CN102250979A - Method for extracting and separating kaempferol from Ligustrum sinense branches and leaves - Google Patents
Method for extracting and separating kaempferol from Ligustrum sinense branches and leaves Download PDFInfo
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- CN102250979A CN102250979A CN2011100903989A CN201110090398A CN102250979A CN 102250979 A CN102250979 A CN 102250979A CN 2011100903989 A CN2011100903989 A CN 2011100903989A CN 201110090398 A CN201110090398 A CN 201110090398A CN 102250979 A CN102250979 A CN 102250979A
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Abstract
The invention discloses a method for extracting and separating kaempferol from Ligustrum sinense branches and leaves, which comprises the following steps: carrying out thermal-soak extraction on Ligustrum sinense twice, regulating the pH value, enriching with macroporous adsorbent resin, and flushing the columns with deionized water flushing liquid; after the effluent liquid becomes clear, eluting the flushed column filler with 0.8-1 wt% sodium hydroxide eluting liquid, and collecting the eluate; and regulating the pH value of the eluate, carrying out enzymolysis, crystallizing, filtering, and recrystallizing multiple times, thereby obtaining the yellow acicular crystal kaempferol refined product. The method has the advantages of low production cost and wide industrialization prospects, is simple to operate and can easily implement industrial production.
Description
Technical field
The present invention relates to extraction and separation method, particularly a kind of from light leaf ligustrum sinense branch and leaf the method for extraction separation kaempferol.
Background technology
Light leaf ligustrum sinense (
L. sinense Lour var ni ti dum Ruhd) be that wood is selected the Oleaceae of section Ligustrum
Ligustrum LinnPlant, be evergreen shrubs.Chemical constitution study shows: mainly contain alkane, high fatty alcohol, and steroid compound, triterpene compound, flavonoid compound, wherein the content of kaempferitrine is higher.
Kaempferol (
Kaempferol), another name: trifolitin-3 kaempferol, Kaempferol, kaempferol, thesine III; Kaempferol belongs to flavonols (molecular formula C
15H
10O
6Molecular weight 286.23), yellow needle, 276 ℃ of-278 ℃ of kaempferols of fusing point are slightly soluble in water, are dissolved in hot ethanol, ether and alkali; Pharmacological action: antibiotic, staphylococcus aureus and Pseudomonas aeruginosa, Corynebacterium diphtheriae, dysentery bacterium all there are restraining effect.Cough-relieving, the treatment bronchitis.Press down enzyme, suppress the eye aldose reductase, help the treatment of diabetic cataract.Have the mutagenic compound activity, when concentration is 1 * 10-4mol/L, can suppress lymphopoiesis.Be mainly used in anticancer, suppress fertility, anti-epileptic, anti-inflammatory, antioxidant, spasmolysis, antiulcer agent, cholagogic diuretic(s), cough-relieving.
Mostly the method for preparing at present kaempferol is directly to separate kaempferol from former plant, and its kaempferol content is low, its technology relative complex, and yield is low.And utilize the method for enzymolysis extraction separation kaempferol from plant to yet there are no report at present.
Summary of the invention
The object of the present invention is to provide a kind of from light leaf ligustrum sinense branch and leaf the method for extraction separation kaempferol, this method is simple.
In order to realize above-mentioned task, the technical solution that the present invention adopts is:
A kind of method of extracting kaempferol from light leaf ligustrum sinense branch and leaf is characterized in that carrying out according to the following steps:
1) powder of at first getting light leaf ligustrum sinense branch and leaf is a raw material, with mass concentration is that 5% calcium hydroxide water temperature lixiviate is got 2 times, extract for the first time the mass concentration of using and be 5% calcium hydroxide water consumption 8 times as the raw material total mass, extract for the second time the mass concentration of using and be 5% calcium hydroxide water consumption 5 times as the raw material total mass, extraction time is 2h, merge extracted twice liquid, transfer extracting liquid pH value to 8-9, standby;
2) purifying: will regulate macroporous resin column on the extracting solution after the pH value, the resin model is AB-8, and the pH value is 8-9, and it is 5-6 times of resin column volume that last sample extracts liquid measure, 1.8 times/h of absorption flow velocity; Wait to adsorb saturated back and use the deionized water washing fluid towards post, after the effluent liquid clarification, the sodium hydroxide wash-out liquid wash-out of mass concentration 0.8%-1% of the cylinder filler after washing, the elutriant consumption is 2 times of-2.5 times of resin column volumes, 1 times/h of flow velocity collects elutriant;
3) enzymolysis: the elutriant of gained is poured in the reactor, and ℃ insulation of adjust pH to 5 post-heating to 50 adds 5-7 and doubly measures alpha-L-Rhamnosidase, enzymolysis 6-8h under heat-retaining condition;
4) crystallization: zymolyte is put cold, centrifugal, is obtained the kaempferol crude product, the kaempferol crude product with ethyl alcohol recrystallization after, get final product the kaempferol elaboration of yellow needle crystal.
The present invention is extraction solvent with the calcium hydroxide aqueous solution, and resin can repeat regeneration, with enzymolysis transformation efficiency height, improved the utilization ratio of resource greatly; Its method is simple to operate, production cost is low, and industrial prospect is better, is easy to realize suitability for industrialized production.
Embodiment
The present invention is described in further detail below in conjunction with embodiment that the contriver provides.
