CN102648939A - Preparation method for geum aleppicum polyphenol - Google Patents
Preparation method for geum aleppicum polyphenol Download PDFInfo
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- CN102648939A CN102648939A CN201110045297XA CN201110045297A CN102648939A CN 102648939 A CN102648939 A CN 102648939A CN 201110045297X A CN201110045297X A CN 201110045297XA CN 201110045297 A CN201110045297 A CN 201110045297A CN 102648939 A CN102648939 A CN 102648939A
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- polyphenol
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- macroporous resin
- herba diclipterae
- diclipterae chinensis
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Abstract
The invention relates to a preparation method for geum aleppicum polyphenol, which specifically comprises the following steps of preparing materials, carrying out supercritical CO2 extraction, macroporous resin adsorption, condensing, drying and the like. In the technical steps of the preparation method disclosed by the invention, water and ethanol are selected as solvents, and therefore the environment pollution is small. Because the use amount of organic solvent is reduced, the environment can be effectively protected. The preparation method for the geum aleppicum polyphenol has the advantages of effective environment protection, good safety, high production efficiency, short period and good product quality and is suitable for large-scale industrial production. Because the supercritical extraction is adopted, the polyphenol is unlikely to oxidize and has stable property.
Description
Technical field:
The invention belongs to technical field of plant extraction, be specifically related to a kind of method for preparing of Herba Diclipterae Chinensis polyphenol.
Background technology:
Research shows; Plant polyphenol is a kind of good food antioxidant that has delaying human body caducity, eliminates activity in vivo free radical and antioxidation; Be described as " the 7th type of nutrient ", along with the extensive use of tea polyphenols and grape polyphenols, the application of polyphenolic substance becomes a big research focus.
Herba Diclipterae Chinensis is the dry Herb of Rosaceae perennial grass undergraduate course plant pubescence Herba Diclipterae Chinensis; Nature and flavor are bitter, hot cold; Have the tonify deficiency kidney tonifying, the effect of promoting blood circulation and detoxication can be used for diseases such as treatment is had a dizzy spell, myasthenia of limbs, seminal emission sexual impotence, exterior deficiency flu, cough haematemesis, asthenia cold abdominalgia, menoxenia, the swollen fracture of skin ulcer; Be used for mainly as Chinese herbal medicine at present clinical, to the active component of Herba Diclipterae Chinensis extract with the Study on Separation report seldom.
The Herba Diclipterae Chinensis polyphenol is the general name of contained polyphenols in the Herba Diclipterae Chinensis; It is the complicated mixture of the element of the first species; Have bioactive functions such as free radical, the oxidation of lipotropism matter, slow down aging, angiocardiopathy preventing, anti-cancer, radioprotective in the body of elimination, the content of polyphenol is 1.7293% in the employing determined by ultraviolet spectrophotometry Herba Diclipterae Chinensises such as Ou Yangyuzhu.
Traditional polyphenol preparation technology comprises: steps such as organic solvent extraction, membrance separation and column chromatography exist following deficiency: 1. contaminated environment, in the preparation process, use a large amount of toxic reagents, and big for environment pollution, dangerous; 2. be not suitable for producing on a large scale, existing technological operation is loaded down with trivial details, complicated, and the cycle is long, and product loss is big.
Summary of the invention:
The method for preparing that the purpose of this invention is to provide the Herba Diclipterae Chinensis polyphenol that a kind of environmental pollution is little, efficient is high, product quality is high.
The present invention realizes through following technical scheme:
A kind of method for preparing of Herba Diclipterae Chinensis polyphenol is characterized in that may further comprise the steps:
1) extracts: with the dry herb of Herba Diclipterae Chinensis, pulverize, put into extractor, supercritical CO
2The polyphenol extract is collected in extraction;
2) macroporous resin adsorption: above-mentioned polyphenol extract is added aqueous dispersion, and through macroporous resin column absorption, earlier with distilled water flush away impurity, the alcoholic solution eluting of reuse 60-80% is collected eluent;
3) concentrate drying: with above-mentioned eluent vacuum concentration, cold drying promptly gets the Herba Diclipterae Chinensis polyphenol.
Supercritical CO in the said step 1)
2Extraction conditions is: extracting pressure 15-28MPa, and extraction temperature 30-45 ℃, extraction time 1-3h resolves pressure 5-8MPa, and temperature 30-40 ℃, CO
2Flow velocity is 15-25L/h, the optional acetone of entrainer, methanol, alcoholic solution, and preferred alcohol solution, percent by volume is 65%, addition is the 10-20% of medical material amount.
