CN1272501A - Supercritical CO2 extraction method for extracting glycyrrhizinic acid from licorice - Google Patents
Supercritical CO2 extraction method for extracting glycyrrhizinic acid from licorice Download PDFInfo
- Publication number
- CN1272501A CN1272501A CN00105599A CN00105599A CN1272501A CN 1272501 A CN1272501 A CN 1272501A CN 00105599 A CN00105599 A CN 00105599A CN 00105599 A CN00105599 A CN 00105599A CN 1272501 A CN1272501 A CN 1272501A
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- CN
- China
- Prior art keywords
- extraction
- supercritical
- potenlini
- temperature
- pressure
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- 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.)
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Links
- 238000000605 extraction Methods 0.000 title claims abstract description 21
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 title claims abstract description 20
- 235000001453 Glycyrrhiza echinata Nutrition 0.000 title claims abstract description 4
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 title claims abstract description 4
- 235000017382 Glycyrrhiza lepidota Nutrition 0.000 title claims abstract description 4
- 229940010454 licorice Drugs 0.000 title claims abstract description 4
- 240000004670 Glycyrrhiza echinata Species 0.000 title claims abstract 3
- 229960004949 glycyrrhizic acid Drugs 0.000 title abstract 4
- 235000019410 glycyrrhizin Nutrition 0.000 title abstract 4
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 239000000284 extract Substances 0.000 claims description 11
- 239000003607 modifier Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- VTAJIXDZFCRWBR-UHFFFAOYSA-N Licoricesaponin B2 Natural products C1C(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2)C(O)=O)C)(C)CC2)(C)C2C(C)(C)CC1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O VTAJIXDZFCRWBR-UHFFFAOYSA-N 0.000 abstract 3
- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 abstract 3
- UYRUBYNTXSDKQT-UHFFFAOYSA-N glycyrrhizic acid Natural products CC1(C)C(CCC2(C)C1CCC3(C)C2C(=O)C=C4C5CC(C)(CCC5(C)CCC34C)C(=O)O)OC6OC(C(O)C(O)C6OC7OC(O)C(O)C(O)C7C(=O)O)C(=O)O UYRUBYNTXSDKQT-UHFFFAOYSA-N 0.000 abstract 3
- 239000001685 glycyrrhizic acid Substances 0.000 abstract 3
- 235000019441 ethanol Nutrition 0.000 abstract 2
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- 208000030507 AIDS Diseases 0.000 description 3
- 241000202807 Glycyrrhiza Species 0.000 description 2
- 241000725303 Human immunodeficiency virus Species 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 102000014150 Interferons Human genes 0.000 description 1
- 108010050904 Interferons Proteins 0.000 description 1
- 210000004404 adrenal cortex Anatomy 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 235000019580 granularity Nutrition 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
- 230000003053 immunization Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229940079322 interferon Drugs 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Extraction Or Liquid Replacement (AREA)
Abstract
The method for extracting and refining glycyrrhizic acid from licorice (or crude glycyrrhizic acid) by using supercritical CO2 extraction includes two steps: first step, using supercritical CO2 extraction to remove non-polar oil impurity, controlling extraction pressure to 25 plus or minus 2 MPa, and its temp. is 55 deg.C; and second step, adding 95% ethyl alcohol modifying agent to supercritical CO2, controlling flow ratio of ethyl alcohol: CO2=5-10 : 100, its pressure is 22 plus or minus 2 MPa, and temp. is 55 deg.C. Its yield is 4%, and purity of refined glycyrrhizic acid is 98.2%. Its technological process is simple and reliable, CO2 and modifying agent can be cyclically used, its product purity is high and it has no solvent residue, and has no environmental pollution.
Description
The present invention relates to a kind of method of from Radix Glycyrrhizae, extracting Potenlini, particularly a kind of supercritical CO
2From Radix Glycyrrhizae, extract the method for Potenlini.
