CN101735290A - Method for extracting phillyrin from forsythia - Google Patents
Method for extracting phillyrin from forsythia Download PDFInfo
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- CN101735290A CN101735290A CN200810176773A CN200810176773A CN101735290A CN 101735290 A CN101735290 A CN 101735290A CN 200810176773 A CN200810176773 A CN 200810176773A CN 200810176773 A CN200810176773 A CN 200810176773A CN 101735290 A CN101735290 A CN 101735290A
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- weeping forsythia
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Abstract
The invention provides a method for extracting phillyrin from forsythia, which relates to a novel method for extracting phillyrin by the steps of soaking with ethyl alcohol solution, adding surfactant and heating by microwaves. The traditional product generally has the defects of low yield rate, poor stability, high production cost and the like. The method comprises the following steps of: crushing forsythia into 16 meshes; adding 58% ethyl alcohol solution for soaking; adding surfactant which accounts for 0.03-0.3% of the weight of the mixture; heating by microwaves, standing and filtering; adding 58% ethyl alcohol solution into residues for soaking; heating by microwaves, standing and filtering; combining filter liquors, evaporating solvent by using a rotary evaporator, adding a small amount of methyl alcohol solution, adding alumina and uniformly stirring, and evaporating. The operations are performed on the basis of official method, the phillyrin is put on a treated neutral alumina column to elute and evaporate, and then the phillyrin powder is prepared. The invention is used for extracting phillyrin.
Description
Technical field:
The invention belongs to the Chinese medicine preparation technical field, be specifically related to a kind of novel process of extracting phyllyrin.
Background technology:
Traditional extracting method mainly contains: decocting method, percolation, poach-alcohol precipitation extraction method etc.In the process of Chinese medicine preparation, microwave is as a kind of novel energy, and it is strong to have penetrance, quick heating, the characteristics of homogeneous heating.The present invention is used for the extraction of Chinese medicine capsule of weeping forsythia effective constituent phyllyrin with microwave, and traditional decocting process technology by comparison is more loaded down with trivial details, and is consuming time longer, and it is bigger to consume energy, defectives such as productive rate is low, product stability can be relatively poor, production cost height.
Summary of the invention:
The objective of the invention is to overcome the deficiency of the prior art and the energy, the method for the effective constituent phyllyrin of a kind of efficient, safety, stable, selectivity is high, consuming time less, energy consumption is low, blowdown flow rate the is few extraction capsule of weeping forsythia is provided.
Above-mentioned purpose is achieved through the following technical solutions:
From the capsule of weeping forsythia, extract the novel method of phyllyrin, at first the capsule of weeping forsythia is crushed to 16 orders, the alcohol immersion of adding 58%, the tensio-active agent of adding mixture weight 0.03-0.3% leaves standstill filtration after the microwave heating, residue adds 58% alcohol immersion once more, leave standstill filtration after the microwave heating, merging filtrate boils off solvent on Rotary Evaporators, adds the small amount of methanol dissolving, add neutral alumina and mix evaporate to dryness thoroughly.Press the official method operation, put on the neutral alumina post of having handled well, wash-out, evaporate to dryness obtains the phyllyrin powder.
The described novel method of extracting phyllyrin from the capsule of weeping forsythia, soaking the used liquor capacity of the capsule of weeping forsythia is that 2-20 doubly measures.
The described novel method of extracting phyllyrin from the capsule of weeping forsythia, the used solution of the immersion capsule of weeping forsythia are 58% ethanol.
The described novel method of extracting phyllyrin from the capsule of weeping forsythia, described tensio-active agent is sodium lauryl sulphate (K
12), perhaps Sodium dodecylbenzene sulfonate (LAS), perhaps palmityl trimethyl ammonium chloride (1631).
The described novel method of from the capsule of weeping forsythia, extracting phyllyrin, used microwave frequency is 2450MHz, and used microwave power is 240W, and the time of microwave heating is 20 minutes.
The described novel method of extracting phyllyrin from the capsule of weeping forsythia, the crude product dissolve with methanol after concentrating adds neutral alumina and mixes thoroughly.
The described novel method of from the capsule of weeping forsythia, extracting phyllyrin, the temperature of rotary evaporation is not higher than 55 ℃, and temperature is no more than 50 ℃ during oven dry.
The present invention compared with prior art has the following advantages:
1, the used technology of the present invention is compared with technology such as high-speed counter-current liquid chromatographies, and applicable surface is wider, and facility investment is lower.
2, the used technology of the present invention is compared with decocting method, percolation, poach-technology such as alcohol precipitation extraction method, and product has advantages such as production rate is fast, productive rate is high, stability is good, production cost is lower.
3, the used technology of the present invention adopts microwave extraction and tensio-active agent synergy, has improved the efficient of extracting capsule of weeping forsythia effective constituent phyllyrin more.
4, proving through the contrast experiment, adopt used technology of the present invention and traditional decoction technology to extract the Chinese medicine capsule of weeping forsythia, is that index compares two kinds of methods with the phyllyrin extraction yield.Phyllyrin extraction yield calculation result is shown that the used technology gained of the present invention phyllyrin content is higher.
