CN102453075A - Separation and purification process of glycyrrhizic acid - Google Patents
Separation and purification process of glycyrrhizic acid Download PDFInfo
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- CN102453075A CN102453075A CN2010105266573A CN201010526657A CN102453075A CN 102453075 A CN102453075 A CN 102453075A CN 2010105266573 A CN2010105266573 A CN 2010105266573A CN 201010526657 A CN201010526657 A CN 201010526657A CN 102453075 A CN102453075 A CN 102453075A
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Abstract
The invention relates to a separation and purification process of glycyrrhizic acid, belonging to the field of pharmaceutical and chemical industry. The method provided by the invention comprises the following steps: hot water extraction, ethanol extraction, macroporous adsorption resin chromatography and elution, and ion-exchange resin chromatography. Because the ion-exchange resin chromatography step is added to the scheme of the invention, the selectivity is greatly improved, so that the purity of the finally obtained product is nearly 99%. The method can be used for preparing medicines and even injections, thereby enlarging the range of application, improving the value of products and lowering the process cost.
Description
Technical field
The present invention relates to a kind of separation purifying technique, more particularly, the present invention relates to a kind of separation purifying technique of Potenlini, belong to field of medicine and chemical technology.
Background technology
Radix Glycyrrhizae (medicinal material title: Radix Glycyrrhiza), be a kind of help herbal medicine.Medicinal part is a root and rhizome, and medicinal material proterties root is cylindrical, long 25～100cm, diameter 0.6～3.5cm.The crust degree of tightness differs, the brown or taupe brown of surface red.Rhizome is cylindrical, and there is the bud trace on the surface, and there is marrow at the section middle part.The little flavor of gas is sweet and special.Function cures mainly clearing heat and detoxicating, expelling phlegm for arresting cough, gastral cavity abdomen etc.Happiness sunlight is abundant, the low arid climate of long temperature at sunshine.Radix Glycyrrhizae is grown in arid, semiarid desert steppe, desert edge and loess hill area more.
Radix Glycyrrhizae is accepted and use by people as a kind of conventional Chinese medicine, and its staple is: glycyrrhizin, Potenlini, liquirtin, flavonoids of Glycyrrhiza, back curtain are than wingceltis element, Formononetin, Quercetin etc.Have detoxifcation, anti-inflammatory, antibechic, antitumor, antiulcer agent, effect such as antibiotic grade.Simultaneously, glycyrrhizin has the inhibition proliferation function to HIV; Glycyrrhetinic acid all has restraining effect to myelomatosis and ascites liver cancer.Potenlini has tangible antidiuretic activity; Liquiritigenin, isoliquiritigenin have antiulcer agent and spasmolysis; The licoflavone class still has antioxygen and bacteriostatic action.
Potenlini is a topmost activeconstituents in the Radix Glycyrrhizae.Potenlini and series product thereof have restraining effect to sarcoma, growth of cancer cells, and the inhibiting rate of AIDS more up to 90%, is had stronger increase immune function of human body effect, and is good foodstuff additive and perfumery base.
Potenlini adopts method extractions such as SX more, but extraction yield is not high, and product purity is lower, with the refining glycyrrhizic acid inclusion compound of macroporous adsorbent resin, has obtained more satisfactory effect afterwards.Macroporous adsorbent resin is big to the adsorptive capacity of glycyrrhizic acid inclusion compound, and can use repeatedly after the flushing, and cost is also lower.
Application number is 88101932.1, and the patent of invention that name is called " separation and refining method of Potenlini " discloses a kind of separation and refining method of Potenlini.Adopting Radix Glycyrrhizae or Radix Glycyrrhizae extract is raw material, carry through water, and acid out, alcohol extracting, it is water-soluble to concentrate the back, transfers PH, with DA-201 type macroporous resin adsorption, again with water elution, drying, the Potenlini product that obtains, purity can reach more than 90%, and yield is 75～85%.Technology of the present invention is simple, and cost is low, and is time saving and energy saving, is applicable to industrial production.
