CN101444557B - Method for producing general flavone of medicinal mulberry by supercritical carbon dioxide extraction - Google Patents
Method for producing general flavone of medicinal mulberry by supercritical carbon dioxide extraction Download PDFInfo
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- CN101444557B CN101444557B CN2008103066344A CN200810306634A CN101444557B CN 101444557 B CN101444557 B CN 101444557B CN 2008103066344 A CN2008103066344 A CN 2008103066344A CN 200810306634 A CN200810306634 A CN 200810306634A CN 101444557 B CN101444557 B CN 101444557B
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- carbon dioxide
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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 invention relates to the technical field of medicinal mulberry extraction, in particular to a method for producing general flavone of medicinal mulberry by supercritical carbon dioxide extraction. The method comprises the following steps: pulverizing dried medicinal mulberry to granules with a particle size in the range from 10 meshes to 30 meshes by using a pulverizer with good leak tightness, loading the pulverized granules to an extraction tank, placing the extraction tank inside an extraction kettle, sealing the extraction kettle, introducing carbon dioxide in supercritical state to allow extraction, and collecting pale-yellow solid extracts. The production method is easy to operate and repeat, and doesn't need any other organic solvents except carbon dioxide and anhydrous alcohol. The carbon dioxide is colorless, tasteless, innoxious, non-flammable and inert to chemicals and has no environmental pollution; and the anhydrous alcohol evaporates spontaneously in the after-treatment without any residues or toxicity, so that the flavonoid extract has high purity, low impurity content, no heavy metal residue and no toxicity to human body. The method for extracting flavonoid components from medicinal mulberry doesn't cause environmental pollution.
Description
Technical field
The present invention relates to the extracting method technical field of medicine mulberry fruit, is a kind of employing supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry.
Background technology
Medicine mulberry fruit (Morusnigra Linn., the medicine mulberry) on plant taxonomy, belongs to Moraceae, Morus plant, be Aksu, Xinjiang and field and Kaxgar Prefecture and the ancient fruit resource of Ba Zhou and gram state, being the medicinal material among the people of nutritive food resource, Chinese medicine and the Uygur nationality of preciousness, is unique special rare your resource in Xinjiang.
The medicine mulberry fruit have anti-cancer antimutagenic, strengthening immunity, guarantor's kidney protect liver, preserve youthful looks anti-ageing, promote hematopoietic cell growth and lowering blood glucose blood fat.The nutritive ingredient of medicine mulberry fruit is very abundant, and especially content of flavonoids is higher, and a large amount of studies show that, the effect of preventing and curing diseases of medicine mulberry fruit is with wherein to contain abundant flavonoid activeconstituents closely related.
Heavy metal is one of important pollutent of Chinese medicine, and the content of heavy metal height has become an important indicator weighing the Chinese medicinal materials quality good or not in the Chinese medicinal materials, and toxic heavy metal element is often referred to lead (Pb) in the Chinese medicine, cadmium (Cd), mercury (Hg), arsenic (As), copper (Cu), chromium (Cr) etc.In recent years, very pay close attention to the content problem of heavy metal element in the Chinese medicine in the world, import Chinese medicine is all had clearly regulation.Therefore, go abroad, participate in the competition of international medical market, reason that the heavy metal element in the tcm product is exceeded standard and research how to control heavy metal content are imperative.
We find in the work in early stage, and the pharmaceutical use research to the medicine mulberry fruit at present all lays particular emphasis on the clinical application aspect, still traditional solvent-extraction process on the flavonoid extraction of active ingredients, and its flavonoid active component content is low, and heavy metal content is more.
Summary of the invention
The invention provides a kind of employing supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry, it has solved effectively and has adopted prior art to extract the back problem that active component content is low, heavy metal content is more.
Technical scheme of the present invention realizes by following measure: a kind of employing supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry, it carries out as follows: it is to pack into behind 10 order to the 30 purpose particles in the extraction batch can that exsiccant medicine mulberry fruit is pulverized with the pulverizer of good leak tightness, to extract batch can and place extraction kettle, the sealing extraction kettle, feeding is in supercritical carbon dioxide and extracts, and use dehydrated alcohol to participate in extraction as entrainment agent, extraction plant processing condition scope: pressure is 25 to 35 megapascal (MPa)s, temperature is 35 degrees centigrade to 45 degrees centigrade, carbon dioxide flow is for per hour 10 rising to 20 liters, the extraction time is 1.5 hours to 3 hours, wherein, per 300 gram medicine mulberry fruits to need entrainment agent dehydrated alcohol consumption be 100 to 300 milliliters; Can obtain the light yellow solid extract.
Be further optimization or improvement below to the foregoing invention technical scheme:
Above-mentioned extraction pressure is 30 megapascal (MPa)s.
Above-mentioned extraction temperature is 40 degrees centigrade.
