CN105669602A - Method for efficiently and quickly extracting paclitaxel, cephalomannine and 10-DAB III from Taxus chinensis - Google Patents
Method for efficiently and quickly extracting paclitaxel, cephalomannine and 10-DAB III from Taxus chinensis Download PDFInfo
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- CN105669602A CN105669602A CN201610120547.4A CN201610120547A CN105669602A CN 105669602 A CN105669602 A CN 105669602A CN 201610120547 A CN201610120547 A CN 201610120547A CN 105669602 A CN105669602 A CN 105669602A
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- paclitaxel
- cephalomannine
- dab iii
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D305/00—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms
- C07D305/14—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms condensed with carbocyclic rings or ring systems
Abstract
The invention discloses a method for efficiently and quickly extracting paclitaxel, cephalomannine and 10-DAB III from Taxus chinensis. The method comprises the following steps: dissolving Taxus chinensis powder in a 10-DAB III extracting agent, carrying out primary ultrasonic extraction, carrying out centrifugal separation, collecting a centrifugal clear solution I, carrying out saturation adsorption on the centrifugal clear solution I through a macroporous resin, eluting while collecting the eluate I, concentrating the eluate I to obtain a 10-DAB III extract, carrying out secondary ultrasonic extraction on the centrifugal clear solution I treated by the macroporous resin, and collecting the filter residue and filtrate; and dissolving the filter residue collected in the step a in a paclitaxel extracting agent, carrying out ultrasonic extraction and centrifugal separation, collecting a centrifugal clear solution II, carrying out saturation adsorption on the centrifugal clear solution II through a macroporous resin, eluting while collecting the eluate II, and concentrating the eluate II to obtain the extract containing paclitaxel and cephalomannine. The method has the characteristics of simple preparation technique, simple production equipment, simple operation steps, short extraction time, recyclable materials, long service time and the like.
Description
Technical field
The present invention relates to the technical field of separation and Extraction effective ingredient from plant, be specifically related to a kind of method of efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae.
Background technology
Bearing taxanes is the compounds being extracted from the positions such as the bark of high gymnosperm Ramulus et folium taxi cuspidatae, root and leaf, mainly contain paclitaxel, Cephalomannine, 10-DAB III, 7-xylosyl taxol etc., many having been demonstrated is had to have cytotoxicity and anti-tumor activity, and it is used for extracting the natural Ramulus et folium taxi cuspidatae resource-constrained of paclitaxel etc., thus the production and supply of natural Japanese yew raw polyol medicine is restricted, the application that paclitaxel is clinical can not be met far away. Present people's implant mass Chinese yew, therefrom extracts the taxane substances such as paclitaxel, Cephalomannine, 10-DAB III, 7-xylosyl taxol, how to make full use of resource taxus resource, therefrom obtain more active substance significant. The method of existing extraction taxanes effective ingredient, such as " a kind of method of high efficiency extraction taxanes effective ingredient from Ramulus et folium taxi cuspidatae " patent that Authorization Notice No. is CN103408512B, the method of disclosed extraction taxanes effective ingredient is: first pass through water extraction, again through alcohol extraction, then purify with conventional purification methods and can obtain the taxane substances monomers such as paclitaxel, 10-DAB III, 7 xylosyl taxol, Cephalomannine be water-insoluble. The method main drawback is that 1. extraction time longer, at 4～48 hours; 2. containing a lot of fine particles in the filtrate after the filter plates of extracted tank bottom, enter resin column and can block resin column, reduce the recycling number of times of resin column; 3. organic monoacid aqueous solution is adopted to carry out extracting the step adding subsequent treatment organic monoacid aqueous solution.
Accordingly, it would be desirable to a kind of method of efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae, having preparation technology and production equipment and operating procedure is simple, extraction time is shorter, and material is capable of circulation, and uses the features such as time length.
