CN102504279B - Method for extracting gettama gum and chlorogenic acid simultaneously from folium cortex eucommiae - Google Patents
Method for extracting gettama gum and chlorogenic acid simultaneously from folium cortex eucommiae Download PDFInfo
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- CN102504279B CN102504279B CN 201110230444 CN201110230444A CN102504279B CN 102504279 B CN102504279 B CN 102504279B CN 201110230444 CN201110230444 CN 201110230444 CN 201110230444 A CN201110230444 A CN 201110230444A CN 102504279 B CN102504279 B CN 102504279B
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- chlorogenic acid
- solvent
- percha
- gutta
- folium eucommiae
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Abstract
The invention aims at extracting gettama gum and chlorogenic acid simultaneously from folium cortex eucommiae with high efficiency and low cost. The method is characterized in that non-polar solvent and weak-polar solvent, which are mutually insoluble, are used simultaneously to perform two-phase homogenate extraction from folium cortex eucommiae containing non-polar gettama gum and weak-polar chlorogenic acid on the condition of high-shear homogenate.
Description
Technical field
The present invention relates to field of plant extraction, particularly a kind of method of from Folium Eucommiae, extracting simultaneously gutta-percha and chlorogenic acid.
Background technology
The bark of eucommia (Eucommia ulmoides Oliver) is the distinctive famous and precious economic tree of China and the high-quality glue source seeds of development potentiality maximum in the world, abundant gutta-percha is all contained at the positions such as bark of eucommia pericarp, leaf, bark, be a kind of special natural macromolecular material, contain gutta-percha 2-5% in the Folium Eucommiae; Chlorogenic Acid in Eucommia ulmoides Oliv. Leaves content reaches 2.50-5.28%, chlorogenic acid has stronger biological activity multiple mushroom is had obvious inhibition or killing action, anticancer effect with pressing down cancer is arranged, chlorogenic acid or the acid antioxidant of a kind of effective new type natural, chlorogenic acid can improve condition of blood, and lowering blood glucose concentration reduces the free radical in the liver mitochondrion, no matter in vivo chlorogenic acid the still external effect that obvious Green Tea Extract is all arranged, and can be used for anti-aging skin care product production.
Therefore from Folium Eucommiae, extract gutta-percha simultaneously and chlorogenic acid has Practical significance.
Propose first fermentation 03117678.X patent of invention " utilizes Folium Eucommiae to produce continuously the production method of eucommia ulmoides extract powder, gutta-percha, bark of eucommia resin and fertilizer ", with three cover flat-turn leachers, added respectively sherwood oil, acetone, moisture level extracting method again.
99114969.6 patent of invention " with the method for supercritical co extracting effective components from Folium Eucommiae " proposes and can by control pressure and temperature, targetedly the effective constituent in the Folium Eucommiae fully be extracted.
92114760.0 patent of invention " a kind of method of extracting gutta-percha " is to adopt grinding method that the non-glue component that contains in leaf surface is ground, and makes to contain glue tissue in the leaf and come out, and reaches the purpose that contains the glue enrichment, then sieves and removes waste residue, uses the organic solvent extraction gutta-percha.
90101268.8 patent of invention " comprehensive extraction of gutta-percha " namely keeps prior fermentation, boiling, the flushing of cancellation machinery; Later stage is carried out the method for the thick glue of solvent extraction and purification.
98112220.5 " extracting the processing method of the thick glue of rubber " from the bark of eucommia, patent of invention it is characterized in that take toluene as solvent, single still in service through extract first and subsequent twice cleaning after carry out again second time and extract and subsequent twice cleaning, carry out then that many stills are operating to be extracted and subsequent twice cleaning and for the second time extraction and subsequent twice cleaning first.
Summary of the invention
The present invention seeks to high-efficiency and low-cost ground and from Folium Eucommiae, extract simultaneously gutta-percha and chlorogenic acid, it is characterized in that utilizing immiscible non-polar solvent and the weak polar solvent while under the high-shear homogenate condition, the Folium Eucommiae that contains nonpolar gutta-percha and low-pole chlorogenic acid is carried out two-phase homogenate extraction; The homogenate extraction refers to that biological tissue carries out tissue homogenate or defibrination by adding extraction solvent, to extract a kind of extracting method of effective constituent in the biological tissue; Two immiscible liquid phases are constantly extracting in whole homogenate extraction process--the process of reextraction, according to " similar mixing " principle, wherein the material chlorogenic acid of low-pole can enter the solvent phase of low-pole, nonpolar material gutta-percha can enter nonpolar organic solvent phase, realizes that finally chlorogenic acid separates with gutta-percha; Because weak polar solvent, has also reduced the resistance that gutta-percha leaches to the swelling action of Folium Eucommiae, has improved extracting efficiency.
