CN1720935A - Yew preparation and method for preparing the same - Google Patents
Yew preparation and method for preparing the same Download PDFInfo
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- CN1720935A CN1720935A CN 200410054728 CN200410054728A CN1720935A CN 1720935 A CN1720935 A CN 1720935A CN 200410054728 CN200410054728 CN 200410054728 CN 200410054728 A CN200410054728 A CN 200410054728A CN 1720935 A CN1720935 A CN 1720935A
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- ramulus
- taxi cuspidatae
- folium taxi
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Abstract
The invention discloses a process for preparing Chinese yew preparation by using fresh branches and leaves of Chinese yew as raw material, which consists of immersing with ethanol, disintegrating in liquid state, separating solid-liquid states, vacuum distilling and concentrating, dissolving with acetic acid ethyl ester, separating precipitate, reclaiming acetic acid ethyl ester through vacuum distillation, eluting the acetic acid ethyl ester, evaporating eluent to dryness, thus obtaining Chinese yew diterpenes, vacuum distillating and concentrating the precipitate to solid with eluted acetic acid ethyl ester, then charging The invention discloses a process for preparing Chinese yew preparation by using fresh branches and leaves of Chinese yew as raw material, which consists of immersing with ethanol, disintegrating in liquid state, separating solid-liquid states, vacuum distilling and concentrating, dissolving with acetic acid ethyl ester, separating precipitate, reclaiming acetic acid ethyl ester through vacuum distillation, eluting the acetic acid ethyl ester, evaporating eluent to dryness, thus obtaining Chinese yew diterpenes, vacuum distillating and concentrating the precipitate to solid with eluted acetic acid ethyl ester, then charging ethyl maltol, milk powder, Aspartame, xylitol for mixed palletizing, tabletting to obtain the Chinese yew lozenge, concentrating the precipitate to solid with eluted acetic acid ethyl ester vacuum distillation, palletizing with dry method, finally splitting and packaging.
Description
Technical field
The present invention relates to the Chinese herbal medicine preparation method, particularly Ramulus et folium taxi cuspidatae preparation and preparation method
Technical background
Ramulus et folium taxi cuspidatae contains diterpene-kind compound, the Ramulus et folium taxi cuspidatae water extract contains ecdysterone, square-bottomed bamboo basket is foretold glycoside, catechin, epicatechin recklessly, find that also its water extract has blood sugar regulation, promotion insulin secretion, suppresses the sugar absorption, urgees sugared the conversion, the zoopery proof has cholesterol reducing, the effect of triglyceride reducing [Wu Hong, Ramulus et folium taxi cuspidatae tea water extract is regulated the research of human body blood fat, the Chinese public health management, 2002,18 (3)].
Existing Ramulus et folium taxi cuspidatae extracting method adopts following method to extract usually:
The first step: get bark of Ramulus et folium taxi cuspidatae or leaves (dry product)
Second step: pulverize
The 3rd step: ethanol lixiviate 3 times
The 4th step: filter
The 5th step: concentrate
The 6th step: water dissolution
The 7th step: petroleum ether extraction
The 8th step: dichloromethane extraction
The 9th step: evaporation dichloromethane extraction
The tenth step: macroporous resin adsorption
Experiment shows: freezing 96 hours of Taxus leaf, 25 ℃ of vacuum 96 hours do not have significant difference with fresh extractor content, but changing appears in 60 ℃ of 96 hours ultraviolet spectra paclitaxel peaks, show that the contained chemical compound of Taxus leaf has degraded [Fett Neto A G.et al under 60 ℃ of conditions, the distribution and the content of Ramulus et folium taxi cuspidatae different parts paclitaxel, external medicine. plant fascicle, 1994,9 (3)]
There is the factor of destroying active ingredient according to the existing extraction process first step of above-mentioned research and second step, because normally adopt the method for oven dry after the gathering of existing Ramulus et folium taxi cuspidatae, existing breaking method also all adopts mechanical crushing method, high speed mechanical movement conversion thermal energy pulverizing chamber being under the pyritous condition of continuing of temperature, though existing comminution by gas stream technology can alleviate problem of temperature rise, but comminution by gas stream only is useful for the little production kind of processing capacity, the quality of material that the comminution by gas stream technology the is pulverized light efficient that heals is lower, the branch and leaf of Ramulus et folium taxi cuspidatae its proportion little airflow after overbaking is pulverized low, its destructiveness difference of drying means that the terpenoid that natural plant raw material is contained is different with the chemical compound of phenols studies have shown that: Folium Ginkgo adopts different its terpene lactoness of drying mode, there were significant differences for flavones content;
