee its quality again.
(5) preparation technology is simple, quality good, purity is high, and most important is to be applicable to suitability for industrialized production.
Description of drawings
Accompanying drawing 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1:
Acidic ethanol extraction under 40～50 ℃ that Potenlini adds PH=3.5～4.0 of its 5 times amounts, 3 times of amounts is respectively 4h, 3h 2 times, filter united extraction liquid, add ammoniacal liquor and transfer PH=7.2～7.5, centrifugal after the sedimentation, wet product ice acetic acid furnishing scattered paste shape, the static centrifugal monoammonium glycyrrhizinate crude product that gets adds 75% ethanol, gac stirring, at 40～50 ℃ of following reflux decolours, sedimentation filter the wet product of monoammonium glycyrrhizinate, under 50～55 ℃ of conditions, dry, pulverize, sieve the monoammonium glycyrrhizinate elaboration.
Embodiment 2:
Acidic ethanol extraction under 40～50 ℃ that Potenlini adds PH=3.5～4.0 of its 5 times amounts, 3 times of amounts is respectively 4h, 3h 2 times, filter united extraction liquid, add ammoniacal liquor and transfer PH=7.2～7.5, centrifugal after the sedimentation, wet product ice acetic acid furnishing scattered paste shape, the static centrifugal monoammonium glycyrrhizinate crude product that gets adds 80% ethanol, gac stirring, at 40～50 ℃ of following reflux decolours, sedimentation filter the wet product of monoammonium glycyrrhizinate, under 55～60 ℃ of conditions, dry, pulverize, sieve the monoammonium glycyrrhizinate elaboration.
Embodiment 3:
Acidic ethanol extraction under 40～50 ℃ that Potenlini adds the PH=3.5 of its 5 times amounts, 3 times of amounts is respectively 4h, 3h 2 times, filter united extraction liquid, add ammoniacal liquor and transfer PH=7.2, centrifugal after the sedimentation, wet product ice acetic acid furnishing scattered paste shape, the static centrifugal monoammonium glycyrrhizinate crude product that gets adds 75% ethanol, gac stirring, at 40～50 ℃ of following reflux decolours, sedimentation filter the wet product of monoammonium glycyrrhizinate, under 55～60 ℃ of conditions, dry, pulverize, sieve the monoammonium glycyrrhizinate elaboration.
Embodiment 4:
Acidic ethanol extraction under 40～50 ℃ that Potenlini adds the PH=4.0 of its 5 times amounts, 3 times of amounts is respectively 4h, 3h 2 times, filter united extraction liquid, add ammoniacal liquor and transfer PH=7.5, centrifugal after the sedimentation, wet product ice acetic acid furnishing scattered paste shape, the static centrifugal monoammonium glycyrrhizinate crude product that gets adds 80% ethanol, gac stirring, at 40～50 ℃ of following reflux decolours, sedimentation filter the wet product of monoammonium glycyrrhizinate, under 50～55 ℃ of conditions, dry, pulverize, sieve the monoammonium glycyrrhizinate elaboration.
Claims (4)
1. the preparation method of a monoammonium glycyrrhizinate, concrete steps are as follows:
(1) the Potenlini acid alcohols material that adds its 5 times amounts, 3 times of amounts extracts 2 times at a certain temperature and is respectively 4h, 3h, filters united extraction liquid;
(2) add ammoniacal liquor and transfer certain PH, centrifugal after the sedimentation, wet product add organic solvent furnishing scattered paste shape, the static centrifugal monoammonium glycyrrhizinate crude product that gets;
(3) the monoammonium glycyrrhizinate crude product adds certain density alcohols material, gac and stirs, reflux decolour at a certain temperature, sedimentation filter the wet product of monoammonium glycyrrhizinate;
(4) 50～60 ℃ of down oven dry, pulverize, sieve the monoammonium glycyrrhizinate elaboration.