Said step 2) one or more among the optional X-5 of macroporous resin, AB-8, H-103 and the H-1020 etc., the eluant consumption is 4-6BV, flow velocity is 0.4-0.6BV/h.
The invention has the advantages that:
(1) adopt supercritical extraction, efficient is high, extracts fully, and impurity is few, and the solvent use amount is few, and is pollution-free, the products obtained therefrom stable in properties, and quality is good.
(2) macroporous resin adsorption purification can effectively be removed plurality of impurities, good separating effect.
To combine the specific embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
The specific embodiment:
Embodiment 1:
With the dry herb of Herba Diclipterae Chinensis, pulverize, get 1kg, put into extractor, supercritical CO
2Extraction, extraction conditions is: extracting pressure 15MPa, 45 ℃ of extraction temperature, extraction time 1.5h resolves pressure 5MPa, 38 ℃ of temperature, CO
2Flow velocity is 18L/h, and entrainer is 65% alcoholic solution, and addition is 20% of a medical material amount, collects the polyphenol extract; Add aqueous dispersion, through the absorption of H-1020 macroporous resin column, earlier with 5BV distilled water flush away impurity; The alcoholic solution eluting of reuse 5BV70%, the control flow velocity is 0.5BV/h, collects eluent; Vacuum concentration, cold drying promptly get Herba Diclipterae Chinensis polyphenol 16.2g, and content is 96.0%.
Embodiment 2:
With the dry herb of Herba Diclipterae Chinensis, pulverize, get 1kg, put into extractor, supercritical CO
2Extraction, extraction conditions is: extracting pressure 28MPa, 30 ℃ of extraction temperature, extraction time 3h resolves pressure 8MPa, 35 ℃ of temperature, CO
2Flow velocity is 20L/h, the optional acetone of entrainer, methanol, alcoholic solution, and preferred alcohol solution, percent by volume is 65%; Addition is 10% of a medical material amount, collects the polyphenol extract, adds aqueous dispersion, adsorbs through the H-103 macroporous resin column; First with 4BV distilled water flush away impurity, the alcoholic solution eluting of reuse 4BV65%, the control flow velocity is 0.5BV/h, collects eluent; Vacuum concentration, cold drying promptly get Herba Diclipterae Chinensis polyphenol 13.7g, and content is 95.7%.
Embodiment 3
With the dry herb of Herba Diclipterae Chinensis, pulverize, get 1kg, put into extractor, supercritical CO
2Extraction, extraction conditions is: extracting pressure 18MPa, 35 ℃ of extraction temperature, extraction time 1h resolves pressure 6MPa, 35 ℃ of temperature, CO
2Flow velocity is 15L/h, the optional acetone of entrainer, methanol, alcoholic solution, and preferred alcohol solution, percent by volume is 65%; Addition is 15% of a medical material amount, collects the polyphenol extract, adds aqueous dispersion, adsorbs through the X-5 macroporous resin column; First with 6BV distilled water flush away impurity, the alcoholic solution eluting of reuse 5BV60%, the control flow velocity is 0.6BV/h, collects eluent; Vacuum concentration, cold drying promptly get Herba Diclipterae Chinensis polyphenol 15.9g, and content is 94.2%.
Embodiment 4
With the dry herb of Herba Diclipterae Chinensis, pulverize, get 1kg, put into extractor, supercritical CO
2Extraction, extraction conditions is: extracting pressure 20MPa, 40 ℃ of extraction temperature, extraction time 2h resolves pressure 6.5MPa, 40 ℃ of temperature, CO
2Flow velocity is 25L/h, the optional acetone of entrainer, methanol, alcoholic solution, and preferred alcohol solution, percent by volume is 65%; Addition is 18% of a medical material amount, collects the polyphenol extract, adds aqueous dispersion, adsorbs through the H-1020 macroporous resin column; First with 3BV distilled water flush away impurity, the alcoholic solution eluting of reuse 4BV70%, the control flow velocity is 0.4BV/h, collects eluent; Vacuum concentration, cold drying promptly get Herba Diclipterae Chinensis polyphenol 14.6g, and content is 97.1%.