Above-mentioned carbon dioxide flow is per hour 15 liters.
Above-mentioned entrainment agent dehydrated alcohol consumption is 200 milliliters.
The present invention is convenient to operation and is repeated, owing to do not use any organic solvent, carbonic acid gas and dehydrated alcohol have only been used, colourless, tasteless, nontoxic, nonflammable, the unreactiveness, pollution-free of carbonic acid gas wherein, dehydrated alcohol can volatilize naturally by aftertreatment, also without any residual and toxicity, therefore flavonoid composition purity height, the impurity that is extracted is few, do not have any heavy-metal residual, to the human body nontoxicity, from the medicine mulberry fruit, extract the flavonoid composition with the present invention and also can not pollute environment.
Embodiment
The present invention is not subjected to the restriction of following embodiment, can determine concrete embodiment according to technical scheme of the present invention and practical situation.
The present invention adopts supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry to carry out as follows: it is to pack into behind 10 order to the 30 purpose particles to extract in the batch can that exsiccant medicine mulberry fruit is pulverized with the pulverizer of good leak tightness, to extract batch can and place extraction kettle, the sealing extraction kettle, feeding is in supercritical carbon dioxide and extracts, and use dehydrated alcohol to participate in extraction as entrainment agent, extraction plant processing condition scope: pressure is 25 to 35 megapascal (MPa)s, temperature is 35 degrees centigrade to 45 degrees centigrade, carbon dioxide flow is for per hour 10 rising to 20 liters, the extraction time is 1.5 hours to 3 hours, wherein, per 300 gram medicine mulberry fruits to need entrainment agent dehydrated alcohol consumption be 100 to 300 milliliters; Can obtain the light yellow solid extract.
For the ease of measuring concrete effect of the present invention, take by weighing medicine mulberry fruit 300 grams and do following experiment by the present invention, wherein, extraction pressure, extraction temperature, carbon dioxide flow, entrainment agent consumption be by selecting in the described scope of following table 1, and concrete experiment is as table 2 (factor A, B in the table 2, C, D selected 1 to 3 be sequence number 1 to 3 pairing factor A, B, C, D in the table 1).
Table 1
Table 2
After extracting with the present invention, each tests extracted amount and medicine Phellinus ketone amount thereof, data after testing and calculation result such as table 3.
Table 3
| The experiment number | Extract must be measured (g) | Total flavones must be measured (g) | General flavone content (%) |
| 1 | ?2.71 | ?0.199 | 7.34 |
| 2 | ?4.29 | ?0.204 | 4.76 |
| 3 | ?4.15 | ?0.215 | 5.18 |
| 4 | ?4.32 | ?0.303 | 7.01 |
| 5 | ?2.35 | ?0.197 | 8.38 |
| 6 | ?6.25 | ?0.480 | 7.68 |
| 7 | ?5.63 | ?0.456 | 8.10 |
| 8 | ?4.10 | ?0.351 | 8.56 |
| 9 | ?3.25 | ?0.284 | 8.74 |
The present invention as known from Table 3 extracts the flavones in the medicine mulberry, and its content can reach 4.76% to 8.74%.
Carry out the comparison and detection of heavy metal below:
(1) carry out the detection of heavy metal to adopting traditional solvent to extract medicine mulberry fruit gained sample:
Accurately take by weighing dry sample 0.2 gram (accurately to 0.0001 gram) for preparing and put into tetrafluoroethylene counteracting tank bottom, add 3 milliliters of nitric acid and 3 milliliters of hydrogen peroxide, in microwave digestion system, cleared up altogether 12 minutes, after waiting to clear up fully, transfer in 25 milliliters of volumetric flasks, be settled to scale with triple distillation water, analyze for inductively coupled plasma atomic emission spectrometry (ICP-AES).
(2) above-mentioned experiment 1 to 9 gained sample is carried out the detection of following heavy metal:
Accurately take by weighing experiment 1 to 9 sample for preparing 0.2 gram (accurately to 0.0001 gram) and put into tetrafluoroethylene counteracting tank bottom, add 3 milliliters of nitric acid and 3 milliliters of hydrogen peroxide, in microwave digestion system, cleared up altogether 12 minutes, after waiting to clear up fully, transfer in 25 milliliters of volumetric flasks, be settled to scale with triple distillation water, analyze for ICP-AES.
By analysis, the content of heavy metal is average as table 4 in the flavones sample of above-mentioned two kinds of method gained.
Table 4
| The heavy metal kind | Content/μ gg in the flavones sample that solvent method extracts -1 | Content in the flavones sample of supercritical fluid extraction/μ gg -1 |
| As | 0.25 | 0.00 |
| Pb | 1.7 | 0.00 |
| Cd | 0.15 | 0.00 |
| Cu | 32 | 0.00 |
| Fe | 276 | 0.00 |
| Cr | 2.5 | 0.00 |
In sum, advantage of the present invention is as follows:
Can find out from above experimental result that (1) adopt the present invention to extract medicine mulberry fruit flavones, the flavones content in its extract is 4.76% to 8.74%, and when adopting traditional solvent to extract medicine mulberry fruit flavones, the flavones content in its extract only is 0.115%. As seen, flavones purity of the present invention improves greatly, and the highest is 76 times of traditional extraction process.