2. the preparation method of a kind of monoammonium glycyrrhizinate as claimed in claim 1 is characterized in that the acid alcohols material in described (1) step is acidic ethanol, and PH is 3.5～4.0; Certain temperature is 40～50 ℃.
3. the preparation method of a kind of monoammonium glycyrrhizinate as claimed in claim 1 is characterized in that certain PH is 7.2～7.5 in described (2) step; Organic solvent is glacial acetic acid.
4. the preparation method of a kind of monoammonium glycyrrhizinate as claimed in claim 1 is characterized in that certain density alcohols material in described (3) step is 75%～80% ethanol; Certain temperature is 40～50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101211823A CN103193856A (en) | 2013-04-10 | 2013-04-10 | Method for preparing mono-ammonium glycyrrhizinate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101211823A CN103193856A (en) | 2013-04-10 | 2013-04-10 | Method for preparing mono-ammonium glycyrrhizinate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103193856A true CN103193856A (en) | 2013-07-10 |
Family
ID=48716688
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101211823A Pending CN103193856A (en) | 2013-04-10 | 2013-04-10 | Method for preparing mono-ammonium glycyrrhizinate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103193856A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819530A (en) * | 2013-12-12 | 2014-05-28 | 吉林长舜制药有限公司 | Monoammonium glycyrrhizinate compound and pharmaceutical composition containing monoammonium 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 |
| CN105237609A (en) * | 2015-10-19 | 2016-01-13 | 新疆天山制药工业有限公司 | Mono-ammonium glycyrrhizinate and preparing method thereof |
| 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 |
| CN108929359A (en) * | 2018-06-20 | 2018-12-04 | 陕西富捷药业有限公司 | A kind of recrystallization method of ammonium glycyrrhizinate |
| CN110051546A (en) * | 2019-05-07 | 2019-07-26 | 绵阳师范学院 | For TiO in cosmetics2The preparation method of careless thuja acid complex microsphere |
| CN112047987A (en) * | 2020-03-31 | 2020-12-08 | 张家港保税区麦福生物制品有限公司 | Preparation method of mono-ammonium glycyrrhizinate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039027A (en) * | 1988-06-30 | 1990-01-24 | 兰州大学 | The manufacture method of edible sweet extract from licorice roots |
| RU2054433C1 (en) * | 1992-01-29 | 1996-02-20 | Малое предприятие "Реакция" | Method for production of glycyrame |
| CN101519422A (en) * | 2008-02-27 | 2009-09-02 | 新疆富沃药业有限公司 | Method for preparing mono-ammonium glycyrrhizinate |
| CN101654471A (en) * | 2009-09-14 | 2010-02-24 | 湖南康普制药有限公司 | Technology of large-scale refining production of glycyrrhetate |
-
2013
- 2013-04-10 CN CN2013101211823A patent/CN103193856A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039027A (en) * | 1988-06-30 | 1990-01-24 | 兰州大学 | The manufacture method of edible sweet extract from licorice roots |
| RU2054433C1 (en) * | 1992-01-29 | 1996-02-20 | Малое предприятие "Реакция" | Method for production of glycyrame |
| CN101519422A (en) * | 2008-02-27 | 2009-09-02 | 新疆富沃药业有限公司 | Method for preparing mono-ammonium glycyrrhizinate |
| CN101654471A (en) * | 2009-09-14 | 2010-02-24 | 湖南康普制药有限公司 | Technology of large-scale refining production of glycyrrhetate |
Non-Patent Citations (4)
| Title |
|---|
| 佟连生 等: "从甘草酸粗品制取甘草酸单铵盐", 《黑龙江医药化学》, vol. 27, no. 4, 31 August 2004 (2004-08-31), pages 51 - 51 * |
| 史高峰 等: "甘草酸单铵盐的制备及纯化新工艺研究", 《食品工业科技》, vol. 23, no. 4, 30 April 2011 (2011-04-30), pages 324 - 326 * |
| 吴安心 等: "甘草酸单铵盐的工艺研究", 《中国医药工业杂志》, vol. 28, no. 11, 30 November 1997 (1997-11-30), pages 486 - 488 * |