Effective ingredient Potenlini in the Radix Glycyrrhizae is precious natural saponin, have the adrenal cortex of promotion and swash the sample effect, enhancing body immunizing power, can impel AIDS VICTIMS's immunologic function to recover especially, induce synthesizing of human interferon, propagation and cytopathy to HIV (human immunodeficiency virus) have the obvious suppression effect, to the inhibiting rate of AIDS high reach 98%, be called as " jinx of AIDS ".
At present, organic solvent method is still adopted in the extraction of Radix Glycyrrhizae, and this method is not only extracted long flow path, consumed a large amount of solvents, energy consumption height, low, the serious environment pollution of yield; And product purity is low, the organic solvent of residual excess, has a strong impact on product quality product and market sale.
The object of the present invention is to provide a kind of supercritical CO
2From Radix Glycyrrhizae (or thick Potenlini), extract the method for Potenlini.Product characteristics is purity height, extraction yield height, low, the environmentally safe of energy consumption.
Embodiment of the present invention are as follows: as shown in Figure 1.Altogether in two steps: the first step, use supercritical CO earlier
2Remove non polar impurities.The licorice that to clean oven dry is crushed to the 20-40 order, places the charging basket of extraction kettle 1, opens high pressure CO
2Pump 10, by condenser 7 with fresh CO
2After sending into high-pressure pump 10, enter high pressure extraction still 1 through preheater 11 and extract.Control extraction kettle 1 pressure is at 25 ± 2MPa, and temperature is 50-55 ℃, extracts time 2-3 hour, and condenser 7 temperature are 5 ℃, and logistics is heated to 55 ℃ through well heater 2 behind the extraction decon, is collected CO at two series connection separator (3,4) step-down rear impurities
2Circulate through condenser 7 again; Second step is for extracting Potenlini.After extraction 2-3 hour, start properties-correcting agent pump 9, with the properties-correcting agent in the properties-correcting agent groove 8, be about to 95% ethanol and also squeeze into preheater 11, control CO as properties-correcting agent
2With the properties-correcting agent throughput ratio be 100: 5-10, pressure are 22 ± 2MPa, and temperature is 55 ℃, extract 3-4 hour, and extract stream is through well heater 2, and 55 ℃ of temperature enter another group two placed in-line separators (5,6), Potenlini under the separated and collected.
Advantage of the present invention is, flow process is simple, reliable, and the Potenlini yield is 4%.
Following preference 1 couple of the present invention in conjunction with the accompanying drawings is described in detail, but does not mean that and limit the scope of the invention.
Example 1 is cleaned 3 kilograms of Radix Glycyrrhizaes, puts into 10 liters of extraction kettle 1 barrels after drying and be crushed to 40 order granularities, starts high-pressure pump 10, with CO
2Through condenser 7 suction and be pressurized to 25 ± 2MPa, be heated to 55 ℃ through preheater 11, send into extraction kettle 1 and extract removal impurity, after having the non polar impurities logistics and coming out from extraction kettle 1, entering well heater 2 controlled temperature is 55 ℃, enters two series connection separators 3,4 after the step-down.CO
2Nonpolar oily impurity is emitted in logistics from separator top.Then, start properties-correcting agent pump 9,95% ethanol modifiers in the properties-correcting agent groove 8 are extracted out, before preheater 11 and CO
2Stream mixes, and its throughput ratio is 5-10: 100 pressure are 22 ± 2MPa, and temperature is 55 ℃, extracted 3-4 hour, and contained the logistics heater via 2 of Potenlini, 55 ℃ of temperature, enter after another group series connection separator (5,6) step-down Potenlini 0.12Kg under the separated and collected, yield is 4%, and purity is 98%.
Example 2, raw material are thick Potenlini, content 70%, and weight is 5 kilograms, puts into extraction kettle 1 charging basket, extraction conditions is constant, must make with extra care 3.5 kilograms of Potenlinis, yield 70%.Product is made with extra care Potenlini purity 98.2% through liquid-phase chromatographic analysis.
