CN102935091A - Propolis flavonoid extracting method - Google Patents
Propolis flavonoid extracting method Download PDFInfo
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- CN102935091A CN102935091A CN2012104668376A CN201210466837A CN102935091A CN 102935091 A CN102935091 A CN 102935091A CN 2012104668376 A CN2012104668376 A CN 2012104668376A CN 201210466837 A CN201210466837 A CN 201210466837A CN 102935091 A CN102935091 A CN 102935091A
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Abstract
The invention provides a propolis flavonoid extracting method which is characterized by including steps of (1), mixing propolis with ethanol solution, soaking at the temperature of 70-85 DEG C for 16-24 hours; (2), refluxing and extracting the solution to obtain leaching liquid; (3) concentrating the leaching liquid to recover ethanol; (4) cooling and centrifuging condensed liquid without ethanol; and (5), extracting supernatant obtained by centrifuging twice by chloroform to obtain water phase, extracting the water phase twice by ehyl acetate, evaporating off the ehyl acetate from the ehyl acetate extract through a rotary evaporator so as to obtain flavonoid compounds. By the method, flavonoid effective components are complete, damage to active components is reduced, ethanol can be recovered easily, the process is simple, and time and energy consumption is low; further, the method is quite suitable for industrial production; and the prepared high-purity propolis flavonoid has high application value in medical healthcare, and has unique special function in cancer resistance.
Description
Technical field
The invention belongs to chemical compound and extract the field, relate in particular to a kind of extracting method of propolis flavone.
Background technology
The propolis natural gum that to be Mel gather from the newborn twig of plant or bark, the mixed fragrant colloid that processes with self secretion.Ten thousand Apiss of 4-5, one is only the propolis that can adopt about 40g-60g, is described as " purple gold ".The propolis emperor is the superfine product in the propolis, and its general flavone content is up to more than the 9300mg, and all the other composition gold proportionings, synergism.Scientists gives the propolis emperor many laudatory titles: blood vessel street cleaner, blood glucose patron saint, anticancer warrier, natural immunity reinforcing agent.
Existing technological means can be isolated more than 20 kind of chromocor compound from propolis, it is that main active substances in the propolis accounts for 4.13% of propolis.These chromocor compounds comprise flavonoid, flavonols and Flavanones etc.Have chrysin, tectochrysin, acacetin, apigenin, the willow that belong to flavonoid are worn Qian Su etc.; What belong to flavonols has alpinin, galangin, rhamnetin, isorhamnetin, rhamnocitrin, kaempferide, Yue Hua element, Quercetin and a derivant thereof etc., and what belong to Flavanones has pinocembrin, Strobilus Pini element, sakuranetin, isosakuranetin, a naringenin etc.Found first that from propolis occurring in nature only has the unique effective ingredient that just has in the propolis, 5,7-dihydroxy-3`, 4`-dimethyl flavone and 5-hydroxyl-4`, the 7-dimethoxy is two
The hydrogen flavone.
At present, the main method of extraction flavone compound is macroreticular resin absorbing method from propolis.Macroreticular resin absorbing method utilizes organic high molecular polymer to be adsorbent, the impact that its materialization stability is high, adsorptive selectivity good, not existed by inorganic matter, cost saving, be widely used in the separation and purification of material, but in the discovered in recent years macroporous resin separate substance resin residue is arranged, and difficult the removal seriously limited its application.
Summary of the invention
The invention provides a kind of extracting method of propolis flavone, be intended to solve the incomplete problem of flavone effective ingredient that prior art is extracted.
The embodiment of the invention provides a kind of extracting method of propolis flavone, and described method comprises the steps:
(1) the propolis powder is that the 80-90% alcoholic solution mixes with concentration, soaks 16-24 hour under 70-85 ℃ temperature;
(2) the solution reflux, extract, obtains lixiviating solution;
(3) lixiviating solution is concentrated, Recycled ethanol;
(4) concentrated solution behind the removal ethanol is cooled to 5-10 ℃, centrifugal 20-30 minute;
(5) supernatant after centrifugal is with chloroform extraction 2 times, and the water that obtains is used ethyl acetate extraction 2 times again, and the acetic acid ethyl acetate extract that obtains after the extraction steams ethyl acetate, obtains flavone compound through Rotary Evaporators.