| 邓保炜: "从甘草酸粗品制取甘草酸单铵盐", 《中国医药工业杂志》, vol. 21, no. 4, 30 April 1990 (1990-04-30), pages 157 - 157 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819530A (en) * | 2013-12-12 | 2014-05-28 | 吉林长舜制药有限公司 | Monoammonium glycyrrhizinate compound and pharmaceutical composition containing monoammonium 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 |
| CN105237609A (en) * | 2015-10-19 | 2016-01-13 | 新疆天山制药工业有限公司 | Mono-ammonium glycyrrhizinate and preparing method thereof |
| 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 |
| CN108929359A (en) * | 2018-06-20 | 2018-12-04 | 陕西富捷药业有限公司 | A kind of recrystallization method of ammonium glycyrrhizinate |
| CN110051546A (en) * | 2019-05-07 | 2019-07-26 | 绵阳师范学院 | For TiO in cosmetics2The preparation method of careless thuja acid complex microsphere |
| CN112047987A (en) * | 2020-03-31 | 2020-12-08 | 张家港保税区麦福生物制品有限公司 | Preparation method of mono-ammonium glycyrrhizinate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103193856A (en) | Method for preparing mono-ammonium glycyrrhizinate | |
| CN103059095B (en) | A kind of green extraction of yellow ginger resource comprehensive efficiency utilization | |
| CN102898486B (en) | Comprehensive method for preparation of raffinose and gossypol from cottonseed meal | |
| CN105061525A (en) | Preparation method of mono-ammonium glycyrrhizinate | |
| CN102319284A (en) | Method for extracting isoflavone from kudzuvine root efficiently | |
| CN105153091B (en) | The method for improving dihydromyricetin yield in ampelopsis grossdentata | |
| CN106072491B (en) | A kind of fructus arctii base Ganoderma lucidum mycelium powder and preparation method thereof | |
| US9662349B2 (en) | Dietary composition having mixed polysaccharides derived from lucid ganoderma, lycium barbarum and polygonatum sibiricum and method of its preparation | |
| CN102408979B (en) | Method for preparing wild papaya fruit vinegar and wild papaya fruit vinegar prepared by method | |
| CN104186746A (en) | Preparation method of strain fermented tea | |
| CN102512353B (en) | Dictyophora indusiata water extract and preparation method and application thereof | |
| CN104277128A (en) | Preparation process of hericium erinaceus sporophore polysaccharide | |
| CN105663444A (en) | Compound immunity-enhancing and aging-resisting agent and preparation method thereof | |
| CN106901326A (en) | A kind of preparation and application of ganoderma lipsiense full agonist | |
| CN101704703A (en) | Method for producing high-purity lycopene powder by utilizing plant products | |
| CN106942738A (en) | A kind of preparation method of chlorella full agonist and products thereof | |
| CN113398153B (en) | Method for utilizing phellinus igniarius mycelium | |
| CN102783647A (en) | Preparation method of kudzu root isoflavone powder | |
| Hao et al. | Solid-state fermentation of Aspergillus Niger to optimize extraction process of Isoliquiritigenin from Glycyrrhiza uralensis | |
| CN102246988B (en) | Preparation method of composite mushroom functional beverage with sweet osmanthus flower flavor | |
| CN106901325A (en) | A kind of preparation and application of ganoderma lucidum full agonist | |
| Chen et al. | Biotransformation of saponins to astragaloside IV from Radix Astragali by immobilized Aspergillus niger | |
| CN103583229A (en) | Method for producing lucid ganoderma and lucid ganoderma tea by taking leguminous traditional Chinese medicine as raw materials | |
| CN102391232B (en) | The method of Liquiritigenin is extracted from Radix Glycyrrhizae | |
| CN102676397B (en) | Artificial cultivation method of Paecilomyces tenuipes (Peck) Samson and pharmaceutical use of Paecilomyces tenuipes (Peck) Ssamson |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130710 |