There is following defective in method in the foregoing invention:
Only make with extra care purifying with macroporous adsorbent resin, effect is bad.Because the selectivity of macroporous adsorbent resin is relatively poor; Can be along with Potenlini washes other plurality of impurities; Make the product purity that obtains at last reduce, can only be applied to the use of foodstuff additive, spices and flavouring agent, and not reach medicinal; The standard of injection Potenlini particularly, range of application is dwindled greatly.
Summary of the invention
It is not high that the present invention is intended to solve the product purity that aforesaid method obtains, and the problem that range of application is dwindled provides a kind of separation purifying technique of Potenlini.
In order to realize the foregoing invention purpose, the present technique scheme is specific as follows:
A kind of separation purification method of Potenlini; Comprise that the poach extraction obtains the Potenlini meal, extraction using alcohol obtains glycyrrhizic acid inclusion compound, macroporous adsorption resin chromatography and wash-out, it is characterized in that: after described macroporous adsorption resin chromatography and wash-out operation, resinbed is carried out in the elutriant recovery and analyse.
Described resinbed is analysed operation: concentrate the recovering liq meoh eluate; To solid content be 50-75%; With the distilled water diluting of 3-5 times of volume, last weakly basic anion exchange resin post carries out chromatography again, with the ammoniacal liquor wash-out of 1mol/1; Condensing crystal, drying obtain the sweet acid product of highly purified grass.
Above-mentioned weakly basic anion exchange resin is D350, D370, D331 or A600.
Above-mentioned drying temperature is 70-120 ℃, and be 2-8 hour time of drying.
Described poach abstraction process is: in the Radix Glycyrrhizae film-making, add the zero(ppm) water of 3-5 times of weight, boil to leach after 20-50 minute and boil liquid, with zero(ppm) water filter residue is being carried out 2-4 poach extraction; Merge and boil liquid, 30-80 ℃ concentrates down, slowly adds the hydrochloric acid of 1mol/l, and adjust pH is 2-4.5.; Leave standstill 2-5 hour after-filtration, solid precipitation is washed till neutrality, grind to form 100-200 order powder, obtain the Potenlini meal.
Described extraction using alcohol operation is: poach is extracted obtains the Potenlini meal with 1-3 times of quality, volumetric concentration be the ethanol of 75-90% 35-55 ℃ of refluxed 2-4 time, 30-50 minute at every turn, obtain glycyrrhizic acid inclusion compound.
Described macroporous adsorption resin chromatography and wash-out operation are: it is soluble in water that extraction using alcohol is obtained glycyrrhizic acid inclusion compound, and regulating the pH value is 7-8.5, with treated D101 macroporous adsorption resin chromatography, with the acetone soln wash-out of 10-30%.
The useful technique effect that the present invention brings:
Because shortcomings such as macroporous adsorbent resin poor selectivity have added the step that resinbed is analysed in the scheme of the present invention, selectivity has obtained significantly improving; Make the product purity that obtains at last near 99%; Can be used for medication preparation, or even in the preparation of injection liquid, so both enlarge range of application; The value of product is improved, and the technology cost reduces.
Embodiment
Embodiment 1
The separation and purification of Potenlini
A, poach abstraction process: in the Radix Glycyrrhizae film-making, add the zero(ppm) water of 3 times of weight, boil to leach after 50 minutes and boil liquid, filter residue is being carried out 2 poach extractions with zero(ppm) water; Merge and boil liquid, 30 ℃ concentrate down, slowly add the hydrochloric acid of 1mol/l, and adjust pH is 4.5.; Leave standstill 5 hours after-filtration, solid precipitation is washed till neutrality, grind to form 100 order powder, obtain the Potenlini meal.
B, extraction using alcohol operation: poach extracted obtain the Potenlini meal with 3 times of quality, volumetric concentration is 90% ethanol 55 ℃ of refluxed 4 times, each 30 minutes, obtains glycyrrhizic acid inclusion compound.