5. the microwave extraction technology is to be the novel extraction technology of base growth in recent years with conventional solvent extraction principle, this technology have the selectivity height, consuming time less, advantage such as energy consumption is low, blowdown flow rate is few, can overcome the defective of traditional extraction process, compare with technology such as high-speed counter-current liquid chromatographies, applicable surface is wider, and facility investment is low.
The specific embodiment of the present invention:
Embodiment 1
Get capsule of weeping forsythia medicinal material 100g, be crushed to 16 orders, the ethanolic soln of adding 58% soaks to 1000ml, the sodium lauryl sulphate (K of adding 0.3 gram
12), leaving standstill filtration with microwave heating after 20 minutes, residue adds 58% ethanolic soln once more and soaks to 1000ml, microwave heating was left standstill filtration after 20 minutes, and merging filtrate boils off solvent on Rotary Evaporators, added the small amount of methanol dissolving, add neutral alumina and mix evaporate to dryness thoroughly.Press the official method operation, put on the neutral alumina post of having handled well, wash-out, evaporate to dryness obtains the phyllyrin powder.High performance liquid chromatography is analyzed, and uses external standard method content, and the cubage extraction yield of phyllyrin in the root a tree name crude drug, and extraction yield is 61% as a result.
Embodiment 2
Get capsule of weeping forsythia medicinal material 100g, be crushed to 16 orders, add 58% ethanolic soln and soak to 1500ml, the Sodium dodecylbenzene sulfonate (LAS) that adds 1 gram, use 2450MHz, the microwave heating of 240W was left standstill filtration after 20 minutes, and residue adds 58% ethanolic soln once more and soaks to 1500ml, at 2450MHz, the microwave heating of 240W was left standstill filtration after 20 minutes, and merging filtrate boils off solvent on Rotary Evaporators, added the small amount of methanol dissolving, add neutral alumina and mix evaporate to dryness thoroughly.Press the official method operation, put on the neutral alumina post of having handled well, wash-out, evaporate to dryness obtains the phyllyrin powder.High performance liquid chromatography is analyzed, and uses external standard method content, and the cubage extraction yield of phyllyrin in the root a tree name crude drug, and extraction yield is 63% as a result.
Embodiment 3
Get capsule of weeping forsythia medicinal material 100g, be crushed to 16 orders, add 58% ethanolic soln and soak to 2000ml, the palmityl trimethyl ammonium chloride (1631) that adds 3 grams, use 2450MHz, the microwave heating of 240W was left standstill filtration after 20 minutes, and residue adds 58% ethanolic soln once more and soaks to 2000ml, at 2450MHz, the microwave heating of 240W was left standstill filtration after 20 minutes, and merging filtrate boils off solvent on Rotary Evaporators, added the small amount of methanol dissolving, add neutral alumina and mix evaporate to dryness thoroughly.Press the official method operation, put on the neutral alumina post of having handled well, wash-out, evaporate to dryness obtains the phyllyrin powder.High performance liquid chromatography is analyzed, and uses external standard method content, and the cubage extraction yield of phyllyrin in the root a tree name crude drug, and extraction yield is 66% as a result.
Embodiment 4:
At first the capsule of weeping forsythia is crushed to 16 orders, the alcohol solution dipping of adding 60%, other tensio-active agents that add mixture weight 0.03-0.3%, leave standstill filtration after the microwave heating, residue adds alcohol solution dipping once more, leaves standstill filtration after the microwave heating, merging filtrate boils off solvent on Rotary Evaporators, add the small amount of methanol dissolving, add neutral alumina and mix evaporate to dryness thoroughly.Press the official method operation, put on the neutral alumina post of having handled well, wash-out, evaporate to dryness obtains the phyllyrin powder.
Contrast experiment's data:
Contrast 1:
Adopt the method for 50 fens kinds of reflux to replace implementing microwave heating extraction step in 1, all the other are handled the capsule of weeping forsythia by the method for embodiment 1.High performance liquid chromatography is analyzed, and uses external standard method content, and the cubage extraction yield of phyllyrin in the root a tree name crude drug, and extraction yield is 50% as a result.
Contrast 2:
Adopt the water of 5 times of amounts to replace implementing 58% ethanolic soln of 10 times of amounts in 1, all the other are handled the capsule of weeping forsythia by the method for embodiment 1.High performance liquid chromatography is analyzed, and uses external standard method content, and the cubage extraction yield of phyllyrin in the root a tree name crude drug, and extraction yield is 56% as a result.
Contrast 3:
Adopt the way that does not add tensio-active agent, all the other are handled the capsule of weeping forsythia by the method for embodiment 2.High performance liquid chromatography is analyzed, and uses external standard method content, and the cubage extraction yield of phyllyrin in the root a tree name crude drug, and extraction yield is 53% as a result.
Contrast 4:
Microwave is selected the 240W among the 600W replacement embodiment 2 for use, and all the other are handled the capsule of weeping forsythia by the method for embodiment 2.High performance liquid chromatography is analyzed, and uses external standard method content, and the cubage extraction yield of phyllyrin in the root a tree name crude drug, and extraction yield is 55% as a result.
