CN103833805A - Process for refining glycyrrhizinic acid in liquorice - Google Patents
Process for refining glycyrrhizinic acid in liquorice Download PDFInfo
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- CN103833805A CN103833805A CN201210489631.5A CN201210489631A CN103833805A CN 103833805 A CN103833805 A CN 103833805A CN 201210489631 A CN201210489631 A CN 201210489631A CN 103833805 A CN103833805 A CN 103833805A
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- radix glycyrrhizae
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- refining
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- poach
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Abstract
The invention relates to a process for refining glycyrrhizinic acid in liquorice, belonging to the technical field of extraction and refining of effective components in traditional Chinese medicines. According to the method, the liquorice acid-base in liquorice is extracted and refined by combining boiling extraction by using water, extraction by using menthol and extraction by using macroporous adsorption resin, thereby solving the problems that in the prior art, glycyrrhizinic acid can not be effectively refined by using a macroporous adsorption resin method, and the conventional technique is complex in process and relatively high in cost; glycyrrhizinic acid in liquorice can be effectively extracted and refined; moreover, the process is simple, and the cost is low.
Description
Technical field
The present invention relates to the extraction and purification process of effective constituent in a kind of Chinese medicine, more particularly, the present invention relates to a kind of process for refining of Radix Glycyrrhizae acid, belong to extracts active ingredients purification techniques field in Chinese medicine.
Background technology
Radix Glycyrrhizae is a kind of help herbal medicine.Medicinal part is root and rhizome, and Medicinal Materials Characters root is cylindrical, long 25～100cm, diameter 0.6～3.5cm.Crust degree of tightness differs, the brown or taupe brown of surface red.Rhizome is cylindrical, and there is bud trace on surface, and there is marrow at section middle part.Gas is micro-, and taste 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.
Potenlini is the main effective constituent in Radix Glycyrrhizae, and tool has been widely used, and in prior art, the methods such as solvent extraction or ion exchange resin that adopt are extracted more, and extraction yield is very low.
It is 88101932.1 that State Intellectual Property Office discloses an application number in 1989.11.8, and name is called the patent of invention of " separation and refining method of Potenlini ", the separation and refining method that this patent is a kind of Potenlini.Adopting Radix Glycyrrhizae or Radix Glycyrrhizae extract is raw material, through water extraction, and acid out, alcohol extracting, concentrated rear water-soluble, adjust PH, by DA-201 type macroporous resin adsorption, then with water elution, dry, the Potenlini product obtaining, purity is more than 90%, and yield is 75-85%.Technique of the present invention is simple, and cost is low, time saving and energy saving, is applicable to industrial production.
It is 201110287907.7 that State Intellectual Property Office discloses an application number in 2012.3.28, name is called the patent of invention of " method of extracting liquirtin from Radix Glycyrrhizae ", this patent discloses a kind of method of extracting liquirtin from Radix Glycyrrhizae, the method comprises the steps: that (1) pulverize Radix Glycyrrhizae, with deionized water extraction, filter, obtain liquirtin crude extract; (2) by hybrid resin post on liquirtin crude extract, and carry out wash-out separation and purification recrystallization.The liquirtin that method of the present invention is extracted is natural extract, and purity is high, and cost is low, and production efficiency is high, stable and controllable for quality.
In above-mentioned first section of patent, be the Flavonoids by Macroporous Adsorption Resin of refining Potenlini, but operating procedure is loaded down with trivial details, cost is higher, and second section be refining to liquirtin, and is not suitable for refining for Potenlini of the present invention.
Summary of the invention
The present invention is intended to solve in above-mentioned prior art and cannot effectively adopts Flavonoids by Macroporous Adsorption Resin to refine Potenlini, and prior art processes is loaded down with trivial details, the problem that cost is higher, a kind of process for refining of Radix Glycyrrhizae acid is provided, adopt the Flavonoids by Macroporous Adsorption Resin of optimizing, Potenlini in high efficiency extraction Radix Glycyrrhizae, and simple to operate, cost is low.
