CN1136225C - Supercritical CO2 extraction method for extracting glycyrrhizinic acid from licorice - Google Patents

Supercritical CO2 extraction method for extracting glycyrrhizinic acid from licorice Download PDF

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CN1136225C
CN1136225C CNB001055992A CN00105599A CN1136225C CN 1136225 C CN1136225 C CN 1136225C CN B001055992 A CNB001055992 A CN B001055992A CN 00105599 A CN00105599 A CN 00105599A CN 1136225 C CN1136225 C CN 1136225C
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extraction
temperature
supercritical
potenlini
pressure
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CN1272501A (en
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孙传经
孙云鹏
孙明华
杨汝华
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孙传经
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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Abstract

The present invention relates to a supercritical CO2 method for extracting and purifying glycyrrhizic acid from liquoric roots (or coarse glycyrrhizic acid). The method has two steps that firstly, supercritical CO2 is used for removing non-polar oil impurities, extraction pressure is controlled at 25 (+/-)2MPa, and extraction temperature is 55 DEG C; secondly, the supercritical CO2 is added in a 95% of alcohol modifier, flow quantity ratio is controlled, the ratio of the alcohol to the CO2 is 5 to 10: 100, pressure is 22 (+/-)2MPa, temperature is 55 DEG C, the extraction yield of the glycyrrhizic acid is 4%, and the purity of the purified glycyrrhizic acid is 98.2%. The method has the advantages of simple and reliable flow path, circular CO2 and modifier use, high refined product purity, no residual solvent and no environmental pollution.

Description

Supercritical CO 2From Radix Glycyrrhizae, extract the method for Potenlini
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 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.The characteristics of this law are product 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 will 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 down CO at two series connection separator 3,4 step-down rear impurities 2Circulate through condenser 7 again; Second step after extraction 2-3 hour, was started properties-correcting agent pump 9 for extracting Potenlini, with the properties-correcting agent in the properties-correcting agent groove 8, was about to 95% ethanol and also squeezed into preheater 11 as properties-correcting agent, control CO 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 two placed in-line separators 5,6 of another group, Potenlini under the separated and collected.
Advantage of the present invention is, flow process is simple, reliable, and the Potenlini yield is 4%.
Following preferred embodiment 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.
Embodiment 1, is crushed to 40 purpose licorices after 3 kilograms are cleaned, dry and puts into 10 liters of extraction kettle 1 barrels, 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 2Logistics is emitted from separator top, and the bottom is nonpolar oily impurity, then, starts properties-correcting agent pump 9,95% ethanol modifiers in the properties-correcting agent groove 8 is extracted out, before preheater 11 and CO 2Stream mixes, and its throughput ratio is 5-10: 100, and pressure is 22 ± 2MPa, temperature is 55 ℃, extracted 3-4 hour, and contained the logistics heater via 2 of Potenlini, 55 ℃ of temperature enter another group series connection separator 5,6, after the step-down, Potenlini 0.12Kg under the separated and collected, yield is 4%, purity is 98%.
Embodiment 2, and raw material is 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.
Among Fig. 1,1 is charging basket in the extraction kettle, and 2 is well heater, and 3,4,5,6 is separator, and 7 is condenser, and 8 is the properties-correcting agent groove, and 9 is the properties-correcting agent pump, and 10 is high-pressure pump, and 11 is well heater.

Claims (1)

1, a kind of supercritical CO 2From Radix Glycyrrhizae, extract the method for Potenlini, it is characterized in that:
1) at first remove nonpolar oily impurity, will clean, dry and be 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 modifier in the properties-correcting agent groove (8) is extracted out, at the preceding and CO of preheater (11) 2Stream mixes, and controlling its throughput ratio is 5-10%, and extracting pressure is 22 ± 2MPa, and temperature is 55 ℃, and extraction back logistics is through well heater (2), and 55 ℃ of temperature enter another group two placed in-line separators (5,6) after the step-down, isolate Potenlini.
CNB001055992A 2000-04-03 2000-04-03 Supercritical CO2 extraction method for extracting glycyrrhizinic acid from licorice Expired - Fee Related CN1136225C (en)

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CNB001055992A CN1136225C (en) 2000-04-03 2000-04-03 Supercritical CO2 extraction method for extracting glycyrrhizinic acid from licorice

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CN1136225C true CN1136225C (en) 2004-01-28

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Cited By (1)

* Cited by examiner, † Cited by third party
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 (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
US8236360B2 (en) 2007-05-02 2012-08-07 Tom's Of Maine, Inc. Supercritical CO2 liquorice extract and products made there from
CN107376406B (en) * 2017-07-27 2020-05-12 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

Cited By (1)

* Cited by examiner, † Cited by third party
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

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