In sum, the present invention by adopt microwave from the capsule of weeping forsythia fast, extracting effective components phyllyrin efficiently, and determined best manufacturing technology.
Claims (7)
1. novel method of from the capsule of weeping forsythia, extracting phyllyrin, it is characterized in that: at first the capsule of weeping forsythia is crushed to 16 orders, the alcohol immersion of adding 58%, the tensio-active agent of adding mixture weight 0.03-0.3% leaves standstill filtration after the microwave heating, residue adds 58% alcohol immersion once more, leave standstill filtration after the microwave heating, merging filtrate boils off solvent on Rotary Evaporators, adds the small amount of methanol dissolving, add neutral alumina and mix evaporate to dryness thoroughly.Press the official method operation, put on the neutral alumina post of having handled well, wash-out, evaporate to dryness obtains the phyllyrin powder.
2. the novel method of extracting phyllyrin from the capsule of weeping forsythia according to claim 1 is characterized in that: soaking the used liquor capacity of the capsule of weeping forsythia is that 2-20 doubly measures.
3. the novel method of extracting phyllyrin from the capsule of weeping forsythia according to claim 1 and 2 is characterized in that: the used solution of the immersion capsule of weeping forsythia is 58% ethanol.
4. the novel method of extracting phyllyrin from the capsule of weeping forsythia according to claim 1 and 2, it is characterized in that: described tensio-active agent is sodium lauryl sulphate (K
12), perhaps Sodium dodecylbenzene sulfonate (LAS), perhaps palmityl trimethyl ammonium chloride (1631).
5. the novel method of from the capsule of weeping forsythia, extracting phyllyrin according to claim 1 and 2, it is characterized in that: used microwave frequency is 2450MHz, and used microwave power is 240W, and the time of microwave heating is 20 minutes.
6. the novel method of extracting phyllyrin from the capsule of weeping forsythia according to claim 1 and 2 is characterized in that: the crude product dissolve with methanol after concentrating adds neutral alumina and mixes thoroughly.
7. the novel method of from the capsule of weeping forsythia, extracting phyllyrin according to claim 1 and 2, it is characterized in that: the temperature of rotary evaporation is not higher than 55 ℃, and temperature is no more than 50 ℃ during oven dry.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810176773XA CN101735290B (en) | 2008-11-18 | 2008-11-18 | Method for extracting phillyrin from forsythia |
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| CN200810176773XA CN101735290B (en) | 2008-11-18 | 2008-11-18 | Method for extracting phillyrin from forsythia |
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| CN101735290A true CN101735290A (en) | 2010-06-16 |
| CN101735290B CN101735290B (en) | 2012-06-27 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161685A (en) * | 2011-03-11 | 2011-08-24 | 河北科星药业有限公司 | Method for preparing forsythin extractive by fructus forsythiae leaves |
| CN104106669A (en) * | 2014-07-02 | 2014-10-22 | 河南科技大学 | Method for preparing grease quality retention agent from forsythin and ascorbic acid |
| CN104170943A (en) * | 2014-07-02 | 2014-12-03 | 河南科技大学 | Composite for meat preservation and preparation method thereof |
| WO2016019685A1 (en) * | 2014-08-07 | 2016-02-11 | 富力 | Quality detection method for active ingredient phillyrin |
| CN108066350A (en) * | 2016-11-16 | 2018-05-25 | 富力 | The application of forsythin, its derivative, forsythin and phillygenol composition in prevention, treatment senile dementia is prepared |
| CN111848702A (en) * | 2020-08-24 | 2020-10-30 | 渠志灿 | Extraction and preparation method of phillyrin |
-
2008
- 2008-11-18 CN CN200810176773XA patent/CN101735290B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161685A (en) * | 2011-03-11 | 2011-08-24 | 河北科星药业有限公司 | Method for preparing forsythin extractive by fructus forsythiae leaves |
| CN104106669A (en) * | 2014-07-02 | 2014-10-22 | 河南科技大学 | Method for preparing grease quality retention agent from forsythin and ascorbic acid |
| CN104170943A (en) * | 2014-07-02 | 2014-12-03 | 河南科技大学 | Composite for meat preservation and preparation method thereof |
| CN104106669B (en) * | 2014-07-02 | 2016-04-13 | 河南科技大学 | The method of oil quality retention agent is prepared with forsythin and ascorbic acid |
| WO2016019685A1 (en) * | 2014-08-07 | 2016-02-11 | 富力 | Quality detection method for active ingredient phillyrin |
| CN108066350A (en) * | 2016-11-16 | 2018-05-25 | 富力 | The application of forsythin, its derivative, forsythin and phillygenol composition in prevention, treatment senile dementia is prepared |
| CN108066350B (en) * | 2016-11-16 | 2020-06-26 | 富力 | Application of phillyrin, phillyrin derivatives, and phillyrin-phillygenin composition in preparation of medicines for preventing and treating senile dementia |
| CN111848702A (en) * | 2020-08-24 | 2020-10-30 | 渠志灿 | Extraction and preparation method of phillyrin |
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| CN101735290B (en) | 2012-06-27 |
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