CN104211667A - Plant extract applied in taxol preparation and preparation method thereof - Google Patents
Plant extract applied in taxol preparation and preparation method thereof Download PDFInfo
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- C07D305/00—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms
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Abstract
The invention discloses a plant extract applied in a taxol preparation and a preparation method thereof. The plant extract applied in the taxol preparation is prepared through following steps: (1) with dried and crushed branches and leaves of taxus chinensis as a raw material, performing extraction through acetone and ethyl acetate; (2) performing pressure reduced concentration to obtain an extract concrete; (3) performing extractive concentration through trichloromethane-water to obtain an extract crude product; and (4) performing stationary phase column chromatoghaphy through an alkaline aluminium oxide and reversed phase chromatography through a C18-silicagel column and performing recrystallization through ethanol to prepare the plant extract. The plant extract is high in the content of taxol and purity and is less in impurities. The preparation method of the plant extract is high in recovery ratio of taxol, is simple in extraction and purification, is low in cost and is energy-saving and environmental-protective.
Description
Technical field
The present invention relates to a kind of plant milk extract being applied to formulation for paclitaxel and preparation method thereof, belong to medical art.
Background technology
Taxol, English name is Paclitaxel, and chemical name is 5 β, 20-epoxy-1,2 α, 4,7 β, 10 β, 13 α-hexahydroxy-Taxan-11-alkene-9-ketone-4,10-diacetate esters-2-benzoic ether-13 [(2 ' R, 3 ' S)-N-benzoyl-3-phenylisoserine ester], molecular weight is 853.92, and molecular formula is C
47h
51nO
14.
Taxol is white crystals body powder, odorless, tasteless, is insoluble in water, is soluble in chloroform, acetone and other organic solvent.Taxol has unique antitumor action, and taxol is mainly applicable to ovarian cancer and mammary cancer, also has certain curative effect to lung cancer, large bowel cancer, melanoma, incidence cancer, lymphoma, brain tumor.Current formulation for paclitaxel is mainly paclitaxel injection etc., and paclitaxel injection is the sterile solution that taxol adds appropriate solubility promoter and stablizer and makes, containing taxol (C
47h
51nO
14) should be the 90.0%-110.0% of labelled amount.
Current taxol mainly extracts from Chinese yew, and all containing taxol in the dry root of taxaceae yew, branches and leaves and bark, but content is lower, is about 0.01% of bark dry weight.Ramulus et folium taxi cuspidatae generally acknowledges endangered natural rare plants for anticancer in the world, has been through the ancient few survivors seeds that quaternary glacier carries over, on earth the history of existing 2,500,000 years.Because growth of taxol speed is slow under field conditions (factors), regenerative power is poor, so for a long time, has not also formed the Ramulus et folium taxi cuspidatae raw material forestbase of advising greatly and touching in world wide.Within 1994, Ramulus et folium taxi cuspidatae is decided to be one-level rare endangered plants by China, is had the country of Ramulus et folium taxi cuspidatae to be called " national treasure " by 42, the whole world simultaneously.
Therefore, the rate of recovery improving taxol in Ramulus et folium taxi cuspidatae seems very necessary.The method of current extraction and isolation taxol has: organic solvent extractionprocess, supercritical fluid extraction, membrane separation process etc.Organic solvent extractionprocess step is many, and the rate of recovery is low, and loss of product is large.Supercritical fluid extraction yield is high, save time, but the method having high input to equipment, high to equipment requirements, operational condition is strict, and production cost is high.Semi-permeable membranes needed for membrane separation process and reverse osmosis unit expensive, operative technique is also very complicated, and production cost is also high.
Summary of the invention
The object of the present invention is to provide a kind of plant milk extract being applied to formulation for paclitaxel and preparation method thereof; improve the rate of recovery of taxol in Ramulus et folium taxi cuspidatae, adopt the method for simple and feasible extraction purification taxol, reduce costs; reduce pollutant emission, be conducive to environment protection.