| Different drying conditions | Flavone % | Terpene lactones % | Ginkgolic acid % |
| Dry in the shade | 1.62 | 0.57 | 0.169 |
| Dry | 1.35 | 0.47 | 0.115 |
| 80 ℃ of oven dry | 1.01 | 0.41 | 0.151 |
[He Jun, He Zhaofan, Zhang Diqing, the Folium Ginkgo ginkgetin of different drying conditions, Folium Ginkgo terpene lactones, ginkgolic acid content difference " Chinese herbal medicine " 2004,35 (1)], the drying study of Ramulus et folium taxi cuspidatae raw material has proved; All bearing taxanes have loss [Elsohly after prolonging 10～15 hours drying time, H N.Planta Med.1997,63 (1)], existing technology show that the purpose product of extraction only has paclitaxel and the material that has physiologically active in a large number fail extraction and application such as ecdysterone, square-bottomed bamboo basket is foretold glycoside, catechin, epicatechin recklessly, even adopt supercritical CO
2Fluid is also failed to extract above-claimed cpd and is utilized supercritical CO
2Fluid carry-over ethanol is that cosolvent can extract the great part paclitaxel of bark [Vandana Vishnu.Fjuid phase Equilib, 1996,116 (1/2)], paclitaxel costs an arm and a leg and existing resources utilizes mode that substantial connection is arranged, the extraction process of Ramulus et folium taxi cuspidatae is improved to contained ecdysterone, Hu square-bottomed bamboo basket fore-telling glycoside, catechin, the epicatechin of extraction Ramulus et folium taxi cuspidatae when extracting paclitaxel, be used to prepare the Ramulus et folium taxi cuspidatae preparation, improve the resources costs of taxus resource utilization can reduction paclitaxel.
The present invention be also extract the contained ecdysterone of Ramulus et folium taxi cuspidatae when the contained paclitaxel of a kind of simultaneous extraction Ramulus et folium taxi cuspidatae will be provided, square-bottomed bamboo basket is foretold the process of glycoside, catechin, epicatechin recklessly, and with ecdysterone, square-bottomed bamboo basket is foretold glycoside, catechin, epicatechin and is prepared into the Ramulus et folium taxi cuspidatae preparation recklessly.
Summary of the invention:
The present invention is achieved in that fresh Ramulus et folium taxi cuspidatae chopping is immersed in the ethanol, adopt the high speed shear device to shear then, cut in the process that the Ramulus et folium taxi cuspidatae medical material is sheared by the high speed shear device in ethanol, draw, the mechanical effect of pressing is shredded branch of Ramulus et folium taxi cuspidatae leaf texture, cell is by pressure break, the cell wall permeability changes, the mechanism mass transport process of mixing high speed shear owing to the solvent ethanol that can dissolve terpene substances with branch of Ramulus et folium taxi cuspidatae leaf texture makes terpene substances cement out from branch of Ramulus et folium taxi cuspidatae leaf texture, separate the solidity thing with centrifuge then and collect centrifugal liquid, with centrifugal liquid decompression≤100Pa, ethanol is reclaimed in temperature control≤36 a ℃ distillation, be distilled to the solidity state, the extract that will be distilled to the solidity state then is dissolved in the ethyl acetate, precipitate is separated out in dissolving back to low temperature chamber cold preservation, to precipitate part partly separates with supernatant, ethyl acetate is reclaimed in reduce pressure temperature control distillation of supernatant, add the residual ethyl acetate of ethanol elution after reclaiming ethyl acetate, the temperature control that reduces pressure again is distilled to and is drying to obtain fresh yew branch and leaf diterpene-kind compound extract.Precipitate is separated out in low temperature chamber cold preservation to add the residual ethyl acetate of the adequate amount of ethanol eluting temperature control that reduces pressure again and is distilled to that drying is a fresh yew branch and leaf ecdysterone, square-bottomed bamboo basket is foretold glycoside, catechin, epicatechin extract recklessly, with ecdysterone, recklessly square-bottomed bamboo basket is foretold glycoside, catechin, epicatechin extract and is adopted dry granulation, with the ecdysterone of dry granulation, recklessly square-bottomed bamboo basket to foretell glycoside, catechin, epicatechin bag distribution packaging be the Ramulus et folium taxi cuspidatae electuary.Ecdysterone, Hu square-bottomed bamboo basket are foretold glycoside, catechin, epicatechin interpolation ethyl maltol, milk powder, aspartame, xylitol adjuvant, and interpolation adjuvant mix homogeneously tabletting afterwards is the Ramulus et folium taxi cuspidatae buccal tablet.