Production method of the present invention comprises the steps:
1. mill: with the Folium Eucommiae of drying with the pulverizing of milling of the disc type grinding machine of known configurations;
2. soak: oneself is milled pulverize Folium Eucommiae and add and accounted for 1.5-3 times of concentration 80-90% of Folium Eucommiae gross weight alcohol immersion 1-3 hour;
3. high-shear homogenate: with oneself soak Folium Eucommiae together with alcohol immersion liquid with account for former dried Folium Eucommiae gross weight 2-4 doubly after No. 6 solvent, send into homogenate in the high-shear homogenate machine of known configurations,
" No. 6 solvents " is edible oil industry universal extraction solvent, and the high-shear homogenate machine is called again the high-shear homogenizer;
4. leave standstill phase-splitting: the mixture that homogenate is contained well Folium Eucommiae composition, ethanol, No. 6 solvents injects known configurations and leaves standstill phase separation tank and leave standstill phase-splitting, according to " similar mixing " principle, wherein the material chlorogenic acid of low-pole can enter in the alcohol solvent of low-pole, nonpolar material gutta-percha can enter in nonpolar No. 6 solvents, ethanol and No. 6 solvents are immiscible, realize that finally chlorogenic acid separates with gutta-percha;
5.1. nonpolar phase Separation and Recovery solvent: take out gutta-percha and No. 6 solvent mixtures from leave standstill phase separation tank, adopt oneself general known equipment and technology of edible oil industry to separate gutta-percha and No. 6 solvents, No. 6 solvent can be recycled;
The recovery solvent 5.2. low-pole is separated: take out chlorogenic acid and alcohol mixture from leave standstill phase separation tank, adopt the own general known equipment and technology separating chlorogenic acid of plant extract industry and ethanol, ethanol can be recycled;
5.3. precipitation slurry dried recovered solvent: from leave standstill phase separation tank, take out at last the precipitation slurry, in the vacuum scraper drying machine, slough liquid phase, liquid phase is that moisture content ethanol adopts the own general known equipment and technology of plant extract industry, remove moisture, ethanol can be recycled behind the purifying, solid phase obtains thing because also contain chlorogenic acid etc., can be used as animal feedstuff additive.
Description of drawings
Figure one is process flow diagram
Embodiment 1
A kind of method of extracting simultaneously gutta-percha and chlorogenic acid from Folium Eucommiae comprises the steps:
1. mill: 1 ton of water ratio is lower than 10% Folium Eucommiae and mills with the disc type grinding machine of known configurations and be crushed to the 10-20 order;
2. soak: will be above-mentioned oneself mill and pulverized Folium Eucommiae adding 1.5-3 ton concentration 80-90% alcohol immersion 1-3 hour;
3. high-shear homogenate: with above-mentioned oneself soak Folium Eucommiae together with alcohol immersion liquid and No. 6 solvent of 2-4 ton after, send into homogenate in the high-shear homogenate machine of known configurations,
" No. 6 solvents " is edible oil industry universal extraction solvent, and the high-shear homogenate machine is called again the high-shear homogenizer;
4. leave standstill phase-splitting: the mixture that above-mentioned homogenate is contained well Folium Eucommiae composition, ethanol, No. 6 solvents injects known configurations and leaves standstill phase separation tank and leave standstill phase-splitting, according to " similar mixing " principle, wherein the material chlorogenic acid of low-pole can enter in the alcohol solvent of low-pole, nonpolar material gutta-percha can enter nonpolar No. 6 solvents, ethanol and No. 6 solvents are immiscible, realize that finally chlorogenic acid separates with gutta-percha;
5.1. nonpolar phase Separation and Recovery solvent: take out gutta-percha and No. 6 solvent mixtures from leave standstill phase separation tank, adopt oneself general known equipment and technology of edible oil industry to separate gutta-percha and No. 6 solvents, No. 6 solvent can be recycled;
Isolate the thick glue of the bark of eucommia and be refined into qualified gutta-percha commodity through known equipment and technology;
The recovery solvent 5.2. low-pole is separated: take out chlorogenic acid and alcohol mixture from leave standstill phase separation tank, adopt the own general known equipment and technology separating chlorogenic acid of plant extract industry and ethanol, ethanol can be recycled;
Isolate the chlorogenic acid crude product and be refined into qualified chlorogenic acid commodity through known equipment and technology;
5.3. precipitation slurry dried recovered solvent: from leave standstill phase separation tank, take out at last the precipitation slurry, in the vacuum scraper drying machine, slough liquid phase, liquid phase is the ethanol of moisture content, adopt the own general known equipment and technology of plant extract industry, remove moisture, ethanol can be recycled behind the purifying, and solid phase obtains thing because also contain chlorogenic acid, can be used as animal feedstuff additive.