In order to realize foregoing invention object, its concrete technical scheme is as follows:
A process for refining for Radix Glycyrrhizae acid, is characterized in that: comprise following processing step:
A, macroporous adsorbent resin pre-treatment
Taking weight ratio is D101 type macroporous adsorbent resin and the AB-8 type macroporous adsorbent resin of 1:2-4, soaks 1-3 days with anhydrous primary isoamyl alcohol, repeat above-mentioned steps 2-5 time until in primary isoamyl alcohol without white precipitate;
B, dress macroporous adsorptive resins
The good macroporous adsorbent resin of pre-treatment is added to methyl alcohol submergence, pour in adsorption column, wash, for subsequent use;
C, poach extract
By Radix Glycyrrhizae crushed after being dried, add water, boil rear maintenance boiling state 40-55 minute, leach water cooking liquid, by filter residue poach extraction at twice, the poach time is 20-25 minute and 10-20 minute, merges three times water cooking liquid, concentrating under reduced pressure at 60-75 DEG C, after being cooled to room temperature, add oxalic acid crystal, then regulate pH value for 2-5, place after 4-7 hour and filter, solid is washed till to neutrality, obtains solid hot water extract;
D, methanol extraction
The solid hot water extract that step C is obtained adopts 75% methanol eddy to extract 30-50 minute, and after filtration, by methanol extract liquid activated carbon decolorizing, elimination gac, is adjusted to 7-9 by the pH value of filtrate, and evaporate to dryness methyl alcohol obtains thickness pulpous state extract;
E, macroporous adsorbent resin extract
The thick extract that step D is obtained is soluble in water, and it be neutral regulating pH, and adopting the ethanol of 10-80% is elutriant, carries out chromatography with the ready adsorption column of step B, obtains the Potenlini extract after refining.
Preferably, the present invention is in steps A, and described D101 type macroporous adsorbent resin and AB-8 type macroporous adsorbent resin gross weight are 1:3.5-5(g/ml with the ratio of anhydrous primary isoamyl alcohol volume).
Preferably, the present invention is in step C, and the described amount of water of poach is for the first time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:5-7(g/ml).
Preferably, the present invention is in step C, and the described amount of water of poach is for the second time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:3-6(g/ml).
Preferably, the present invention is in step C, and the described amount of water of poach is for the third time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:2-5(g/ml).
Preferably, the present invention is in step C, and described adjusting pH value adopts the sulfuric acid of 1mol/L to regulate for 2-5 refers to.
Preferably, the present invention is in step D, and 75% described methyl alcohol add-on is that described solid hot water extract and the weightmeasurement ratio of 75% methyl alcohol are 1:3.5-6(g/ml).
Preferably, the present invention is in step e, and described elutriant is 15% ethanol.
Preferably, the present invention is in step e, and described elutriant speed control is 0.5-2ml/(cm
2min).
The useful technique effect that the present invention brings:
1, the mode that the present invention adopts poach extraction, methanol extraction and macroporous absorption tree to extract combination is carried out purifying to the Radix Glycyrrhizae soda acid in Radix Glycyrrhizae, having solved prior art cannot effectively adopt Flavonoids by Macroporous Adsorption Resin to refine Potenlini, and prior art processes is loaded down with trivial details, the problem that cost is higher, can high efficiency extraction refine the Potenlini in Radix Glycyrrhizae, and technique is simple, with low cost.
2,, in steps A, adopt the ratio of two kinds of macroporous adsorbent resins of parameter control of the present invention, better the Potenlini in the refining Radix Glycyrrhizae of chromatography.
3, three poach that the present invention adopts in step C and the processing parameter of amount of water can effectively and stably make process transition refining in conjunction with the chromatography of macroporous adsorbent resin, make adsorption effect reach best, improve the effect of final refining.