The method of extracting kaempferol from light leaf ligustrum sinense branch and leaf of the present invention comprises the following steps:
At first get the powder 10kg of light leaf ligustrum sinense branch and leaf, kaempferitrine content 0.9%, with the calcium hydroxide water extraction of mass concentration 5% 2 times, add-on is 80L for the first time, extracts 2h under 80 ℃～90 ℃ conditions, and add-on is 50L for the second time, extract 2h under 80 ℃～90 ℃ conditions, merge extracted twice liquid, the accent extracting liquid pH value is 8-9, and is standby;
With macroporous resin column on the extracting solution after the adjusting pH value, the resin model is AB-8, and the pH value is 8-9, and it is 60L that last sample extracts liquid measure, 1.8 times/h of absorption flow velocity; Wait to adsorb saturated back and use the deionized water washing fluid towards post, after the effluent liquid clarification, the cylinder filler mass concentration after washing is 0.8%～1% sodium hydroxide wash-out liquid wash-out, and the elutriant consumption is 2～2.5 times of resin column volumes, and 1 times/h of flow velocity collects elutriant.
The elutriant that is obtained is poured in the reactor, transferred insulation behind pH to 5 post-heating to 50 ℃, under heat-retaining condition, add 54g alpha-L-Rhamnosidase, enzymolysis 6-8H then;
Zymolyte is put cold, centrifugal, obtained content and be 72% kaempferol crude product 45g, the saturated dissolving of ethanol of kaempferol crude product, add 0.5% activated carbon decolorizing then, add 3 times of water recrystallize after being concentrated to 1/3 times after the filtration, get final product to such an extent that the content of yellow needle crystal is 98% kaempferol elaboration.
Claims (1)
1. method of extracting kaempferol from light leaf ligustrum sinense branch and leaf is characterized in that carrying out according to the following steps:
1) powder of at first getting light leaf ligustrum sinense branch and leaf is a raw material, with mass concentration is that 5% calcium hydroxide water temperature lixiviate is got 2 times, extract for the first time the mass concentration of using and be 5% calcium hydroxide water consumption 8 times as the raw material total mass, extract for the second time the mass concentration of using and be 5% calcium hydroxide water consumption 5 times as the raw material total mass, extraction time is 2h, merge extracted twice liquid, transfer extracting liquid pH value to 8-9, standby;
2) purifying: will regulate macroporous resin column on the extracting solution after the pH value, the resin model is AB-8, and the pH value is 8-9, and it is 5 times-6 times resin column volume that last sample extracts liquid measure, 1.8 times/h of absorption flow velocity; Wait to adsorb saturated back and use the deionized water washing fluid towards post, after the effluent liquid clarification, the sodium hydroxide wash-out liquid wash-out of mass concentration 0.8%-1% of the cylinder filler after washing, the elutriant consumption is 2 times-2.5 times a resin column volume, 1 times/h of flow velocity collects elutriant;
3) enzymolysis: the elutriant of gained is poured in the reactor, and ℃ insulation of adjust pH to 5 post-heating to 50 adds 5-7 and doubly measures alpha-L-Rhamnosidase, enzymolysis 6-8h under heat-retaining condition;
4) crystallization: zymolyte is put cold, centrifugal, is filtered, obtain the kaempferol crude product, the kaempferol crude product with ethyl alcohol recrystallization after, promptly get the kaempferol elaboration of yellow needle crystal.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110090398 CN102250979B (en) | 2011-04-12 | 2011-04-12 | Method for extracting and separating kaempferol from Ligustrum sinense branches and leaves |
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| CN 201110090398 CN102250979B (en) | 2011-04-12 | 2011-04-12 | Method for extracting and separating kaempferol from Ligustrum sinense branches and leaves |
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| CN102250979A true CN102250979A (en) | 2011-11-23 |
| CN102250979B CN102250979B (en) | 2013-01-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103638114A (en) * | 2013-12-14 | 2014-03-19 | 梁新平 | Method for preparing medicine through breeder seed ligustrum sinense |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1702174A (en) * | 2005-01-06 | 2005-11-30 | 清华大学 | Method for improving polarity of flavonoid glycoside |
| US20080280335A1 (en) * | 2005-01-18 | 2008-11-13 | Amorepacific Corporation | Manufacturing Method of Kaempferol |
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2011
- 2011-04-12 CN CN 201110090398 patent/CN102250979B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1702174A (en) * | 2005-01-06 | 2005-11-30 | 清华大学 | Method for improving polarity of flavonoid glycoside |
| US20080280335A1 (en) * | 2005-01-18 | 2008-11-13 | Amorepacific Corporation | Manufacturing Method of Kaempferol |
Non-Patent Citations (1)
| Title |
|---|
| 顾少君: "银杏黄酮山萘酚和异鼠李素的体外代谢与药物相互作用研究", 《中国优秀硕士学位论文全文数据库（医药卫生科技辑）》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103638114A (en) * | 2013-12-14 | 2014-03-19 | 梁新平 | Method for preparing medicine through breeder seed ligustrum sinense |
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Effective date of registration: 20190911 Address after: 712100 No. 8 Xinqiao Road, Yangling demonstration area, Shaanxi, Xi'an Patentee after: SHAANXI DONGKE PHARMACEUTICAL CO., LTD. Address before: 710043, four storey, Dongxing building, 1 st Lu, Xi'an, Shaanxi Patentee before: Ankang Zhongke Maidisen Natural Pharmaceutical Co.,Ltd. |
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