For solving the problems of the technologies described above, the plant milk extract being applied to formulation for paclitaxel of the present invention with the Ramulus et folium taxi cuspidatae after drying and crushing for raw material, lixiviate is carried out with the mixed solvent of acetoneand ethyl acetate, extract medicinal extract is obtained after concentrating under reduced pressure, extract crude product is obtained after trichloromethane-water extraction is concentrated, through alkali alumina stationary phase column chromatography, then through C
18-silicagel column reversed phase chromatography, obtains finally by ethyl alcohol recrystallization.
For solving the problems of the technologies described above, the preparation method being applied to the plant milk extract of formulation for paclitaxel of the present invention, the method comprises the steps:
Step 1, cleans Ramulus et folium taxi cuspidatae, is ground into powder after cryodrying with pulverizer, carries out lixiviate, vat liquor is carried out concentrating under reduced pressure, recycling design, obtain extract medicinal extract with the mixed solvent of acetoneand ethyl acetate;
Step 2, dissolves extract medicinal extract trichloromethane, then adds purified water, stratification after stirring, and reclaims organic phase, water layer chloroform extraction, merges organic phase, organic phase concentrating under reduced pressure is reclaimed trichloromethane, obtains extract crude product;
Step 3, extract crude product trichloromethane is dissolved, join in the alkali alumina stationary phase post activated, drain, first drain with trichloromethane drip washing, then drain with the mixing eluent drip washing of trichloromethane and methyl alcohol, then use the mixtures of eluents wash-out of trichloromethane and methyl alcohol, by the elutriant concentrating under reduced pressure collected, obtain extract work in-process;
Extract work in-process are dissolved in acetonitrile solution by step 4, join the C balanced
18in-silicagel column, then use acetonitrile solution wash-out, by the elutriant concentrating under reduced pressure crystallization collected, the crystallization filtered out carries out recrystallization with dissolve with ethanol again, finally filters out crystallization, obtains highly purified extract after vacuum-drying.
As improvement of the present invention, the temperature of cryodrying in this step 1 is 50 ~ 60 DEG C, and moisture content≤10% after dry, is ground into 100 ~ 120 object powder.
As improvement of the present invention, in this step 1, the weight of the mixed solvent of acetoneand ethyl acetate is 4 ~ 5 times of Ramulus et folium taxi cuspidatae powder, in mixed solvent, the volume ratio of acetoneand ethyl acetate is 1:0.8 ~ 1, lixiviate is carried out under ultrasonic assistant, extraction temperature is 35 ~ 45 DEG C, extraction time is 1 ~ 2 hour/time, and extracting times is 3 times.
As improvement of the present invention, in this step 1, concentrating under reduced pressure temperature is 50 ~ 60 DEG C, and vacuum tightness is 0.07 ~ 0.09MPa.
As improvement of the present invention, for dissolving 1 ~ 2 times that the weight of the trichloromethane of extract medicinal extract is extract medicinal extract in this step 2, the weight of purified water is 1 ~ 1.5 times of extract medicinal extract, and the stratification time is 4 ~ 6 hours.
As improvement of the present invention, be 1 ~ 2 times of extract medicinal extract for the weight of the trichloromethane of water layer extraction in this step 2, extraction times is 2 times.
As improvement of the present invention, for dissolving 10 ~ 15 times that the weight of the trichloromethane of extract crude product is extract crude product in this step 3, the residence time of extract crude product solution in alkali alumina stationary phase post is 30 ~ 40 minutes.
As improvement of the present invention, the volume ratio of the trichloromethane and methyl alcohol that mix eluent in this step 3 is 98:2 ~ 98.5:1.5, and the trichloromethane of mixtures of eluents and the volume ratio of methyl alcohol are 95:5 ~ 96:4.
As improvement of the present invention, be half-finished 3 ~ 5 times of extract for dissolving the weight of the half-finished acetonitrile solution of extract in this step 4, in acetonitrile solution, the volume ratio of acetonitrile and purified water is 40:60, the each add-on of extract semi-finished product solution is 2 ~ 2.5mg taxol every gram of stationary phase, and in the acetonitrile solution of wash-out, the volume ratio of acetonitrile and purified water is 50:50.