Embodiment
embodiment 1
A process for refining for Radix Glycyrrhizae acid, comprises following processing step:
A, macroporous adsorbent resin pre-treatment
Taking weight ratio is D101 type macroporous adsorbent resin and the AB-8 type macroporous adsorbent resin of 1:2, soaks 1 day with anhydrous primary isoamyl alcohol, repeat above-mentioned steps 2 times until in primary isoamyl alcohol without white precipitate;
B, dress macroporous adsorptive resins
The good macroporous adsorbent resin of pre-treatment is added to methyl alcohol submergence, pour in adsorption column, wash, for subsequent use;
C, poach extract
By Radix Glycyrrhizae crushed after being dried, add water, boil rear maintenance boiling state 40 minutes, leach water cooking liquid, by filter residue poach extraction at twice, the poach time is 20 minutes and 10 minutes, merges three times water cooking liquid, concentrating under reduced pressure at 60 DEG C, after being cooled to room temperature, add oxalic acid crystal, then to regulate pH value be 2, place after 4 hours and filter, solid is washed till to neutrality, obtains solid hot water extract;
D, methanol extraction
The solid hot water extract that step C is obtained adopts 75% methanol eddy to extract 30 minutes, and after filtration, by methanol extract liquid activated carbon decolorizing, elimination gac, is adjusted to 7 by the pH value of filtrate, and evaporate to dryness methyl alcohol obtains thickness pulpous state extract;
E, macroporous adsorbent resin extract
The thick extract that step D is obtained is soluble in water, and it be neutral regulating pH, and adopting 10% ethanol is elutriant, carries out chromatography with the ready adsorption column of step B, obtains the Potenlini extract after refining.
embodiment 2
A process for refining for Radix Glycyrrhizae acid, comprises following processing step:
A, macroporous adsorbent resin pre-treatment
Taking weight ratio is D101 type macroporous adsorbent resin and the AB-8 type macroporous adsorbent resin of 1:4, soaks 3 days with anhydrous primary isoamyl alcohol, repeat above-mentioned steps 5 times until in primary isoamyl alcohol without white precipitate;
B, dress macroporous adsorptive resins
The good macroporous adsorbent resin of pre-treatment is added to methyl alcohol submergence, pour in adsorption column, wash, for subsequent use;
C, poach extract
By Radix Glycyrrhizae crushed after being dried, add water, boil rear maintenance boiling state 55 minutes, leach water cooking liquid, by filter residue poach extraction at twice, the poach time is 25 minutes and 20 minutes, merges three times water cooking liquid, concentrating under reduced pressure at 75 DEG C, after being cooled to room temperature, add oxalic acid crystal, then to regulate pH value be 5, place after 7 hours and filter, solid is washed till to neutrality, obtains solid hot water extract;
D, methanol extraction
The solid hot water extract that step C is obtained adopts 75% methanol eddy to extract 50 minutes, and after filtration, by methanol extract liquid activated carbon decolorizing, elimination gac, is adjusted to 9 by the pH value of filtrate, and evaporate to dryness methyl alcohol obtains thickness pulpous state extract;
E, macroporous adsorbent resin extract
The thick extract that step D is obtained is soluble in water, and it be neutral regulating pH, and adopting 80% ethanol is elutriant, carries out chromatography with the ready adsorption column of step B, obtains the Potenlini extract after refining.