Claims (1)
1, a kind of supercritical CO
2From Radix Glycyrrhizae, extract the method for Potenlini.It is characterized in that:
1) at first removes nonpolar oily impurity.The Radix Glycyrrhizae wash clean is dried and is crushed to granularity is 20-40 purpose licorice, puts into the barrel of extraction kettle 1, opens high pressure CO
2Pump 10, suction CO
2After entering high-pressure pump 10 by condenser 7, enter extraction kettle 1 through preheater 11, control extraction kettle 1 pressure is at 25 ± 2MPa, temperature is 55 ℃, extracted 2-3 hour, the temperature of condenser 7 is 5 ℃, and extract stream is heated to 55 ℃ through well heater 2, nonpolar oily impurity is collected in step-down in two series connection separators 3,4;
2) and then extract Potenlini.After extraction 2-3 hour, start properties-correcting agent pump 9,95% ethanol modifiers in the properties-correcting agent groove 8 are extracted out, before preheater 11 and CO
2Stream mixes, and controlling its throughput ratio is 5-10: 100.Extracting pressure is 22 ± 2MPa, and temperature is 55 ℃, enters another group two placed in-line separators (5,6) after the step-down of extraction back logistics process well heater 2 (55 ℃ of temperature), isolates Potenlini.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001055992A CN1136225C (en) | 2000-04-03 | 2000-04-03 | Supercritical CO2 extraction method for extracting glycyrrhizinic acid from licorice |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001055992A CN1136225C (en) | 2000-04-03 | 2000-04-03 | Supercritical CO2 extraction method for extracting glycyrrhizinic acid from licorice |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1272501A true CN1272501A (en) | 2000-11-08 |
| CN1136225C CN1136225C (en) | 2004-01-28 |
Family
ID=4577806
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001055992A Expired - Fee Related CN1136225C (en) | 2000-04-03 | 2000-04-03 | Supercritical CO2 extraction method for extracting glycyrrhizinic acid from licorice |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1136225C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8236360B2 (en) | 2007-05-02 | 2012-08-07 | Tom's Of Maine, Inc. | Supercritical CO2 liquorice extract and products made there from |
| US8877266B2 (en) | 2007-05-02 | 2014-11-04 | Tom's Of Maine, Inc. | Supercritical CO2 liquorice extract anti-microbial and anti-inflammatory isolates and products made there from |
| CN107376406A (en) * | 2017-07-27 | 2017-11-24 | 源田生物科技有限公司 | Preparation method of sweetener |
| CN107814827A (en) * | 2017-11-06 | 2018-03-20 | 金学芳 | A kind of extracting method of high activity glycyrrhizic acid |
| CN108997470A (en) * | 2018-08-31 | 2018-12-14 | 杨雯君 | A method of extracting glycyrrhizic acid |
Families Citing this family (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 |
-
2000
- 2000-04-03 CN CNB001055992A patent/CN1136225C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8236360B2 (en) | 2007-05-02 | 2012-08-07 | Tom's Of Maine, Inc. | Supercritical CO2 liquorice extract and products made there from |
| US8877266B2 (en) | 2007-05-02 | 2014-11-04 | Tom's Of Maine, Inc. | Supercritical CO2 liquorice extract anti-microbial and anti-inflammatory isolates and products made there from |
| CN107376406A (en) * | 2017-07-27 | 2017-11-24 | 源田生物科技有限公司 | Preparation method of sweetener |
| CN107814827A (en) * | 2017-11-06 | 2018-03-20 | 金学芳 | A kind of extracting method of high activity glycyrrhizic acid |
| CN108997470A (en) * | 2018-08-31 | 2018-12-14 | 杨雯君 | A method of extracting glycyrrhizic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1136225C (en) | 2004-01-28 |
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