Embodiment 5
With the dry herb of Herba Diclipterae Chinensis, pulverize, get 1kg, put into extractor, supercritical CO
2Extraction, extraction conditions is: extracting pressure 25MPa, 35 ℃ of extraction temperature, extraction time 1h resolves pressure 5MPa, 30 ℃ of temperature, CO
2Flow velocity is 15L/h, the optional acetone of entrainer, methanol, alcoholic solution, and preferred alcohol solution, percent by volume is 65%; Addition is 20% of a medical material amount, collects the polyphenol extract, adds aqueous dispersion, adsorbs through the AB-8 macroporous resin column; First with 3BV distilled water flush away impurity, the alcoholic solution eluting of reuse 6BV80%, the control flow velocity is 0.6BV/h, collects eluent; Vacuum concentration, cold drying promptly get Herba Diclipterae Chinensis polyphenol 16.6g, and content is 94.4%.
Claims (3)
1. the method for preparing of a Herba Diclipterae Chinensis polyphenol is characterized in that may further comprise the steps:
1) extracts: with the dry herb of Herba Diclipterae Chinensis, pulverize, put into extractor, supercritical CO
2The polyphenol extract is collected in extraction;
2) macroporous resin adsorption: above-mentioned polyphenol extract is added aqueous dispersion, and through macroporous resin column absorption, earlier with distilled water flush away impurity, the alcoholic solution eluting of reuse 60-80% is collected eluent;
3) concentrate drying: with above-mentioned eluent vacuum concentration, cold drying promptly gets the Herba Diclipterae Chinensis polyphenol.
2. the method for preparing described in claim 1 is characterized in that supercritical CO in the said step 1)
2Extraction conditions is: extracting pressure 15-28MPa, and extraction temperature 30-45 ℃, extraction time 1-3h resolves pressure 5-8MPa, and temperature 30-40 ℃, CO
2Flow velocity is 15-25L/h, the optional acetone of entrainer, methanol, alcoholic solution, and preferred alcohol solution, percent by volume is 65%, addition is the 10-20% of medical material amount.
3. the method for preparing described in claim 1 is characterized in that said step 2) among the optional X-5 of macroporous resin, AB-8, H-103 and the H-1020 etc. one or more, the eluant consumption is 4-6BV, flow velocity is 0.4-0.6BV/h.
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| CN201110045297XA CN102648939A (en) | 2011-02-25 | 2011-02-25 | Preparation method for geum aleppicum polyphenol |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105076488A (en) * | 2015-08-28 | 2015-11-25 | 成都市新津迎先粮油有限公司 | Antioxidative health care rapeseed oil |
| CN109966326A (en) * | 2019-04-17 | 2019-07-05 | 济南维瑞医药科技开发有限公司 | A kind of extracting method of indigo plant potted flower tannin |
| CN110368411A (en) * | 2019-08-02 | 2019-10-25 | 龙岩学院 | A kind of extraction process and its isolation and purification method of white back semiaquilegia adoxoides polyphenol |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101851223A (en) * | 2010-05-05 | 2010-10-06 | 浙江永达实业集团有限公司 | Method for extracting tea polyphenol from white tea by using supercritical CO2 fluid |
-
2011
- 2011-02-25 CN CN201110045297XA patent/CN102648939A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101851223A (en) * | 2010-05-05 | 2010-10-06 | 浙江永达实业集团有限公司 | Method for extracting tea polyphenol from white tea by using supercritical CO2 fluid |
Non-Patent Citations (2)
| Title |
|---|
| İ.HASBAY ADIL,ETC: "Subcritical (carbon dioxide+ethanol)extraction of polyphenols from apple and peach pomaces,and determination of the antioxidant activities of the extracts", 《THE JOUNAL OF SUPERCRITICAL FLUIDS》 * |
| 欧阳玉祝，等: "路边青中总多酚的提取与分离研究", 《食品科学》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105076488A (en) * | 2015-08-28 | 2015-11-25 | 成都市新津迎先粮油有限公司 | Antioxidative health care rapeseed oil |
| CN109966326A (en) * | 2019-04-17 | 2019-07-05 | 济南维瑞医药科技开发有限公司 | A kind of extracting method of indigo plant potted flower tannin |
| CN110368411A (en) * | 2019-08-02 | 2019-10-25 | 龙岩学院 | A kind of extraction process and its isolation and purification method of white back semiaquilegia adoxoides polyphenol |
| CN110368411B (en) * | 2019-08-02 | 2021-08-06 | 龙岩学院 | Extraction process and separation and purification method of gynura bicolor polyphenol |
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Application publication date: 20120829 |