embodiment 3
A process for refining for Radix Glycyrrhizae acid, comprises following processing step:
A, macroporous adsorbent resin pre-treatment
Taking weight ratio is D101 type macroporous adsorbent resin and the AB-8 type macroporous adsorbent resin of 1:3, soaks 2 days with anhydrous primary isoamyl alcohol, repeat above-mentioned steps 3 times until in primary isoamyl alcohol without white precipitate;
B, dress macroporous adsorptive resins
The good macroporous adsorbent resin of pre-treatment is added to methyl alcohol submergence, pour in adsorption column, wash, for subsequent use;
C, poach extract
By Radix Glycyrrhizae crushed after being dried, add water, boil rear maintenance boiling state 50 minutes, leach water cooking liquid, by filter residue poach extraction at twice, the poach time is 22 minutes and 15 minutes, merges three times water cooking liquid, concentrating under reduced pressure at 65 DEG C, after being cooled to room temperature, add oxalic acid crystal, then to regulate pH value be 3, place after 5 hours and filter, solid is washed till to neutrality, obtains solid hot water extract;
D, methanol extraction
The solid hot water extract that step C is obtained adopts 75% methanol eddy to extract 40 minutes, and after filtration, by methanol extract liquid activated carbon decolorizing, elimination gac, is adjusted to 8 by the pH value of filtrate, and evaporate to dryness methyl alcohol obtains thickness pulpous state extract;
E, macroporous adsorbent resin extract
The thick extract that step D is obtained is soluble in water, and it be neutral regulating pH, and adopting 45% ethanol is elutriant, carries out chromatography with the ready adsorption column of step B, obtains the Potenlini extract after refining.
embodiment 4
On the basis of embodiment 1-3, preferred:
In steps A, described D101 type macroporous adsorbent resin and AB-8 type macroporous adsorbent resin gross weight are 1:3.5 with the ratio of anhydrous primary isoamyl alcohol volume.
In step C, the described amount of water of poach is for the first time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:5.
In step C, the described amount of water of poach is for the second time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:3.
In step C, the described amount of water of poach is for the third time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:2.
In step C, described adjusting pH value is 2 to refer to and adopt the sulfuric acid of 1mol/L to regulate.
In step D, 75% described methyl alcohol add-on is that described solid hot water extract and the weightmeasurement ratio of 75% methyl alcohol are 1:3.5.
In step e, described elutriant is 15% ethanol.
In step e, described elutriant speed control is 0.5ml/(cm
2min).
embodiment 5
On the basis of embodiment 1-3, preferred:
In steps A, described D101 type macroporous adsorbent resin and AB-8 type macroporous adsorbent resin gross weight are 1:5 with the ratio of anhydrous primary isoamyl alcohol volume.
In step C, the described amount of water of poach is for the first time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:7.
In step C, the described amount of water of poach is for the second time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:6.
In step C, the described amount of water of poach is for the third time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:5.
In step C, described adjusting pH value is 5 to refer to and adopt the sulfuric acid of 1mol/L to regulate.
In step D, 75% described methyl alcohol add-on is that described solid hot water extract and the weightmeasurement ratio of 75% methyl alcohol are 1:6.
In step e, described elutriant is 15% ethanol.
In step e, described elutriant speed control is 2ml/(cm
2min).
embodiment 6
On the basis of embodiment 1-3, preferred:
In steps A, described D101 type macroporous adsorbent resin and AB-8 type macroporous adsorbent resin gross weight are 1:4 with the ratio of anhydrous primary isoamyl alcohol volume.
In step C, the described amount of water of poach is for the first time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:6.
In step C, the described amount of water of poach is for the second time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:4.
In step C, the described amount of water of poach is for the third time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:3.
In step C, described adjusting pH value is 3 to refer to and adopt the sulfuric acid of 1mol/L to regulate.
In step D, 75% described methyl alcohol add-on is that described solid hot water extract and the weightmeasurement ratio of 75% methyl alcohol are 1:4.
In step e, described elutriant is 15% ethanol.
In step e, described elutriant speed control is 1ml/(cm
2min).