Claims (1)
1. method of from Folium Eucommiae, extracting simultaneously gutta-percha and chlorogenic acid, it is characterized in that utilizing immiscible non-polar solvent and the weak polar solvent while under the high-shear homogenate condition, the Folium Eucommiae that contains nonpolar gutta-percha and low-pole chlorogenic acid is carried out two-phase homogenate extraction; Comprise the steps:
1.1. mill: with the Folium Eucommiae of drying with the pulverizing of milling of the disc type grinding machine of known configurations;
1.2. soak: the pulverizing Folium Eucommiae adding of will milling accounted for 1.5-3 times of concentration 80-90% of Folium Eucommiae gross weight alcohol immersion 1-3 hour;
1.3. high-shear homogenate: will soak Folium Eucommiae together with alcohol immersion liquid with account for former dried Folium Eucommiae gross weight 2-4 doubly after No. 6 solvent, send into homogenate in the high-shear homogenate machine of known configurations,
" No. 6 solvents " is edible oil industry universal extraction solvent, and the high-shear homogenate machine is called again the high-shear homogenizer;
1.4. leave standstill phase-splitting: the mixture that homogenate is contained well Folium Eucommiae composition, ethanol, No. 6 solvents injects known configurations and leaves standstill phase separation tank and leave standstill phase-splitting, according to " similar mixing " principle, wherein the material chlorogenic acid of low-pole can enter in the alcohol solvent of low-pole, nonpolar material gutta-percha can enter in nonpolar No. 6 solvents, ethanol and No. 6 solvents are immiscible, realize that finally chlorogenic acid separates with gutta-percha;
1.5.1. nonpolar phase Separation and Recovery solvent: take out gutta-percha and No. 6 solvent mixtures from leave standstill phase separation tank, adopt the general known equipment and technology of edible oil industry to separate gutta-percha and No. 6 solvents, No. 6 solvent can be recycled;
The recovery solvent 1.5.2. low-pole is separated: take out chlorogenic acid and alcohol mixture from leave standstill phase separation tank, adopt the general known equipment and technology separating chlorogenic acid of plant extract industry and ethanol, ethanol can be recycled;
1.5.3. precipitation slurry dried recovered solvent: from leave standstill phase separation tank, take out at last the precipitation slurry, in the vacuum scraper drying machine, slough liquid phase, liquid phase is the ethanol of moisture content, adopt the general known equipment and technology of plant extract industry, remove moisture, ethanol can be recycled behind the purifying, and solid phase obtains thing because also contain chlorogenic acid, can be used as animal feedstuff additive.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110230444 CN102504279B (en) | 2011-08-09 | 2011-08-09 | Method for extracting gettama gum and chlorogenic acid simultaneously from folium cortex eucommiae |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110230444 CN102504279B (en) | 2011-08-09 | 2011-08-09 | Method for extracting gettama gum and chlorogenic acid simultaneously from folium cortex eucommiae |
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| Publication Number | Publication Date |
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| CN102504279A CN102504279A (en) | 2012-06-20 |
| CN102504279B true CN102504279B (en) | 2013-04-24 |
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| CN 201110230444 Expired - Fee Related CN102504279B (en) | 2011-08-09 | 2011-08-09 | Method for extracting gettama gum and chlorogenic acid simultaneously from folium cortex eucommiae |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2014114283A (en) * | 2012-11-19 | 2014-06-26 | Fujifilm Corp | Method for producing polyphenol |
| CN106674540A (en) * | 2015-11-05 | 2017-05-17 | 柴守环 | Preparation method of Eucommia ulmoides gum |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1241560A (en) * | 1999-06-25 | 2000-01-19 | 遵义古特杜仲开发有限公司 | Method of extracting the effective components from gettama leaf by using supercritical carbon dioxide |
| CN1273964A (en) * | 1999-05-18 | 2000-11-22 | 孙波 | Process for preparing chlorogenic acid from eucommia leaves |
| CN1360903A (en) * | 2000-12-27 | 2002-07-31 | 中国科学院化学研究所 | Effective component extracting method from gettama leaf, bark or seed as material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09263787A (en) * | 1996-01-26 | 1997-10-07 | Nof Corp | Production of highly unsaturated fatty acid or alkyl ester thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273964A (en) * | 1999-05-18 | 2000-11-22 | 孙波 | Process for preparing chlorogenic acid from eucommia leaves |
| CN1241560A (en) * | 1999-06-25 | 2000-01-19 | 遵义古特杜仲开发有限公司 | Method of extracting the effective components from gettama leaf by using supercritical carbon dioxide |
| CN1360903A (en) * | 2000-12-27 | 2002-07-31 | 中国科学院化学研究所 | Effective component extracting method from gettama leaf, bark or seed as material |
Non-Patent Citations (1)
| Title |
|---|
| JP特开平9-263787A 1997.10.07 |
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Effective date of registration: 20151112 Address after: 200062, room 36, No. 28, Lane 616, Danba Road, Shanghai, Putuo District Patentee after: Shanghai crown Biotechnology Co., Ltd. Address before: 350012, Red Bridge No. 35, new town, Fuzhou, Fujian Patentee before: Liu Yuerong Patentee before: Zheng Jiancan Patentee before: Hou Mengbin |
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