The Ramulus et folium taxi cuspidatae of drying is ground into 100 ~ 120 object powder, is conducive to the better extract of taxol, realizes optimum efficiency.With the taxol in the mixed solvent lixiviate Ramulus et folium taxi cuspidatae of 4 ~ 5 times of acetoneand ethyl acetates (volume ratio is 1:0.8 ~ 1), can obtain best extraction effect, the content of taxol in extract medicinal extract is the highest, and the weight of extract medicinal extract is minimum.With Ultrasonic Wave-Assisted Extraction, can extraction time be shortened, improve extraction effect.Extracting times is 3 times, can realize taxol and extract more completely.With alkali alumina stationary phase column chromatography extract crude product, a large amount of hydroaropic substances, lipid matter and 7-epi-taxol can be removed, taxol can obtain the purification of more than tens times simultaneously, and the rate of recovery of taxol can be greater than 100%, obtains the highest rate of recovery of taxol and purity.The residence time of extract crude product solution in alkali alumina stationary phase post is 30 ~ 40 minutes, 7-epi-taxol can be made constantly to be converted into taxol, also can prevent degradation of paclitaxel.Best drip washing effect can be obtained with the mixing eluent (volume ratio is 98:2 ~ 98.5:1.5) of trichloromethane and methyl alcohol.The best elute effect to taxol can be obtained by the mixtures of eluents (volume ratio is 95:5 ~ 96:4) of trichloromethane and methyl alcohol, realize the recovery that taxol is best.By extract work in-process C
18-silicagel column normal pressure reversed phase chromatography is refined, and can use simple operation step, just can obtain highly purified taxol.At C
18in-silicagel column reversed phase chromatography, each add-on of employing extract semi-finished product solution is the amount of 2 ~ 2.5mg taxol every gram of stationary phase, can obtain best refining effect.Highly purified extract can be applied in formulation for paclitaxel.Compared with prior art, the plant milk extract the being applied to formulation for paclitaxel of the present invention feature that has that content of taxol is high, purity is high, impurity is few etc.The preparation method being applied to the plant milk extract of formulation for paclitaxel of the present invention has the features such as the taxol rate of recovery is high, extraction purification is easy and simple to handle, production cost is low, energy-conserving and environment-protective.
Embodiment
Below in conjunction with specific embodiment, embodiment of the present invention are described in detail.Should be appreciated that enforcement of the present invention is not limited to the following examples, any pro forma accommodation make the present invention and/or change all will fall into protection scope of the present invention.
embodiment 1
Cleaned by Ramulus et folium taxi cuspidatae and remove other foreign material, through 50 DEG C of cryodryings, control moisture content below 10%, pulverizing with pulverizer is 100 object powder.10 kilograms of Ramulus et folium taxi cuspidatae powder are filled in leaching vessel equably, the mixed solvent at every turn adding the acetoneand ethyl acetate (volume ratio of acetoneand ethyl acetate is 1:0.8) of 40 kilograms extracts under ultrasonic assistant, extraction temperature is 35 DEG C, extraction time is 2 hours/time, lixiviate 3 times, merges vat liquor.By the vat liquor of merging temperature 50 degree, concentrate, recycling design under vacuum tightness 0.09MPa condition, obtain Ramulus et folium taxi cuspidatae concentrated extract medicinal extract 1450 grams, in extract medicinal extract, the content of taxol is 0.083%.
By the trichloromethane stirring and dissolving of extract medicinal extract by 1 times of extract medicinal extract weight, then add the purified water of 1 times of extract medicinal extract weight, stir 15-30 minute, stratification 4 hours, reclaim organic phase, water layer adds the chloroform extraction twice of extract medicinal extract weight 1 times again, merges organic phase.Organic phase concentrating under reduced pressure reclaims trichloromethane, and obtain extract crude product 70.20 grams, in extract crude product, paclitaxel concentration is 1.68%.