C, macroporous adsorption resin chromatography and wash-out operation: it is soluble in water that extraction using alcohol is obtained glycyrrhizic acid inclusion compound, and regulating the pH value is 7, with treated D101 macroporous adsorption resin chromatography, and the acetone soln wash-out with 10%.
D, described resinbed are analysed operation and are: concentrate the recovering liq meoh eluate; To solid content be 50%; Use the distilled water diluting of 5 times of volumes again, last weakly basic anion exchange resin A600 post carries out chromatography, with the ammoniacal liquor wash-out of 1mol/l; Condensing crystal, 120 ℃ obtained the sweet acid product of highly purified grass down in dry 2 hours.
Embodiment 2
The separation and purification of Potenlini
A, poach abstraction process: in the Radix Glycyrrhizae film-making, add the zero(ppm) water of 5 times of weight, boil to leach after 20 minutes and boil liquid, filter residue is being carried out 2 poach extractions with zero(ppm) water; Merge and boil liquid, 30 ℃ concentrate down, slowly add the hydrochloric acid of 1mol/l, and adjust pH is 2; Leave standstill 2 hours after-filtration, solid precipitation is washed till neutrality, grind to form 100 order powder, obtain the Potenlini meal.
B, extraction using alcohol operation: poach extracted obtain the Potenlini meal with times quality, volumetric concentration is 75% ethanol 35 ℃ of refluxed 2-4 time, each 30 minutes, obtains glycyrrhizic acid inclusion compound.
C, macroporous adsorption resin chromatography and wash-out operation: it is soluble in water that extraction using alcohol is obtained glycyrrhizic acid inclusion compound, and regulating the pH value is 7, with treated D101 macroporous adsorption resin chromatography, and the acetone soln wash-out with 10%.
D, described resinbed are analysed operation and are: concentrate the recovering liq meoh eluate; To solid content be 50%; Use the distilled water diluting of 3 times of volumes again, last weakly basic anion exchange resin D350 post carries out chromatography, with the ammoniacal liquor wash-out of 1mol/l; Condensing crystal, 70 ℃ obtained the sweet acid product of highly purified grass down in dry 2 hours.
Embodiment 3
The separation and purification of Potenlini
A, poach abstraction process: in the Radix Glycyrrhizae film-making, add the zero(ppm) water of 5 times of weight, boil to leach after 50 minutes and boil liquid, filter residue is being carried out 4 poach extractions with zero(ppm) water; Merge and boil liquid, 80 ℃ concentrate down, slowly add the hydrochloric acid of 1mol/l, and adjust pH is 4.5.; Leave standstill 5 hours after-filtration, solid precipitation is washed till neutrality, grind to form 200 order powder, obtain the Potenlini meal.
B, extraction using alcohol operation: poach extracted obtain the Potenlini meal with 3 times of quality, volumetric concentration is 90% ethanol 55 ℃ of refluxed 4 times, each 50 minutes, obtains glycyrrhizic acid inclusion compound.
C, macroporous adsorption resin chromatography and wash-out operation: it is soluble in water that extraction using alcohol is obtained glycyrrhizic acid inclusion compound, and regulating the pH value is 8.5, with treated D101 macroporous adsorption resin chromatography, and the acetone soln wash-out with 30%.
D, described resinbed are analysed operation and are: concentrate the recovering liq meoh eluate; To solid content be 75%; Use the distilled water diluting of 5 times of volumes again, last weakly basic anion exchange resin D370 post carries out chromatography, with the ammoniacal liquor wash-out of 1mol/l; Condensing crystal, 120 ℃ obtained the sweet acid product of highly purified grass down in dry 8 hours.
