CN101759678A - Method for preparing kaempferol - Google Patents
Method for preparing kaempferol Download PDFInfo
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- CN101759678A CN101759678A CN200910234062A CN200910234062A CN101759678A CN 101759678 A CN101759678 A CN 101759678A CN 200910234062 A CN200910234062 A CN 200910234062A CN 200910234062 A CN200910234062 A CN 200910234062A CN 101759678 A CN101759678 A CN 101759678A
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- kaempferol
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Abstract
The invention relates to a method for separating and purifying kaempferol, which is low in cost, high in yield, short in period and easy to industrialize. The method comprises the process steps of: pulverizing raw materials containing the kaempferol, then adding 1 to 2 percent sodium hydroxide solution into the raw materials for extraction, regulating a pH value to 5 to 7 for enzymolysis, extracting enzymolysis liquid by using ethyl acetate, and after decompressing and concentrating the extraction liquid, performing three times of recrystallization by using methyl alcohol to prepare products. The kaempferol prepared by adopting the method is simple in process, high in utilization rate of the raw materials and high in purity.
Description
Technical field:
The present invention relates to the extraction and purification process of kaempferol, particularly a kind of method of using enzymolysis, recrystallization purification kaempferol.
Background technology:
Kaempferol
Another name: trifolitin-3, kaempferol, Kaempferol, kaempferol, thesine III.
English name: Kaempferol
CAS number: 520-18-3
Structural formula:
Molecular formula and molecular weight: C
15H
10O
6286.23
Physical properties: kaempferol belongs to flavonols, yellow needle, and 276 ℃-278 ℃ of fusing points are to light and air-sensitive.Kaempferol is slightly soluble in water, is 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.Has the mutagenic compound activity, when concentration is 1 * 10
-4During mol/L, can suppress lymphopoiesis.Be mainly used in anticancer, suppress fertility, anti-epileptic, anti-inflammatory, antioxidant, spasmolysis, antiulcer agent, cholagogic diuretic(s), cough-relieving.
About the document that extracts the kaempferol single component seldom.
Summary of the invention:
The objective of the invention is in order to provide a kind of production technique simple, the raw material availability height, production cost is low, and kaempferol purity reaches more than 90%, and yield is greater than 80%, and output is big, and the cycle is short, is easy to realize industrialized kaempferol extraction process.
The object of the present invention is achieved like this:
1. alkali is carried: with raw material pulverizing, add alkali lye and dissolve, the boiling water bath heating is extracted, and cooling is filtered, and gets filtrate;
2. enzymolysis: the filtrate acid adjustment to slightly acidic, is added the enzyme of raw materials quality 0.5～1%, is stirred and heated to 40～50 ℃ of hydrolysis 15～20 hours, hydrolyzed solution;
3. extraction: said hydrolyzed liquid is concentrated into 1/10～1/15 of original volume, adds ethyl acetate and stir extraction, ester phase reclaim under reduced pressure ethyl acetate gets medicinal extract;
4. recrystallization: medicinal extract is with recrystallizing methanol 3 times, yellow needle crystal product;
Above-mentioned preparing kaempferol is characterized in that described raw material refers to that exsiccant Kaempferia galanga, thesium Chinese turcz, Ginkgo Leaf or other contain one or more of plant of kaempferol and derivative thereof.
Above-mentioned preparing kaempferol is characterized in that it is that 1～2% sodium hydroxide concentration is 8～10 times of amounts of raw materials quality that described alkali is carried the used alkali lye of step, and extraction time is 1.5～2 hours.
Above-mentioned preparing kaempferol is characterized in that described acid adjustment can use acetic acid, phosphoric acid, and pH transfers to 5～7.
Above-mentioned preparing kaempferol is characterized in that in the optional amylase of described enzyme, cellulase, the beta-glucan glycosides enzyme one or more.
Above-mentioned preparing kaempferol is characterized in that described methanol concentration is 80～95%, and saturated dissolving refluxes.