Extract crude product is dissolved with the trichloromethane of 10 times of extract crude product weight in batches, dissolves completely for subsequent use.In alkali alumina (200-300 order) stationary phase post, first add methyl alcohol, trichloromethane draining successively, activate.Then be added in post by the trichloromethane being dissolved with extract crude product, the residence time is 30 minutes, drains.Then drain with trichloromethane drip washing, drain with mixing eluent (volume ratio 98:2) drip washing of trichloromethane and methyl alcohol.In the pillar that drip washing is good, add the mixtures of eluents (volume ratio 95:5) of trichloromethane and methyl alcohol again, collect elutriant.Repeat above step, merge elutriant, by the elutriant concentrating under reduced pressure merged, obtain extract work in-process 7.76 grams, in extract work in-process, paclitaxel concentration is 15.2%.
Used by extract work in-process the acetonitrile solution (the volume ratio 40:60 of acetonitrile and purified water) of 3 times of extract work in-process weight to dissolve in batches, dissolve completely for subsequent use.First by C
18-silicagel column acetonitrile fully washes out the impurity in stationary phase, then balances with the acetonitrile solution of volume ratio 40:60.Extract semi-finished product solution is added to C by the amount of 2.5mg taxol every gram of stationary phase
18in-silicagel column, then use the acetonitrile solution wash-out of volume ratio 50:50, collect elutriant.Repeat above step, merge elutriant, by the elutriant concentrating under reduced pressure crystallization at 40 DEG C merged, recrystallization is carried out with dissolve with ethanol again after filtering out crystallization, finally filter out crystallization and in 40 DEG C of vacuum-dryings, obtain highly purified extract 1.06 grams, in extract, paclitaxel concentration is 99.6%.
embodiment 2
Cleaned by Ramulus et folium taxi cuspidatae and remove other foreign material, through 60 DEG C of cryodryings, control moisture content below 10%, pulverizing with pulverizer is 120 object powder.10 kilograms of Ramulus et folium taxi cuspidatae powder are filled in leaching vessel equably, the mixed solvent at every turn adding the acetoneand ethyl acetate (volume ratio of acetoneand ethyl acetate is 1:1) of 50 kilograms extracts under ultrasonic assistant, extraction temperature is 40 DEG C, extraction time is 1.5 hours/time, lixiviate 3 times, merges vat liquor.By the vat liquor of merging temperature 55 degree, concentrate, recycling design under vacuum tightness 0.08MPa condition, obtain Ramulus et folium taxi cuspidatae concentrated extract medicinal extract 1433 grams, in extract medicinal extract, the content of taxol is 0.084%.
By the trichloromethane stirring and dissolving of extract medicinal extract by 2 times of extract medicinal extract weight, add the purified water of 1.5 times of extract medicinal extract weight again, stir 15-30 minute, stratification 6 hours, reclaim organic phase, water layer adds the chloroform extraction twice of extract medicinal extract weight 2 times again, merges organic phase.Organic phase concentrating under reduced pressure reclaims trichloromethane, and obtain extract crude product 67.45 grams, in extract crude product, paclitaxel concentration is 1.75%.
Extract crude product is dissolved with the trichloromethane of 15 times of extract crude product weight in batches, dissolves completely for subsequent use.In alkali alumina (200-300 order) stationary phase post, first add methyl alcohol, trichloromethane draining successively, activate.Then be added in post by the trichloromethane being dissolved with extract crude product, the residence time is 35 minutes, drains.Then drain with trichloromethane drip washing, drain with mixing eluent (volume ratio 98.5:1.5) drip washing of trichloromethane and methyl alcohol.In the pillar that drip washing is good, add the mixtures of eluents (volume ratio 96:4) of trichloromethane and methyl alcohol again, collect elutriant.Repeat above step, merge elutriant, by the elutriant concentrating under reduced pressure merged, obtain extract work in-process 6.35 grams, in extract work in-process, paclitaxel concentration is 18.6%.