Embodiment 4
The separation and purification of Potenlini
A, poach abstraction process: in the Radix Glycyrrhizae film-making, add the zero(ppm) water of 4 times of weight, boil to leach after 35 minutes and boil liquid, filter residue is being carried out 3 poach extractions with zero(ppm) water; Merge and boil liquid, 50 ℃ concentrate down, slowly add the hydrochloric acid of 1mol/l, and adjust pH is 3.5.; Leave standstill 3.5 hours after-filtration, solid precipitation is washed till neutrality, grind to form 150 order powder, obtain the Potenlini meal.
B, extraction using alcohol operation: poach extracted obtain the Potenlini meal with 2 times of quality, volumetric concentration is 80% ethanol 40 ℃ of refluxed 3 times, each 40 minutes, obtains glycyrrhizic acid inclusion compound.
C, macroporous adsorption resin chromatography and wash-out operation: it is soluble in water that extraction using alcohol is obtained glycyrrhizic acid inclusion compound, and regulating the pH value is 7.5, with treated D101 macroporous adsorption resin chromatography, and the acetone soln wash-out with 20%.
D, described resinbed are analysed operation and are: concentrate the recovering liq meoh eluate; To solid content be 65%; Use the distilled water diluting of 4 times of volumes again, last weakly basic anion exchange resin D331 post carries out chromatography, with the ammoniacal liquor wash-out of 1mol/l; Condensing crystal, 100 ℃ obtained the sweet acid product of highly purified grass down in dry 6 hours.
Claims (7)
1. the separation purification method of a Potenlini; Comprise that the poach extraction obtains the Potenlini meal, extraction using alcohol obtains glycyrrhizic acid inclusion compound, macroporous adsorption resin chromatography and wash-out, it is characterized in that: after described macroporous adsorption resin chromatography and wash-out operation, resinbed is carried out in the elutriant recovery and analyse.
2. the separation purification method of a kind of Potenlini according to claim 1; It is characterized in that: described resinbed is analysed operation and is: concentrate the recovering liq meoh eluate, to solid content be 50-75%, again with the distilled water diluting of 3-5 times of volume; Last weakly basic anion exchange resin post carries out chromatography; With the ammoniacal liquor wash-out of 1mol/l, condensing crystal, drying obtains the sweet acid product of highly purified grass.
3. the separation purification method of a kind of Potenlini according to claim 2, it is characterized in that: above-mentioned weakly basic anion exchange resin is D350, D370, D331 or A600.
4. the separation purification method of a kind of Potenlini according to claim 2, it is characterized in that: above-mentioned drying temperature is 70-120 ℃, be 2-8 hour time of drying.
5. the separation purification method of a kind of Potenlini according to claim 1; It is characterized in that: described poach abstraction process is: the zero(ppm) water that in the Radix Glycyrrhizae film-making, adds 3-5 times of weight; Boil to leach after 20-50 minute and boil liquid, filter residue is being carried out 2-4 poach extraction with zero(ppm) water; Merge and boil liquid, 30-80 ℃ concentrates down, slowly adds the hydrochloric acid of 1mol/l, and adjust pH is 2-4.5; Leave standstill 2-5 hour after-filtration, solid precipitation is washed till neutrality, grind to form 100-200 order powder, obtain the Potenlini meal.
6. the separation purification method of a kind of Potenlini according to claim 1; It is characterized in that: described extraction using alcohol operation is: poach is extracted obtain the Potenlini meal with 1-3 times of quality; Volumetric concentration is that the ethanol of 75-90% is 35-55 ℃ of refluxed 2-4 time; Each 30-50 minute, obtain glycyrrhizic acid inclusion compound.