Adopt fresh yew branch and leaf raw material to reduce the active component that fresh yew branch and leaf raw material drying process causes and destroy, leaching process temperature control≤36 ℃ have avoided the extraction process heating to cause that biological activity destroys.
Embodiment 1:
The first step: get 10 kilograms in fresh yew branch and leaf.
Second step: strand cut chopping (chopping is extremely less than 5MM length).
The 3rd step: be soaked in 100 liters and contain in the alcohol 95 % solution.
The 4th step: liquid down cut machine is trimmed to No. 5 sieves of solidity thing by " pharmacopeia " regulation.
The 5th step: centrifuge separates solidity thing, extracting centrifugal liquid.
The 6th step:, reclaim ethanol with centrifugal liquid distilling under reduced pressure (be decompressed to≤100Pa, temperature control≤36 ℃); Steam the part moisture that removes in the mixed solution, be distilled to drying solid.
The 7th step: will be distilled to exsiccant solid and add an amount of ethyl acetate, and mix the back and stirred 60 minutes.
The 8th step: the mixed liquor after the stirring is seated in 5 ℃ of environment Cryoprecipitation (separate out the ethyl acetate insoluble matter and make it precipitation) 24 hours with it.
The 9th step: supernatant behind the Cryoprecipitation and precipitate are separated.
The tenth step: ethyl acetate (be decompressed to 100Pa, temperature control≤36 ℃) is reclaimed in the supernatant distilling under reduced pressure, add 2 liter of 95% residual ethyl acetate of ethanol elution after being distilled to solid, distilling under reduced pressure is to being drying to obtain fresh yew branch and leaf Diterpenes extract again.
The 11 step: the precipitate told behind the Cryoprecipitation is added 2 liter of 95% residual ethyl acetate of ethanol elution, and distilling under reduced pressure again (be decompressed to≤100Pa, temperature control≤46 ℃) evaporate to dryness ethanol and residual moisture can collect that the fresh yew branch and leaf extract the Ramulus et folium taxi cuspidatae ecdysterone, square-bottomed bamboo basket is foretold glycoside, catechin, epicatechin mixture recklessly.
The 12 step: Ramulus et folium taxi cuspidatae ecdysterone, Hu square-bottomed bamboo basket are foretold glycoside, catechin, epicatechin mixture employing dry granulation.
The 13 step: with the particulate mixtures splitting encapsulation of dry granulation is the Ramulus et folium taxi cuspidatae electuary.
The 14 step: with the Ramulus et folium taxi cuspidatae ecdysterone, recklessly square-bottomed bamboo basket is foretold glycoside, catechin, epicatechin mixture and added ethyl maltol, milk powder, aspartame, xylitol (ratio of interpolation and Ramulus et folium taxi cuspidatae ecdysterone, square-bottomed bamboo basket fore-telling glycoside, catechin, epicatechin mixture 1: 1) recklessly.
The 15 step: with mix homogeneously behind ecdysterone, Hu square-bottomed bamboo basket fore-telling glycoside, catechin, epicatechin mixture interpolation ethyl maltol, milk powder, aspartame, the xylitol.
The 16 step: with dry granulation behind the mix homogeneously behind ecdysterone, Hu square-bottomed bamboo basket fore-telling glycoside, catechin, epicatechin mixture interpolation ethyl maltol, milk powder, aspartame, the xylitol.
The 17 step: with mixture punching behind the ecdysterone after granulating, Hu square-bottomed bamboo basket fore-telling glycoside, catechin, epicatechin mixture interpolation ethyl maltol, milk powder, aspartame, the xylitol is the Ramulus et folium taxi cuspidatae buccal tablet.
Claims (14)
1. the Ramulus et folium taxi cuspidatae preparation is characterized in that raw material is a fresh yew branch and leaf extract ecdysterone, square-bottomed bamboo basket fore-telling glycoside, catechin, epicatechin mix with adjuvant recklessly.
2. be ethyl maltol, milk powder, aspartame, xylitol by the described Ramulus et folium taxi cuspidatae pharmaceutical adjunct of claim 1.
3. be buccal tablet by the described Ramulus et folium taxi cuspidatae preparation formulation of claim 1.
4. be electuary by the described Ramulus et folium taxi cuspidatae preparation formulation of claim 1.