The color of the propolis flavone extracting solution that the embodiment of the invention obtains is yellowish-brown or brown, and special fragrance is arranged, and taste is puckery.Complete with the flavone effective ingredient that this kind method is extracted, the destruction that can reduce active component, and ethanol easily reclaims, technique is simple, few during consumption energy consumption, is very suitable for suitability for industrialized production.And resulting high-purity propolis flavone has very high using value aspect health care, and especially at anticancer aspect, its special effect is rare especially.
The specific embodiment
Example one
Propolis powder 100g is that 85% alcoholic solution mixes by solid-to-liquid ratio at 1: 15 with concentration, soaks 20 hours under 80 ℃ temperature; The solution reflux, extract, is extracted 3 times, and each 1 hour, merge extractive liquid, afterwards; The extracting solution concentrating under reduced pressure, Recycled ethanol; Concentrated solution behind the removal ethanol is cooled to 5 ℃, centrifugal 20 minutes; Chloroform extraction 2 times of supernatant after centrifugal, the water that obtains is used ethyl acetate extraction 2 times again, and the acetic acid ethyl acetate extract that obtains after the extraction steams ethyl acetate, obtains flavone compound 4.08g through Rotary Evaporators.
Example two
Propolis powder 100g is that 90% alcoholic solution mixes by solid-to-liquid ratio at 1: 20 with concentration, soaks 18 hours under 80 ℃ temperature; The solution reflux, extract, is extracted 3 times, and each 1 hour, merge extractive liquid, afterwards; The extracting solution concentrating under reduced pressure, Recycled ethanol; Concentrated solution behind the removal ethanol is cooled to 8 ℃, centrifugal 30 minutes; Chloroform extraction 2 times of supernatant after centrifugal, the water that obtains is used ethyl acetate extraction 2 times again, and the acetic acid ethyl acetate extract that obtains after the extraction steams ethyl acetate, obtains flavone compound 4.03g through Rotary Evaporators.
Example three
Propolis powder 100g is that 80% alcoholic solution mixes by solid-to-liquid ratio at 1: 20 with concentration, soaks 24 hours under 80 ℃ temperature; The solution reflux, extract, is extracted 3 times, and each 1 hour, merge extractive liquid, afterwards; The extracting solution concentrating under reduced pressure, Recycled ethanol; Concentrated solution behind the removal ethanol is cooled to 8 ℃, centrifugal 30 minutes; Chloroform extraction 2 times of supernatant after centrifugal, the water that obtains is used ethyl acetate extraction 2 times again, and the acetic acid ethyl acetate extract that obtains after the extraction steams ethyl acetate through Rotary Evaporators, obtains flavone compound 4.12g.
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. the extracting method of a propolis flavone is characterized in that, described method comprises the steps:
(1) the propolis powder is that the 80-90% alcoholic solution mixes with concentration, soaks 16-24 hour under 70-85 ℃ temperature;
(2) the solution reflux, extract, obtains lixiviating solution;
(3) lixiviating solution is concentrated, Recycled ethanol;
(4) concentrated solution behind the removal ethanol is cooled to 5-10 ℃, centrifugal 20-30 minute;
(5) supernatant after centrifugal is with chloroform extraction 2 times, and the water that obtains is used ethyl acetate extraction 2 times again, and the acetic acid ethyl acetate extract that obtains after the extraction steams ethyl acetate through Rotary Evaporators, obtains flavone compound.
2. the method for claim 1 is characterized in that, the solid-to-liquid ratio of described propolis powder and alcoholic solution is 1: 15-20.
3. the method for claim 1 is characterized in that, described reflux, extract,, and extraction time is 3 times, each 1 hour, merge extractive liquid.
4. the method for claim 1 is characterized in that, described concentrating is concentrating under reduced pressure.
5. the method for claim 1 is characterized in that, the step of described extraction specifically comprises:
(1) supernatant chloroform extraction 2 times, each 40ml, water merges;
(2) water ethyl acetate extraction 2 times, each 35ml, acetic acid ethyl acetate extract merges;
(3) steam ethyl acetate through Rotary Evaporators and obtain flavone compound.
