CN1023805C - Separate refining method to prepare licorice acid - Google Patents
Separate refining method to prepare licorice acid Download PDFInfo
- Publication number
- CN1023805C CN1023805C CN 88101932 CN88101932A CN1023805C CN 1023805 C CN1023805 C CN 1023805C CN 88101932 CN88101932 CN 88101932 CN 88101932 A CN88101932 A CN 88101932A CN 1023805 C CN1023805 C CN 1023805C
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- CN
- China
- Prior art keywords
- potenlini
- water
- radix glycyrrhizae
- acid
- extract
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- Expired - Fee Related
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The present invention relates to a method for separating and refining glycyrrhizic acid. Glycyrrhiza or the extract of glycyrrhiza is used as a raw material, extracted by using water, separated by using acid, extracted by using alcohol, concentrated, dissolved in water, processed through PH value regulation, adsorbed by using DA-20 macroporous resin, washed by using water, and dried to obtain glycyrrhizic acid with purity higher than 90% and a yield of 75% to 85%. The method for separating and refining glycyrrhizic acid has the advantages of simple technology, low cost, and time and labor saving, and is applicable for commercial production.
Description
The present invention be a kind of from Radix Glycyrrhizae or Radix Glycyrrhizae extract the method for separation and purification Potenlini (GLYCYRRHIZIC ACID).Potenlini has structural formula:
The method of separation and purification Potenlini has multiple from Radix Glycyrrhizae or Radix Glycyrrhizae extract, as solvent extration, ion-exchange-resin process, polymeric amide adsorption method of separation and the ultrafiltration process etc. of classics, it is numerous and diverse that these methods all exist technology, and yield is low, the cost height, shortcoming such as waste time and energy.After the eighties, Japan adopts hydroxyl, amino, ester class macroporous adsorbent resin separation and purification Potenlini, (JP-57-159800,55-13217), though improved yield, separating effect and purity are still undesirable, for obtaining the higher Potenlini of purity, the present invention proposes a kind of new method, its main points are Radix Glycyrrhizae extract to be carried acid out through water, alcohol extracting, after concentrating, be dissolved in water, adjusting PH is 4-9, become and contain Potenlini solution, by being skeleton with vinylbenzene and divinylbenzene, have on the main chain of forming by vinyl cyanide-DA-201 type macroporous resin (production of Tianjin gum plant) the post absorption of CN base is once or once, with water or rare lower alcohol wash-out, collect elutriant, drying obtains the Potenlini product.
Adopt the principle of aforesaid method to be, DA-201 type polymeric adsorbent is strong to the little material adsorption of polarity in water, and bigger to molecular weight, and the material adsorption that wetting ability is strong is more weak or do not adsorb.Contain the flavonoid similar (FLAVONOIDS) in Radix Glycyrrhizae or the Radix Glycyrrhizae extract to the Potenlini physico-chemical property, Coumarins (COUMARIN), cinnamic acid derivative, amino acid, impurity such as carbohydrate, but these impurity are when by DA-201 type resin, adsorbed by resin because polarity is little, and the strong Potenlini of wetting ability is difficult for by resin absorption, water elutes Potenlini, boils off elutriant, can obtain high-purity liquorice acid.
During the invention process, the first step is made Radix Glycyrrhizae extract with Radix Glycyrrhizae earlier, is dissolved in water, drip ore deposit acid while stirring, make below the solution PH to 4, leave standstill and treat post precipitation, supernatant liquor inclines, throw out is washed with water, carrying out drying below 80 ℃, obtain thick Potenlini, the lower alcohol with 70-95% refluxes then, filter, remove insoluble impurities, mother liquor adds ammoniacal liquor, regulates PH to neutral, lower alcohol is removed in distillation, carrying out drying below 80 ℃ once more, prepared post, glycyrrhizic acid content is 38-50% in the product at this moment.
Second step, the thick Potenlini that makes is mixed with the solution of 5-35%, after transferring PH4-9, by DA-201 type resin column, with water or lower alcohol wash-out, till detecting no Potenlini, collect elutriant, carry out evaporated under reduced pressure or spraying drying, obtain product purity and can reach more than 90%, yield is 75-85%.Further improve Potenlini purity as need, also can repeat post.