When (2) adopting the present invention to extract medicine mulberry fruit flavones, do not use any organic solvent, carbon dioxide and absolute ethyl alcohol have only been used, colourless, tasteless, nontoxic, nonflammable, the chemical inertness, pollution-free of carbon dioxide wherein, absolute ethyl alcohol can volatilize naturally by post processing, also without any residual and toxicity. And in the conventional solvent extraction method, can use the organic solvents such as bulk petroleum ether, ethyl acetate, n-butanol, and can't all eliminate, will remain in the sample, human body, environment are worked the mischief and toxicity. Therefore, supercritical extraction extraction medicine mulberry fruit flavones is harmless, free of contamination industry.
(3) no any heavy-metal residual in the flavones sample of employing the present invention extraction, the product of producing also is " green product ", is much better than conventional method.
Claims (9)
1. one kind is adopted supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry, it is characterized in that carrying out as follows: it is to pack into behind 10 order to the 30 purpose particles in the extraction batch can that exsiccant medicine mulberry fruit is pulverized with the pulverizer of good leak tightness, to extract batch can and place extraction kettle, the sealing extraction kettle, feeding is in supercritical carbon dioxide and extracts, and use dehydrated alcohol to participate in extraction as entrainment agent, extraction plant processing condition scope: pressure is 25 to 35 megapascal (MPa)s, temperature is 35 degrees centigrade to 45 degrees centigrade, carbon dioxide flow is for per hour 10 rising to 20 liters, the extraction time is 1.5 hours to 3 hours, wherein, per 300 gram medicine mulberry fruits to need entrainment agent dehydrated alcohol consumption be 100 to 300 milliliters; Can obtain the light yellow solid extract.
2. employing supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry according to claim 1, it is characterized in that extracting pressure is 35 megapascal (MPa)s.
3. employing supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry according to claim 1 and 2 is characterized in that extraction temperature is 45 degrees centigrade.
4. employing supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry according to claim 1 and 2 is characterized in that carbon dioxide flow is per hour 15 liters.
5. employing supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry according to claim 3 is characterized in that carbon dioxide flow is per hour 15 liters.
6. employing supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry according to claim 1 and 2 is characterized in that entrainment agent dehydrated alcohol consumption is 100 milliliters.
7. employing supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry according to claim 3 is characterized in that entrainment agent dehydrated alcohol consumption is 100 milliliters.
8. employing supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry according to claim 4 is characterized in that entrainment agent dehydrated alcohol consumption is 100 milliliters.
9. employing supercritical carbon dioxide process extraction method for producing general flavone of medicinal mulberry according to claim 5 is characterized in that entrainment agent dehydrated alcohol consumption is 100 milliliters.
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| CN101905090B (en) * | 2010-05-31 | 2012-08-15 | 中国农业大学 | Method for extracting polar or medium polar plant source natural product |
| CN112694435A (en) * | 2020-04-13 | 2021-04-23 | 中南林业科技大学 | Method for extracting gynura procumbens alkaloid with high antibacterial activity |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1951931A (en) * | 2006-11-15 | 2007-04-25 | 江苏瑞迪生科技有限公司 | Method for supercritical CO2 extraction of falconoid from northern aweto |
| CN1966499A (en) * | 2005-11-18 | 2007-05-23 | 重庆锦程实业有限公司 | Hypercritical fluid extraction method for olive flavone |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1966499A (en) * | 2005-11-18 | 2007-05-23 | 重庆锦程实业有限公司 | Hypercritical fluid extraction method for olive flavone |
| CN1951931A (en) * | 2006-11-15 | 2007-04-25 | 江苏瑞迪生科技有限公司 | Method for supercritical CO2 extraction of falconoid from northern aweto |
Non-Patent Citations (2)
| Title |
|---|
| 张志伟等.超临界CO2流体萃取桑椹籽油的研究.《中国油脂》.2007,第32卷(第1期),77-80. * |
| 李国章等.桑椹籽中黄酮的CO2超临界流体萃取及抑菌作用研究.《现代食品科技》.2006,第22卷(第2期),86-88. * |
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Application publication date: 20090603 Assignee: Urumqi Zhixin Kang Biotechnology Co. Ltd. Assignor: Xinjiang Medicine University Contract record no.: 2013650000025 Denomination of invention: Method for producing general flavone of medicinal mulberry by supercritical carbon dioxide extraction Granted publication date: 20110810 License type: Exclusive License Record date: 20130619 |
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