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| CN2012104668376A CN102935091A (en) | 2012-11-19 | 2012-11-19 | Propolis flavonoid extracting method |
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| CN2012104668376A CN102935091A (en) | 2012-11-19 | 2012-11-19 | Propolis flavonoid extracting method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557834A (en) * | 2015-01-21 | 2015-04-29 | 聊城大学 | Method for separating and purifying pinocembrin, chrysin and galangin from Chinese propolis aqueous extract |
| CN104592188A (en) * | 2015-01-21 | 2015-05-06 | 聊城大学 | Method for separating and purifying derivative of pinobanksin and caffeic acid from Chinese propolis aqueous extract |
| CN105726448A (en) * | 2016-04-12 | 2016-07-06 | 广州智媛生物科技有限公司 | Skin care product containing multiple honeycomb active ingredients and preparing method thereof |
| CN106420833A (en) * | 2016-08-15 | 2017-02-22 | 上海沪郊蜂业联合社有限公司 | Propolis flavone, propolis flavone refining method and application of propolis flavone |
| CN106420833B (en) * | 2016-08-15 | 2019-07-16 | 上海沪郊蜂业联合社有限公司 | The refining methd and propolis flavone of a kind of propolis flavone and application |
| CN112409313A (en) * | 2020-12-17 | 2021-02-26 | 海南医学院 | Method for extracting galangin from galangal by high-temperature-ethanol combination |
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| CN101081233A (en) * | 2007-02-02 | 2007-12-05 | 北京蜜香村蜂胶有限责任公司 | Method for preparing water-soluble propolis extract liquid |
| CN101417990A (en) * | 2008-11-18 | 2009-04-29 | 大连工业大学 | Method for extracting burdock leaf flavonoids |
| CN102283866A (en) * | 2011-06-16 | 2011-12-21 | 张大辉 | Method for extracting propolis containing high-purity flavones |
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2012
- 2012-11-19 CN CN2012104668376A patent/CN102935091A/en active Pending
Patent Citations (3)
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| CN101081233A (en) * | 2007-02-02 | 2007-12-05 | 北京蜜香村蜂胶有限责任公司 | Method for preparing water-soluble propolis extract liquid |
| CN101417990A (en) * | 2008-11-18 | 2009-04-29 | 大连工业大学 | Method for extracting burdock leaf flavonoids |
| CN102283866A (en) * | 2011-06-16 | 2011-12-21 | 张大辉 | Method for extracting propolis containing high-purity flavones |
Non-Patent Citations (1)
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| 程伟贤等: "蜂胶中黄酮成分及提取方法研究", 《云南大学学报（自然科学版）》, vol. 28, no. 1, 31 December 2006 (2006-12-31) * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557834A (en) * | 2015-01-21 | 2015-04-29 | 聊城大学 | Method for separating and purifying pinocembrin, chrysin and galangin from Chinese propolis aqueous extract |
| CN104592188A (en) * | 2015-01-21 | 2015-05-06 | 聊城大学 | Method for separating and purifying derivative of pinobanksin and caffeic acid from Chinese propolis aqueous extract |
| CN104592188B (en) * | 2015-01-21 | 2016-08-24 | 聊城大学 | A kind of isolated and purified pinobanksin and method of caffeinic derivant from China's Water extracts of propolis |
| CN105726448A (en) * | 2016-04-12 | 2016-07-06 | 广州智媛生物科技有限公司 | Skin care product containing multiple honeycomb active ingredients and preparing method thereof |
| CN105726448B (en) * | 2016-04-12 | 2018-08-24 | 广州智媛生物科技有限公司 | A kind of skin care item and preparation method thereof of the honeycomb active constituent containing there are many |
| CN106420833A (en) * | 2016-08-15 | 2017-02-22 | 上海沪郊蜂业联合社有限公司 | Propolis flavone, propolis flavone refining method and application of propolis flavone |
| CN106420833B (en) * | 2016-08-15 | 2019-07-16 | 上海沪郊蜂业联合社有限公司 | The refining methd and propolis flavone of a kind of propolis flavone and application |
| CN112409313A (en) * | 2020-12-17 | 2021-02-26 | 海南医学院 | Method for extracting galangin from galangal by high-temperature-ethanol combination |
| CN112409313B (en) * | 2020-12-17 | 2023-09-01 | 海南医学院 | Method for extracting galangin from galangal by high temperature-ethanol combination |
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Application publication date: 20130220 |