Claims (9)
1. a process for refining for Radix Glycyrrhizae acid, is characterized in that: comprise following processing step:
A, macroporous adsorbent resin pre-treatment
Taking weight ratio is D101 type macroporous adsorbent resin and the AB-8 type macroporous adsorbent resin of 1:2-4, soaks 1-3 days with anhydrous primary isoamyl alcohol, repeat above-mentioned steps 2-5 time until in primary isoamyl alcohol without white precipitate;
B, dress macroporous adsorptive resins
The good macroporous adsorbent resin of pre-treatment is added to methyl alcohol submergence, pour in adsorption column, wash, for subsequent use;
C, poach extract
By Radix Glycyrrhizae crushed after being dried, add water, boil rear maintenance boiling state 40-55 minute, leach water cooking liquid, by filter residue poach extraction at twice, the poach time is 20-25 minute and 10-20 minute, merges three times water cooking liquid, concentrating under reduced pressure at 60-75 DEG C, after being cooled to room temperature, add oxalic acid crystal, then regulate pH value for 2-5, place after 4-7 hour and filter, solid is washed till to neutrality, obtains solid hot water extract;
D, methanol extraction
The solid hot water extract that step C is obtained adopts 75% methanol eddy to extract 30-50 minute, and after filtration, by methanol extract liquid activated carbon decolorizing, elimination gac, is adjusted to 7-9 by the pH value of filtrate, and evaporate to dryness methyl alcohol obtains thickness pulpous state extract;
E, macroporous adsorbent resin extract
The thick extract that step D is obtained is soluble in water, and it be neutral regulating pH, and adopting the ethanol of 10-80% is elutriant, carries out chromatography with the ready adsorption column of step B, obtains the Potenlini extract after refining.
2. the process for refining of a kind of Radix Glycyrrhizae acid according to claim 1, is characterized in that: in steps A, described D101 type macroporous adsorbent resin and AB-8 type macroporous adsorbent resin gross weight are 1:3.5-5 with the ratio of anhydrous primary isoamyl alcohol volume.
3. the process for refining of a kind of Radix Glycyrrhizae acid according to claim 1, is characterized in that: in step C, the described amount of water of poach is for the first time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:5-7.
4. the process for refining of a kind of Radix Glycyrrhizae acid according to claim 1, is characterized in that: in step C, the described amount of water of poach is for the second time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:3-6.
5. the process for refining of a kind of Radix Glycyrrhizae acid according to claim 1, is characterized in that: in step C, the described amount of water of poach is for the third time that described Radix Glycyrrhizae and the weightmeasurement ratio of water are 1:2-5.
6. the process for refining of a kind of Radix Glycyrrhizae acid according to claim 1, is characterized in that: in step C, described adjusting pH value adopts the sulfuric acid of 1mol/L to regulate for 2-5 refers to.
7. the process for refining of a kind of Radix Glycyrrhizae acid according to claim 1, is characterized in that: in step D, 75% described methyl alcohol add-on is that described solid hot water extract and the weightmeasurement ratio of 75% methyl alcohol are 1:3.5-6.
8. the process for refining of a kind of Radix Glycyrrhizae acid according to claim 1, is characterized in that: in step e, described elutriant is 15% ethanol.
9. the process for refining of a kind of Radix Glycyrrhizae acid according to claim 1, is characterized in that: in step e, described elutriant speed control is 0.5-2ml/(cm
2min).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105707658A (en) * | 2016-02-24 | 2016-06-29 | 高颖 | Preparation method of radix glycyrrhizae sweetening agent for removing bitter taste |
| CN107501094A (en) * | 2017-07-26 | 2017-12-22 | 天津泽达天健科技有限公司 | A kind of preparation method of high-purity chlorogenic acid |
| CN114478680A (en) * | 2021-12-15 | 2022-05-13 | 贵州弘康药业有限公司 | Licorice extraction process |
-
2012
- 2012-11-27 CN CN201210489631.5A patent/CN103833805A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105707658A (en) * | 2016-02-24 | 2016-06-29 | 高颖 | Preparation method of radix glycyrrhizae sweetening agent for removing bitter taste |
| CN107501094A (en) * | 2017-07-26 | 2017-12-22 | 天津泽达天健科技有限公司 | A kind of preparation method of high-purity chlorogenic acid |
| CN114478680A (en) * | 2021-12-15 | 2022-05-13 | 贵州弘康药业有限公司 | Licorice extraction process |
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Application publication date: 20140604 |