7. the separation purification method of a kind of Potenlini according to claim 1; It is characterized in that: described macroporous adsorption resin chromatography and wash-out operation are: it is soluble in water that extraction using alcohol is obtained glycyrrhizic acid inclusion compound; Regulating the pH value is 7-8.5; With treated D101 macroporous adsorption resin chromatography, with the acetone soln wash-out of 10-30%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242393A (en) * | 2013-05-13 | 2013-08-14 | 兰州理工大学 | Method for separating and purifying glycyrrhizic acid extracting solution through macroporous resin separation |
| CN104250279A (en) * | 2013-06-28 | 2014-12-31 | 江苏天晟药业有限公司 | Preparation method of 24-hydroxyglycyrrhizic acid |
| CN104262448A (en) * | 2014-09-07 | 2015-01-07 | 四川宝鼎香中药科技开发有限公司 | Method for extracting glycyrrhizic acid for licorice |
| CN104447940A (en) * | 2014-11-28 | 2015-03-25 | 新疆中林生物科技有限公司 | Processing method of glycyrrhizic acid |
| CN106418549A (en) * | 2015-08-06 | 2017-02-22 | 安徽华明制药有限公司 | Glycyrrhizin-containing enteral nutrition emulsion and preparation method thereof |
| CN106892949A (en) * | 2017-02-20 | 2017-06-27 | 大连工业大学 | It is a kind of to extract the method for separating glycyrrhizic acid, glycyrrhiza total flavonoid simultaneously based on continuous chromatography technology |
| CN107412319A (en) * | 2017-06-02 | 2017-12-01 | 新疆全泰兴药业科技有限公司 | A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound |
| CN109315668A (en) * | 2018-11-20 | 2019-02-12 | 中国科学院兰州化学物理研究所 | A kind of fructus lycii Radix Glycyrrhizae solid beverage and preparation method thereof |
| CN111214637A (en) * | 2020-03-10 | 2020-06-02 | 贵州神奇药物研究院 | Traditional Chinese medicine composition and preparation method and medicinal application thereof |
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2010
- 2010-10-26 CN CN2010105266573A patent/CN102453075A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242393A (en) * | 2013-05-13 | 2013-08-14 | 兰州理工大学 | Method for separating and purifying glycyrrhizic acid extracting solution through macroporous resin separation |
| CN104250279A (en) * | 2013-06-28 | 2014-12-31 | 江苏天晟药业有限公司 | Preparation method of 24-hydroxyglycyrrhizic acid |
| CN104262448A (en) * | 2014-09-07 | 2015-01-07 | 四川宝鼎香中药科技开发有限公司 | Method for extracting glycyrrhizic acid for licorice |
| CN104262448B (en) * | 2014-09-07 | 2017-02-08 | 四川宝鼎香中药科技开发有限公司 | Method for extracting glycyrrhizic acid for licorice |
| CN104447940A (en) * | 2014-11-28 | 2015-03-25 | 新疆中林生物科技有限公司 | Processing method of glycyrrhizic acid |
| CN106418549A (en) * | 2015-08-06 | 2017-02-22 | 安徽华明制药有限公司 | Glycyrrhizin-containing enteral nutrition emulsion and preparation method thereof |
| CN106892949A (en) * | 2017-02-20 | 2017-06-27 | 大连工业大学 | It is a kind of to extract the method for separating glycyrrhizic acid, glycyrrhiza total flavonoid simultaneously based on continuous chromatography technology |
| CN106892949B (en) * | 2017-02-20 | 2019-03-26 | 大连工业大学 | A method of extracting separation glycyrrhizic acid, glycyrrhiza total flavonoid simultaneously based on continuous chromatography technology |
| CN107412319A (en) * | 2017-06-02 | 2017-12-01 | 新疆全泰兴药业科技有限公司 | A kind of efficiency reduces the method for glycyrrhizic acid and enoxolone in liquorice flavonoids compound |
| CN109315668A (en) * | 2018-11-20 | 2019-02-12 | 中国科学院兰州化学物理研究所 | A kind of fructus lycii Radix Glycyrrhizae solid beverage and preparation method thereof |
| CN111214637A (en) * | 2020-03-10 | 2020-06-02 | 贵州神奇药物研究院 | Traditional Chinese medicine composition and preparation method and medicinal application thereof |
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