There is following advantage in the present invention:
1) improves the extraction yield of kaempferol with the alkaline extraction kaempferol, protected the unstable structure of kaempferol not to be destroyed simultaneously;
2) both reduced the solubleness of kaempferol with the weak acid acidifying, and generated buffer solvent simultaneously and make enzymolysis process can be stabilized in activation condition;
3) hydrolysis can make the kaempferol that is present in the raw material with the glycosides form decompose out, improves raw material availability, and with relative other hydrolysis method condition milders of enzymic hydrolysis, more saves energy.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
10kg raw material (kaempferol and derivative equivalence content 2.4% thereof) is pulverized, added 80L and add 1% sodium hydroxide, stirring heating is 1.5 hours in the boiling water bath, and cooling is filtered; Adding phosphoric acid accent pH in the filtrate is 5, adds the 50g cellulase, is warmed up to 40 ℃ in agitating heater, stablizes hydrolysis in 15 hours, gets the 84L hydrolyzed solution; The hydrolyzed solution heating is concentrated to 8L, adds ethyl acetate and stir extraction, get ester phase reclaim under reduced pressure ethyl acetate, get 487g medicinal extract; Medicinal extract is with 2L 95% methyl alcohol, finally obtains 213g content and be 92.1% kaempferol finished product.
Embodiment 2:
10kg raw material (kaempferol and derivative equivalence content 3.1% thereof) is pulverized, added 90L and add 1.5% sodium hydroxide, stirring heating is 1.7 hours in the boiling water bath, and cooling is filtered; Adding phosphoric acid accent pH in the filtrate is 6, adds 75g amylase, is warmed up to 45 ℃ in agitating heater, stablizes hydrolysis in 18 hours, gets the 95L hydrolyzed solution; The hydrolyzed solution heating is concentrated to 8L, adds ethyl acetate and stir extraction, get ester phase reclaim under reduced pressure ethyl acetate, get 506g medicinal extract; Medicinal extract is with 2.5L 85% methyl alcohol, finally obtains 279g content and be 94.3% kaempferol finished product.
Embodiment 3:
10kg raw material (kaempferol and derivative equivalence content 2.7% thereof) is pulverized, added 100L and add 1.5% sodium hydroxide, stirring heating is 2 hours in the boiling water bath, and cooling is filtered; Adding acetic acid accent pH in the filtrate is 7, adds 100g beta-glucan glycosides enzyme, is warmed up to 50 ℃ in agitating heater, stablizes hydrolysis in 20 hours, gets the 107L hydrolyzed solution; The hydrolyzed solution heating is concentrated to 7L, adds ethyl acetate and stir extraction, get ester phase reclaim under reduced pressure ethyl acetate, get 496g medicinal extract; Medicinal extract is with 3L 80% methyl alcohol, finally obtains 246g content and be 96.5% kaempferol finished product.
Claims (6)
1. preparing kaempferol is characterized in that comprising following step:
1. alkali is carried: with raw material pulverizing, add alkali lye and dissolve, the boiling water bath heating is extracted, and cooling is filtered, and gets filtrate;
2. enzymolysis: the filtrate acid adjustment to slightly acidic, is added the enzyme of raw materials quality 0.5-1%, is stirred and heated to 40～50 ℃ of hydrolysis 15～20 hours, hydrolyzed solution;
3. extraction: said hydrolyzed liquid is concentrated into 1/10～1/15 of original volume, adds ethyl acetate and stir extraction, ester phase reclaim under reduced pressure ethyl acetate gets medicinal extract;
4. recrystallization: medicinal extract is with recrystallizing methanol 3 times, yellow needle crystal product.
2. according to the described preparing kaempferol of claim 1, it is characterized in that described raw material refers to that exsiccant Kaempferia galanga, thesium Chinese turcz, Ginkgo Leaf or other contain one or more of plant of kaempferol and derivative thereof.
3. according to the described preparing kaempferol of claim 1, it is characterized in that it is 1～2% sodium hydroxide that described alkali is carried the used alkali lye of step, consumption is 8～10 times of amounts of raw materials quality, and extraction time is 1.5～2 hours.