Used by extract work in-process the acetonitrile solution (the volume ratio 40:60 of acetonitrile and purified water) of 5 times of extract work in-process weight to dissolve in batches, dissolve completely for subsequent use.First by C
18-silicagel column acetonitrile fully washes out the impurity in stationary phase, then balances with the acetonitrile solution of volume ratio 40:60.Extract semi-finished product solution is added to C by the amount of 2mg taxol every gram of stationary phase
18in-silicagel column, then use the acetonitrile solution wash-out of volume ratio 50:50, collect elutriant.Repeat above step, merge elutriant, by the elutriant concentrating under reduced pressure crystallization at 45 DEG C merged, recrystallization is carried out with dissolve with ethanol again after filtering out crystallization, finally filter out crystallization and in 40 DEG C of vacuum-dryings, obtain highly purified extract 1.06 grams, in extract, paclitaxel concentration is 99.7%.
embodiment 3
Cleaned by Ramulus et folium taxi cuspidatae and remove other foreign material, through 55 DEG C of cryodryings, control moisture content below 10%, pulverizing with pulverizer is 110 object powder.10 kilograms of Ramulus et folium taxi cuspidatae powder are filled in leaching vessel equably, the mixed solvent at every turn adding the acetoneand ethyl acetate (volume ratio of acetoneand ethyl acetate is 1:0.9) of 45 kilograms extracts under ultrasonic assistant, extraction temperature is 45 DEG C, extraction time is 1 hour/time, lixiviate 3 times, merges vat liquor.By the vat liquor of merging temperature 60 degree, concentrate, recycling design under vacuum tightness 0.07MPa condition, obtain Ramulus et folium taxi cuspidatae concentrated extract medicinal extract 1455 grams, in extract medicinal extract, the content of taxol is 0.083%.
By the trichloromethane stirring and dissolving of extract medicinal extract by 1.5 times of extract medicinal extract weight, add the purified water of 1.3 times of extract medicinal extract weight again, stir 15-30 minute, stratification 5 hours, reclaim organic phase, water layer adds the chloroform extraction twice of extract medicinal extract weight 1.5 times again, merges organic phase.Organic phase concentrating under reduced pressure reclaims trichloromethane, and obtain extract crude product 69.04 grams, in extract crude product, paclitaxel concentration is 1.70%.
Extract crude product is dissolved with the trichloromethane of 12 times of extract crude product weight in batches, dissolves completely for subsequent use.In alkali alumina (200-300 order) stationary phase post, first add methyl alcohol, trichloromethane draining successively, activate.Then be added in post by the trichloromethane being dissolved with extract crude product, the residence time is 40 minutes, drains.Then drain with trichloromethane drip washing, drain with mixing eluent (volume ratio 98.3:1.7) drip washing of trichloromethane and methyl alcohol.In the pillar that drip washing is good, add the mixtures of eluents (volume ratio 95.5:4.5) of trichloromethane and methyl alcohol again, collect elutriant.Repeat above step, merge elutriant, by the elutriant concentrating under reduced pressure merged, obtain extract work in-process 6.99 grams, in extract work in-process, paclitaxel concentration is 16.8%.
Used by extract work in-process the acetonitrile solution (the volume ratio 40:60 of acetonitrile and purified water) of 4 times of extract work in-process weight to dissolve in batches, dissolve completely for subsequent use.First by C
18-silicagel column acetonitrile fully washes out the impurity in stationary phase, then balances with the acetonitrile solution of volume ratio 40:60.Extract semi-finished product solution is added to C by the amount of 2.2mg taxol every gram of stationary phase
18in-silicagel column, then use the acetonitrile solution wash-out of volume ratio 50:50, collect elutriant.Repeat above step, merge elutriant, by the elutriant concentrating under reduced pressure crystallization at 50 DEG C merged, recrystallization is carried out with dissolve with ethanol again after filtering out crystallization, finally filter out crystallization and in 40 DEG C of vacuum-dryings, obtain highly purified extract 1.06 grams, in extract, paclitaxel concentration is 99.6%.
