CN1450063A - Process of supercritical carbon dioxide extracting licoflavone - Google Patents
Process of supercritical carbon dioxide extracting licoflavone Download PDFInfo
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- CN1450063A CN1450063A CN02109473A CN02109473A CN1450063A CN 1450063 A CN1450063 A CN 1450063A CN 02109473 A CN02109473 A CN 02109473A CN 02109473 A CN02109473 A CN 02109473A CN 1450063 A CN1450063 A CN 1450063A
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- carbon dioxide
- supercritical carbon
- licoflavone
- extraction
- radix glycyrrhizae
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- 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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Abstract
The method for extracting licoflavone by using supercritical Co2 extraction process mainly includes the following steps: drying licorice root, pulverizing, supercritical Co2 extraction, first reduced pressure separation, second reduced pressure separation to obtain licoflavone extract. Its extraction temp. is low, extraction speed is quick, extraction rate is high, it has no solvent residue and the licoflavone content in the product is high.
Description
Affiliated technical field:
The present invention relates to a kind of extracting process of licoflavone, particularly a kind of method of supercritical carbon dioxide extracting licoflavone.
Background technology:
At present, licoflavone mainly is with extracting the Radix Glycyrrhizae residue of conventional solvent-extraction process after extracting Potenlini, having long, shortcomings such as cost is high, yield is low, organic solvent residual of cycle.
Effective constituent supercritical carbon dioxide extraction research report is few in the Radix Glycyrrhizae, has (JP 2225491) such as Sun Chuanjing etc. (CN 1272501) and Fujimoto Yasuo to use supercritical carbon dioxide extraction method through the domestic and foreign literature retrieval and extracts two pieces of Potenlini patents; Shishikura Akihiro (Yukagaku, 1988; 37 (9): 731-5) use one piece in supercritical carbon dioxide extraction method extraction Radix Glycyrrhizae anti-inflammatory component document, one piece of patent with Goto Hiroki people such as (JP 1135723); Goto Hiroki is used for three pieces of food fresh keeping patents (JP 2113866, and JP 2113846, and JP 2113845) with Radix Glycyrrhizae supercritical carbon dioxide extraction thing; Xiang W. is used for one piece of smoking-cessation and health-care product patent (CN 1242999) with Radix Glycyrrhizae supercritical carbon dioxide extraction thing; Ling Y.C. etc. remove organochlorine pesticide document one piece of (Journal of chromatography, 1999 in the Radix Glycyrrhizae with the Radix Glycyrrhizae supercritical carbon dioxide extraction method; 835 (1-2): 145-157); The bibliographical information relevant with this patent only has two pieces: Li Guozhong, Li Nan, the supercritical carbon dioxide extraction Liquiritigenin of guarantor's space etc.(chemical engineering, 1994; 22 (5): 26-28); Manabe.A, Tokumori.T, supercritical carbon dioxide extraction Radix Glycyrrhizae pigment (Yakugaku Zasshi, 1987 of Sumida.Y etc.; 107 (7): 506-510), the scope of these two pieces report researchs is narrower, and the Radix Glycyrrhizae pigment and Liquiritigenin, isoliquiritigenin, licochalcone A, the B that only relate in the licoflavone extract, and do not relate to the extraction of Radix Glycyrrhizae total flavones.
Summary of the invention:
The object of the invention is to overcome above-mentioned weak point, and the method for the supercritical carbon dioxide extracting licoflavone that a kind of extraction temperature is low, speed is fast, percentage extraction is high, products obtained therefrom licoflavone content is high is provided.
To achieve these goals, the technical solution used in the present invention is: Radix Glycyrrhizae rhizome oven dry → pulverizing → supercritical carbon dioxide extraction → one-level decompression separation → second depressurized separation → licoflavone extraction liquid.
Advantage of the present invention is:
1. extraction temperature is low, speed is fast, percentage extraction is high.
2. no solvent residue.
3. the content about 30% of licoflavone.
4. human and environment is had no adverse effects
Embodiment:
Below embodiments of the invention are described in further detail:
The present invention is a kind of method of supercritical carbon dioxide extracting licoflavone, it is characterized in that: Radix Glycyrrhizae rhizome oven dry → pulverizing → supercritical carbon dioxide extraction → one-level decompression separation → second depressurized separation → licoflavone extracting solution.
Described Radix Glycyrrhizae rhizome bake out temperature is 50-80 ℃, and drying time is 4-6 hour.
Described Radix Glycyrrhizae rhizome oven dry back grinding particle size is the 60-80 order.
In the described extractor with Radix Glycyrrhizae rhizome powder input supercritical extraction unit, as solvent, 60-95% ethanol is done entrainment agent with supercritical co, is 20-35MPa at pressure, temperature is to extract under the 40-60 ℃ of condition, and the supercritical carbon dioxide extraction time is 3-6 hour.
The described one-level decompression separation pressure that carries out in separating tank is 5-10MPa, and temperature is 40-60 ℃; The second depressurized separating pressure is 5-7MPa, and temperature is 35-50 ℃.