4. according to the described preparing kaempferol of claim 1, it is characterized in that described acid adjustment can use acetic acid, phosphoric acid, pH transfers to 5～7.
5. according to the described preparing kaempferol of claim 1, it is characterized in that in the optional amylase of described enzyme, cellulase, the beta-glucan glycosides enzyme one or more.
6. according to the described preparing kaempferol of claim 1, it is characterized in that described methanol concentration is 80～95%, saturated dissolving refluxes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910234062A CN101759678A (en) | 2009-11-20 | 2009-11-20 | Method for preparing kaempferol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910234062A CN101759678A (en) | 2009-11-20 | 2009-11-20 | Method for preparing kaempferol |
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| CN101759678A true CN101759678A (en) | 2010-06-30 |
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| CN200910234062A Pending CN101759678A (en) | 2009-11-20 | 2009-11-20 | Method for preparing kaempferol |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845467A (en) * | 2010-05-10 | 2010-09-29 | 苏州瑞蓝博中药技术开发有限公司 | Method for extracting kaempferol |
| CN101941961A (en) * | 2010-09-20 | 2011-01-12 | 河南科技大学 | Method for extracting and separating kaempferol from impatiens balsamina |
| CN103142742A (en) * | 2013-03-21 | 2013-06-12 | 河北康利动物药业有限公司 | Method for preparing oral solution of poplar flower |
| CN104458857A (en) * | 2014-12-12 | 2015-03-25 | 广西科技大学 | Preparation method of kaempferol molecularly imprinted membrane based electrochemical sensor |
| CN104557833A (en) * | 2015-01-08 | 2015-04-29 | 廊坊弘祥隆生物技术有限公司 | Method for extracting kaempferol by utilizing peach blossoms |
| CN111675618A (en) * | 2020-06-20 | 2020-09-18 | 贵州中医药大学 | Compound in pyrrosia pedunculata and separation and purification method and application thereof |
| CN112168835A (en) * | 2020-11-03 | 2021-01-05 | 重庆医科大学 | Application of murysicin in preparation of cholagogue drugs |
-
2009
- 2009-11-20 CN CN200910234062A patent/CN101759678A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845467A (en) * | 2010-05-10 | 2010-09-29 | 苏州瑞蓝博中药技术开发有限公司 | Method for extracting kaempferol |
| CN101941961A (en) * | 2010-09-20 | 2011-01-12 | 河南科技大学 | Method for extracting and separating kaempferol from impatiens balsamina |
| CN101941961B (en) * | 2010-09-20 | 2012-12-12 | 河南科技大学 | Method for extracting and separating kaempferol from impatiens balsamina |
| CN103142742A (en) * | 2013-03-21 | 2013-06-12 | 河北康利动物药业有限公司 | Method for preparing oral solution of poplar flower |
| CN104458857A (en) * | 2014-12-12 | 2015-03-25 | 广西科技大学 | Preparation method of kaempferol molecularly imprinted membrane based electrochemical sensor |
| CN104557833A (en) * | 2015-01-08 | 2015-04-29 | 廊坊弘祥隆生物技术有限公司 | Method for extracting kaempferol by utilizing peach blossoms |
| CN111675618A (en) * | 2020-06-20 | 2020-09-18 | 贵州中医药大学 | Compound in pyrrosia pedunculata and separation and purification method and application thereof |
| CN111675618B (en) * | 2020-06-20 | 2023-03-31 | 贵州中医药大学 | Compound in pyrrosia pedunculata and separation and purification method and application thereof |
| CN112168835A (en) * | 2020-11-03 | 2021-01-05 | 重庆医科大学 | Application of murysicin in preparation of cholagogue drugs |
| CN112168835B (en) * | 2020-11-03 | 2022-04-08 | 重庆医科大学 | Application of murysicin in preparation of cholagogue drugs |
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Application publication date: 20100630 |