The Ramulus et folium taxi cuspidatae of drying is ground into 100 ~ 120 object powder, is conducive to the better extract of taxol, realizes optimum efficiency.With the taxol in the mixed solvent lixiviate Ramulus et folium taxi cuspidatae of 4 ~ 5 times of acetoneand ethyl acetates (volume ratio is 1:0.8 ~ 1), can obtain best extraction effect, the content of taxol in extract medicinal extract is the highest, and the weight of extract medicinal extract is minimum.With Ultrasonic Wave-Assisted Extraction, can extraction time be shortened, improve extraction effect.Extracting times is 3 times, can realize taxol and extract more completely.With alkali alumina stationary phase column chromatography extract crude product, a large amount of hydroaropic substances, lipid matter and 7-epi-taxol can be removed, taxol can obtain the purification of more than tens times simultaneously, and the rate of recovery of taxol can be greater than 100%, obtains the highest rate of recovery of taxol and purity.The residence time of extract crude product solution in alkali alumina stationary phase post is 30 ~ 40 minutes, 7-epi-taxol can be made constantly to be converted into taxol, also can prevent degradation of paclitaxel.Best drip washing effect can be obtained with the mixing eluent (volume ratio is 98:2 ~ 98.5:1.5) of trichloromethane and methyl alcohol.The best elute effect to taxol can be obtained by the mixtures of eluents (volume ratio is 95:5 ~ 96:4) of trichloromethane and methyl alcohol, realize the recovery that taxol is best.By extract work in-process C
18-silicagel column normal pressure reversed phase chromatography is refined, and can use simple operation step, just can obtain highly purified taxol.At C
18in-silicagel column reversed phase chromatography, each add-on of employing extract semi-finished product solution is the amount of 2 ~ 2.5mg taxol every gram of stationary phase, can obtain best refining effect.Highly purified extract can be applied in formulation for paclitaxel.
Compared with prior art, the plant milk extract the being applied to formulation for paclitaxel of the present invention feature that has that content of taxol is high, purity is high, impurity is few etc.The preparation method being applied to the plant milk extract of formulation for paclitaxel of the present invention has the features such as the taxol rate of recovery is high, extraction purification is easy and simple to handle, production cost is low, energy-conserving and environment-protective.
Claims (10)
1. one kind is applied to the plant milk extract of formulation for paclitaxel, it is characterized in that: described in be applied to formulation for paclitaxel plant milk extract with the Ramulus et folium taxi cuspidatae after drying and crushing for raw material, lixiviate is carried out with the mixed solvent of acetoneand ethyl acetate, extract medicinal extract is obtained after concentrating under reduced pressure, extract crude product is obtained after trichloromethane-water extraction is concentrated, through alkali alumina stationary phase column chromatography, then through C
18-silicagel column reversed phase chromatography, obtains finally by ethyl alcohol recrystallization.
2. the preparation method being applied to the plant milk extract of formulation for paclitaxel according to claim 1, is characterized in that: the method comprises the steps:
Step 1, cleans Ramulus et folium taxi cuspidatae, is ground into powder after cryodrying with pulverizer, carries out lixiviate, vat liquor is carried out concentrating under reduced pressure, recycling design, obtain extract medicinal extract with the mixed solvent of acetoneand ethyl acetate;
Step 2, dissolves extract medicinal extract trichloromethane, then adds purified water, stratification after stirring, and reclaims organic phase, water layer chloroform extraction, merges organic phase, organic phase concentrating under reduced pressure is reclaimed trichloromethane, obtains extract crude product;
Step 3, extract crude product trichloromethane is dissolved, join in the alkali alumina stationary phase post activated, drain, first drain with trichloromethane drip washing, then drain with the mixing eluent drip washing of trichloromethane and methyl alcohol, then use the mixtures of eluents wash-out of trichloromethane and methyl alcohol, by the elutriant concentrating under reduced pressure collected, obtain extract work in-process;
Extract work in-process are dissolved in acetonitrile solution by step 4, join the C balanced
18in-silicagel column, then use acetonitrile solution wash-out, by the elutriant concentrating under reduced pressure crystallization collected, the crystallization filtered out carries out recrystallization with dissolve with ethanol again, finally filters out crystallization, obtains highly purified extract after vacuum-drying.