5. be that fresh yew branch and leaf extract ecdysterone, Hu square-bottomed bamboo basket are foretold glycoside, catechin, epicatechin by the described Ramulus et folium taxi cuspidatae preparation raw material of claim 4.
6. be that fresh yew branch and leaf extract ecdysterone, Hu square-bottomed bamboo basket are foretold glycoside, catechin, epicatechin dry granulation by the described Ramulus et folium taxi cuspidatae preparation of claim 4.
7. the preparation method of Ramulus et folium taxi cuspidatae preparation, by shearing, alcohol mixed solution immersion, liquid grinding, solid-liquid separation, distilling under reduced pressure to solid, acetic acid ethyl dissolution, cold precipitation, tell precipitate, distilling under reduced pressure and reclaim ethyl acetate, the residual ethyl acetate of ethanol elution, reclaim ethanol and form.
8. by claim 8 Ramulus et folium taxi cuspidatae preparation and preparation method, it is characterized in that the fresh yew branch and leaf put liquid the shearing.
9. by claim 8 Ramulus et folium taxi cuspidatae preparation and preparation method, it is characterized in that the mixed solution ethanol content is 95%.
10. by claim 8 Ramulus et folium taxi cuspidatae preparation and preparation method, it is characterized in that distilling under reduced pressure is decompressed to≤100Pa, temperature control≤36 ℃, reclaims ethanol.
11., it is characterized in that concentrating the solidity thing and add acetic acid ethyl dissolution, make cold precipitation by claim 8 Ramulus et folium taxi cuspidatae preparation and preparation method.
12. by claim 12 Ramulus et folium taxi cuspidatae preparation and preparation method, 2～5 ℃ of Cryoprecipitation environment temperature controls.
13. by claim 8 Ramulus et folium taxi cuspidatae preparation and preparation method, it is characterized in that Cryoprecipitation is separated out the supernatant distilling under reduced pressure reclaims ethyl acetate, decompression 100Pa, temperature control≤40 ℃.
14., it is characterized in that the residual ethyl acetate of ethanol elution by claim 8 Ramulus et folium taxi cuspidatae preparation and preparation method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410054728 CN1720935A (en) | 2004-07-18 | 2004-07-18 | Yew preparation and method for preparing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410054728 CN1720935A (en) | 2004-07-18 | 2004-07-18 | Yew preparation and method for preparing the same |
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| CN1720935A true CN1720935A (en) | 2006-01-18 |
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| CN 200410054728 Pending CN1720935A (en) | 2004-07-18 | 2004-07-18 | Yew preparation and method for preparing the same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102641308A (en) * | 2012-05-16 | 2012-08-22 | 江苏红豆杉生物科技有限公司 | Taxus chinensis var mairei Chinese herbal material as well as processing method and application thereof |
| CN103690596A (en) * | 2013-12-04 | 2014-04-02 | 黎川县东鑫实业有限公司 | Compound ground hemlock tea buccal tablet and preparation process thereof |
| CN103719485A (en) * | 2013-12-04 | 2014-04-16 | 黎川县东鑫实业有限公司 | Compound yew tea effervescent tablet and preparation process thereof |
| CN105541761A (en) * | 2015-12-28 | 2016-05-04 | 深圳中农科工创业资产管理有限公司 | Paclitaxel crystal and preparation method of medicinal liquor and oral liquid of paclitaxel crystal |
| CN105878301A (en) * | 2014-11-28 | 2016-08-24 | 北京罗瑞生物科技有限公司 | Yew extract external use anti-diabetic preparation |
-
2004
- 2004-07-18 CN CN 200410054728 patent/CN1720935A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102641308A (en) * | 2012-05-16 | 2012-08-22 | 江苏红豆杉生物科技有限公司 | Taxus chinensis var mairei Chinese herbal material as well as processing method and application thereof |
| CN103690596A (en) * | 2013-12-04 | 2014-04-02 | 黎川县东鑫实业有限公司 | Compound ground hemlock tea buccal tablet and preparation process thereof |
| CN103719485A (en) * | 2013-12-04 | 2014-04-16 | 黎川县东鑫实业有限公司 | Compound yew tea effervescent tablet and preparation process thereof |
| CN105878301A (en) * | 2014-11-28 | 2016-08-24 | 北京罗瑞生物科技有限公司 | Yew extract external use anti-diabetic preparation |
| CN105541761A (en) * | 2015-12-28 | 2016-05-04 | 深圳中农科工创业资产管理有限公司 | Paclitaxel crystal and preparation method of medicinal liquor and oral liquid of paclitaxel crystal |
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Open date: 20060118 |