Embodiment 1
Extracting liquorice rhizome 180g, being crushed to granularity is about 60 orders, and drop in the extraction kettle oven dry back, and extraction conditions is: extracting pressure is 25MPa, and temperature is 45 ℃; Separation condition is: flash trapping stage still pressure is 6MPa, and temperature is 45 ℃, and secondary separating still pressure is 5MPa, and temperature is 35 ℃; 75% ethanol is done entrainment agent.Behind the dynamic operation 3 hours.Obtain licoflavone extracting solution 645ml in flash trapping stage still and secondary separating still, percentage extraction is: 1.217%.
Embodiment 2
Extracting liquorice rhizome 180g, being crushed to granularity is 70 orders, and drop in the extraction kettle oven dry back, and extraction conditions is: extracting pressure is 30MPa, and temperature is 50 ℃; Separation condition is: one-level decompression separation still pressure is 7MPa, and temperature is 45 ℃, and second depressurized separating still pressure is 6MPa, and temperature is 40 ℃.85% ethanol is done entrainment agent.Behind the dynamic operation 5 hours.Obtain licoflavone extracting solution 720ml in one-level decompression separation still and second depressurized separating still, percentage extraction is:
1.499％。
Embodiment 3
Extracting liquorice rhizome 180g, being crushed to granularity is 80 orders, and drop in the extraction kettle oven dry back, and extraction conditions is: extracting pressure is 35MPa, and temperature is 55 ℃; Separation condition is: flash trapping stage still pressure is 8MPa, and temperature is 50 ℃, and secondary separating still pressure is 7MPa, and temperature is 45 ℃.95% ethanol is done entrainment agent.Behind the dynamic operation 6 hours.Obtain licoflavone extracting solution 670ml in one-level decompression separation still and second depressurized separating still, percentage extraction is: 1.264%.
Claims (5)
1, a kind of method of supercritical carbon dioxide extracting licoflavone is characterized in that: Radix Glycyrrhizae rhizome oven dry → pulverizing → supercritical carbon dioxide extraction → one-level decompression separation → second depressurized separation → licoflavone extracting solution.
2, according to the method for the described supercritical carbon dioxide extracting licoflavone of claim 1, it is characterized in that: Radix Glycyrrhizae rhizome bake out temperature is 50-80 ℃, and drying time is 4-6 hour.
3, according to the method for the described supercritical carbon dioxide extracting licoflavone of claim 1, it is characterized in that: Radix Glycyrrhizae rhizome oven dry back grinding particle size is the 60-80 order.
4, according to the method for the described supercritical carbon dioxide extracting licoflavone of claim 1, it is characterized in that: Radix Glycyrrhizae rhizome powder is dropped in the extractor of supercritical extraction unit, with supercritical co as solvent, 60-95% ethanol is done entrainment agent, at pressure is 20-35MPa, temperature is to extract under the 40-60 ℃ of condition, and the supercritical carbon dioxide extraction time is 3-6 hour.
5, according to the method for the described supercritical carbon dioxide extracting licoflavone of claim 1, it is characterized in that: carrying out one-level decompression separation pressure in separating tank is 5-10MPa, and temperature is 40-60 ℃; The second depressurized separating pressure is 5-7MPa, and temperature is 35-50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02109473XA CN1190430C (en) | 2002-04-10 | 2002-04-10 | Process of supercritical carbon dioxide extracting licoflavone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02109473XA CN1190430C (en) | 2002-04-10 | 2002-04-10 | Process of supercritical carbon dioxide extracting licoflavone |
Publications (2)
| Publication Number | Publication Date |
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| CN1450063A true CN1450063A (en) | 2003-10-22 |
| CN1190430C CN1190430C (en) | 2005-02-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB02109473XA Expired - Fee Related CN1190430C (en) | 2002-04-10 | 2002-04-10 | Process of supercritical carbon dioxide extracting licoflavone |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337042A (en) * | 2011-07-26 | 2012-02-01 | 江苏天晟药业有限公司 | Preparation method of liquorice pigment |
| CN105112149A (en) * | 2015-02-15 | 2015-12-02 | 李玉山 | Method for extracting and purifying licorice morin |
| CN107376406A (en) * | 2017-07-27 | 2017-11-24 | 源田生物科技有限公司 | A kind of preparation method of sweetener |
| CN108101923A (en) * | 2017-12-14 | 2018-06-01 | 中山大学 | A kind of process for separation and purification of glabridin monomer |
-
2002
- 2002-04-10 CN CNB02109473XA patent/CN1190430C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337042A (en) * | 2011-07-26 | 2012-02-01 | 江苏天晟药业有限公司 | Preparation method of liquorice pigment |
| CN105112149A (en) * | 2015-02-15 | 2015-12-02 | 李玉山 | Method for extracting and purifying licorice morin |
| CN107376406A (en) * | 2017-07-27 | 2017-11-24 | 源田生物科技有限公司 | A kind of preparation method of sweetener |
| CN108101923A (en) * | 2017-12-14 | 2018-06-01 | 中山大学 | A kind of process for separation and purification of glabridin monomer |
| CN108101923B (en) * | 2017-12-14 | 2020-07-31 | 中山大学 | Separation and purification method of glabridin monomer |
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| Publication number | Publication date |
|---|---|
| CN1190430C (en) | 2005-02-23 |
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