3. the preparation method being applied to the plant milk extract of formulation for paclitaxel according to claim 2, is characterized in that: the temperature of cryodrying in described step 1 is 50 ~ 60 DEG C, and moisture content≤10% after dry, is ground into 100 ~ 120 object powder.
4. the preparation method being applied to the plant milk extract of formulation for paclitaxel according to claim 2, it is characterized in that: in described step 1, the weight of the mixed solvent of acetoneand ethyl acetate is 4 ~ 5 times of Ramulus et folium taxi cuspidatae powder, in mixed solvent, the volume ratio of acetoneand ethyl acetate is 1:0.8 ~ 1, lixiviate is carried out under ultrasonic assistant, extraction temperature is 35 ~ 45 DEG C, extraction time is 1 ~ 2 hour/time, and extracting times is 3 times.
5. the preparation method being applied to the plant milk extract of formulation for paclitaxel according to claim 2, is characterized in that: in described step 1, concentrating under reduced pressure temperature is 50 ~ 60 DEG C, and vacuum tightness is 0.07 ~ 0.09MPa.
6. the preparation method being applied to the plant milk extract of formulation for paclitaxel according to claim 2, it is characterized in that: for dissolving 1 ~ 2 times that the weight of the trichloromethane of extract medicinal extract is extract medicinal extract in described step 2, the weight of purified water is 1 ~ 1.5 times of extract medicinal extract, and the stratification time is 4 ~ 6 hours.
7. the preparation method being applied to the plant milk extract of formulation for paclitaxel according to claim 2, is characterized in that: be 1 ~ 2 times of extract medicinal extract for the weight of the trichloromethane of water layer extraction in described step 2, extraction times is 2 times.
8. the preparation method being applied to the plant milk extract of formulation for paclitaxel according to claim 2, it is characterized in that: for dissolving 10 ~ 15 times that the weight of the trichloromethane of extract crude product is extract crude product in described step 3, the residence time of extract crude product solution in alkali alumina stationary phase post is 30 ~ 40 minutes.
9. the preparation method being applied to the plant milk extract of formulation for paclitaxel according to claim 2, it is characterized in that: the volume ratio of the trichloromethane and methyl alcohol that mix eluent in described step 3 is 98:2 ~ 98.5:1.5, and the trichloromethane of mixtures of eluents and the volume ratio of methyl alcohol are 95:5 ~ 96:4.
10. the preparation method being applied to the plant milk extract of formulation for paclitaxel according to claim 2, it is characterized in that: be half-finished 3 ~ 5 times of extract for dissolving the weight of the half-finished acetonitrile solution of extract in described step 4, in acetonitrile solution, the volume ratio of acetonitrile and purified water is 40:60, the each add-on of extract semi-finished product solution is 2 ~ 2.5mg taxol every gram of stationary phase, and in the acetonitrile solution of wash-out, the volume ratio of acetonitrile and purified water is 50:50.
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| CN107365284A (en) * | 2017-08-16 | 2017-11-21 | 桂林茗兴生物科技有限公司 | A kind of method that taxol is extracted from Chinese yew |
| CN107382914A (en) * | 2017-08-16 | 2017-11-24 | 桂林茗兴生物科技有限公司 | The method that taxol is extracted from Chinese yew |
| CN110003143A (en) * | 2019-04-15 | 2019-07-12 | 云南汉德生物技术有限公司 | A method of extracting natural Japanese yew alcohol |
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| CN110003143A (en) * | 2019-04-15 | 2019-07-12 | 云南汉德生物技术有限公司 | A method of extracting natural Japanese yew alcohol |
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