Thereby the method that the employing U.S. AMBERITE XAD-8 macroporous adsorbent resin of the present invention through generally acknowledging with foreign literature reaches the optimal separation effect relatively, no matter all is being better than this method aspect performance and the separating effect, and the purity of Potenlini can improve 6-7%.
Several embodiments of the present invention are provided below.
Embodiment 1:
Extracting liquorice soaks 300 milliliters of warm dissolvings of powder 100 gram adding distil waters, leaves standstill, and discards insolubles, under agitation slowly drip 3.5 mol sulfuric acid to the PH of solution be 2.0, leave standstill, the supernatant liquor that inclines, precipitation is washed with 3 times of water gagings, and is dry that thick Potenlini 37 restrains.Add 10 times of amount alcohol refluxs, extract secondary, united extraction liquid, dropping ammonia is transferred PH to 7.5, concentrates, and drying gets extract 30 grams.Extract is dissolved in an amount of distilled water, is made into 10% solution, it is extremely neutral to regulate PH, crosses homemade DA-201 type macroporous resin column is housed, and uses the distilled water wash-out, collects elutriant, concentrates, and drying gets faint yellow Potenlini 13.70 grams (containing Potenlini 91.92%).
Embodiment 2:
To go up that used sulfuric acid changes hydrochloric acid among the embodiment, ethanol changes methyl alcohol into, and elutriant is used 10% ethanol instead, and other conditions are constant, obtains refining Potenlini 14.0 grams (containing the Potenlini amount is 90.00%).
Embodiment 3:
Got post Potenlini 30 grams one time, adding distil water makes its dissolving in right amount, is made into 10% solution, transfers PH to neutral, cross homemade DA-201 type macroporous resin column is housed, use the distilled water wash-out, collect elutriant, concentrate, drying gets faint yellow Potenlini 23.21 grams (containing the Potenlini amount is 98.3%).
Adopt major advantage of the present invention to be: good separating effect, the yield height, product purity can reach more than 90%, and technology is simple, and cost is low, and is time saving and energy saving, but resin Reusability after treatment, separating effect does not subtract, and is suitable for suitability for industrialized production.
Claims (1)
- A kind of from Radix Glycyrrhizae or Radix Glycyrrhizae extract the method for separation and purification Potenlini, Potenlini has structural formula:
It is characterized in that Radix Glycyrrhizae or Radix Glycyrrhizae extract are proposed through water acid out, alcohol extracting, after concentrating, be dissolved in water, make 5--35% Potenlini solution, transferring PH is 4～9, by being skeleton with vinylbenzene and divinylbenzene, the DA-201 type macroporous resin column absorption that has a CN base on the main chain of being made up of vinyl cyanide with water or rare lower alcohol wash-out, is collected elutriant once or once, through super-dry, obtain the Potenlini product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88101932 CN1023805C (en) | 1988-04-14 | 1988-04-14 | Separate refining method to prepare licorice acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88101932 CN1023805C (en) | 1988-04-14 | 1988-04-14 | Separate refining method to prepare licorice acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1036960A CN1036960A (en) | 1989-11-08 |
| CN1023805C true CN1023805C (en) | 1994-02-16 |
Family
ID=4831945
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88101932 Expired - Fee Related CN1023805C (en) | 1988-04-14 | 1988-04-14 | Separate refining method to prepare licorice acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1023805C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100343205C (en) * | 2005-11-15 | 2007-10-17 | 江西汇仁药业有限公司 | Method for separating Chinese medicinal active substances |
Families Citing this family (4)
| 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 |
| CN105707658A (en) * | 2016-02-24 | 2016-06-29 | 高颖 | Preparation method of radix glycyrrhizae sweetening agent for removing bitter taste |
| CN107510024A (en) * | 2017-08-24 | 2017-12-26 | 兰溪市捷喜食品加工技术有限公司 | A kind of Flavor release agent and preparation method thereof |
| CN114031664A (en) * | 2021-12-10 | 2022-02-11 | 新疆全安药业股份有限公司 | Method for purifying glycyrrhizic acid |
-
1988
- 1988-04-14 CN CN 88101932 patent/CN1023805C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100343205C (en) * | 2005-11-15 | 2007-10-17 | 江西汇仁药业有限公司 | Method for separating Chinese medicinal active substances |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1036960A (en) | 1989-11-08 |
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