Summary of the invention
In view of this, it is an object of the invention to provide a kind of method of efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae, have preparation technology and production equipment and operating procedure is simple, extraction time is shorter, material is capable of circulation, and uses the features such as time length.
The method of efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae of the present invention, comprises the following steps:
A. Ramulus et folium taxi cuspidatae powder is dissolved in after 10-DAB III extractant carries out supersound extraction and collects centrifugal clear liquid I through centrifugation, centrifugal clear liquid I carries out eluting collection eluent I after the saturated absorption of macroporous resin concentrate, obtaining 10-DAB III extractum, the centrifugal clear liquid I after macroporous resin treatment collects filtering residue and filtrate after supersound extraction;
B. the filtering residue collected in step a is dissolved in paclitaxel extractant and after first, after supersound extraction and centrifugation, collects centrifugal clear liquid II, centrifugal clear liquid II carries out eluting collection eluent II after the saturated absorption of macroporous resin concentrate, obtain the extractum containing paclitaxel, Cephalomannine;
Further, in step a, the mass volume ratio of Ramulus et folium taxi cuspidatae powder and 10-DAB III extractant is 1: 5～100;
Further, in step a, the supersonic frequency of first time supersound extraction is for for 20～50KHz, and extraction time is 2-6 hour;
Further, the filtrate after second time supersound extraction in step a is followed bad use as 10-DAB III extractant;
Further, in step a, described 10-DAB III extractant is water; Adopt concentration to be the methanol of 40～60% or the ethanol of 40～60% carries out eluting as eluant; The tube centrifuge that rotating speed is 6000～20000r/min is centrifuged separating treatment;
Further, in step b, according to the ratio that mass volume ratio is 1: 5～100 of Ramulus et folium taxi cuspidatae powder Yu paclitaxel extractant, adding paclitaxel extractant to filtering residue, described paclitaxel extractant is the ethanol of the methanol of concentration 20～50% or 20～50%;
Further, in step b, supersound extraction frequency is 20～50KHz, and the time is 2-6 hour;
Further, in step b, adopt concentration to be the methanol of 60～99.5% or the ethanol of 60～99.5% carries out eluting;
Further, in step b, in the tube centrifuge that rotating speed is 6000～20000r/min, it is centrifuged separating treatment obtains centrifugal clear liquid II; Centrifugal clear liquid II after macroporous resin treatment is collected filtrate after supersound extraction and is recycled as paclitaxel extractant;
Further, then undertaken drying in the shade by Taxus media branch and leaf is crushed to 0.1～2mm, just prepares Ramulus et folium taxi cuspidatae powder; 10-DAB III extractum in step a and the paclitaxel in step b, Cephalomannine extractum purification are prepared paclitaxel, Cephalomannine and 10-DAB III.
Beneficial effects of the present invention: the efficient rapid extraction paclitaxel from Ramulus et folium taxi cuspidatae of the present invention, the method of Cephalomannine and 10-DAB III, with Taxus media branch and leaf for raw material, the method that ultrasound wave is combined with resin absorption is adopted to extract paclitaxel respectively, Cephalomannine and 10-DAB III, the extraction ratio more than 98% of paclitaxel, Cephalomannine extraction ratio more than 98%, 10-DAB III extraction ratio more than 98%, 10-DAB III content 2%～5% in 10-DAB III extractum, paclitaxel, content of taxol 2%～5% in Cephalomannine extractum, Cephalomannine content 2%～5%, adopt this method extraction time short, efficiency is high, do not block resin column, extractant reusable edible, economizes on resources, environmental protection, the solvent recoverable adopted, environmental pollution is little. production equipment used by the inventive method is simple, and working condition is easily implemented, easy to operate applicable industrialized production.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described:
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
The method of efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae of the present invention, comprises the following steps:
A. Ramulus et folium taxi cuspidatae powder is dissolved in after 10-DAB III extractant carries out supersound extraction and collects centrifugal clear liquid I through centrifugation, centrifugal clear liquid I carries out eluting collection eluent I after the saturated absorption of macroporous resin concentrate, obtaining 10-DAB III extractum, the centrifugal clear liquid I after macroporous resin treatment collects filtering residue and filtrate after supersound extraction;
B. the filtering residue collected in step a is dissolved in paclitaxel extractant and after first, after supersound extraction and centrifugation, collects centrifugal clear liquid II, centrifugal clear liquid II carries out eluting collection eluent II after the saturated absorption of macroporous resin concentrate, obtain the extractum containing paclitaxel, Cephalomannine; The method that ultrasound wave is combined with resin absorption is adopted to extract paclitaxel, Cephalomannine and 10-DAB III respectively, the extraction ratio more than 98% of paclitaxel, Cephalomannine extraction ratio more than 98%, 10-DAB III extraction ratio more than 98%, 10-DAB III content 2%～5% in 10-DAB III extractum, content of taxol 2%～5%, Cephalomannine content 2%～5% in paclitaxel, Cephalomannine extractum, this method extraction time is short, efficiency is high, do not block resin column in employing. The macroporous resin of the present embodiment and following embodiment can adopt AB-8 or D101 or HPD300 macroporous resin.
In the present embodiment, in step a, the mass volume ratio of Ramulus et folium taxi cuspidatae powder and 10-DAB III extractant is 1: 5～100; The amount ratio of Ramulus et folium taxi cuspidatae powder and extractant ensure that the effect of extraction, increase the ratio of extraction ratio, the present embodiment and the Ramulus et folium taxi cuspidatae powder in the following embodiment quality that mass volume ratio is Ramulus et folium taxi cuspidatae powder (kg) with 10-DAB III extractant and the volume (L) of 10-DAB III extractant.
In the present embodiment, in step a, the first time supersonic frequency of supersound extraction is 20～50KHz, and extraction time is 2-6 hour; By suitable ultrasonic cavitation effect, heat effect and mechanism and in conjunction with centrifugation and macroporous resin adsorption, while improving extraction ratio, it is easy to again filter, it is to avoid blocking resin column, reduces the recycling number of times of resin column.
In the present embodiment, the filtrate after second time supersound extraction in step a is recycled as 10-DAB III extractant; As the extractant of next group material, can recycle with this, save Financial cost.
In the present embodiment, in step a, described 10-DAB III extractant is water; Adopt concentration to be the methanol of 40～60% or the ethanol of 40～60% carries out eluting as eluant; The tube centrifuge that rotating speed is 6000～20000r/min is centrifuged separating treatment; Extracting solution filter plate under supersound extraction tank enters in tube centrifuge after being filtered and is centrifuged, and obtains centrifugal clear liquid and precipitum, and precipitum is as Solid state fermentation; Eluant recycling use.
In the present embodiment, in step b, according to the ratio that mass volume ratio is 1: 5～100 of Ramulus et folium taxi cuspidatae powder Yu paclitaxel extractant, adding paclitaxel extractant to filtering residue, described paclitaxel extractant is the ethanol of the methanol of concentration 20～50% or 20～50%; The consumption of paclitaxel extractant is determined with reference to the proportion relation of Ramulus et folium taxi cuspidatae amount of powder that uses in step a, the amount ratio of paclitaxel extractant and filtering residue directly affects the extraction ratio of paclitaxel, Cephalomannine, and extracts the purity problem of paclitaxel, Cephalomannine.
In the present embodiment, in step b, supersound extraction frequency is 20～50KHz, and the time is 2-6 hour, the amount ratio of filtering residue and paclitaxel is in conjunction with supersonic frequency and ultrasonic time, it is effectively ensured paclitaxel, the extraction efficiency of Cephalomannine, in the present embodiment and above-described embodiment, Ramulus et folium taxi cuspidatae powder is excessive or too small with the consumption of extractant, ultrasonic frequency is excessive or too small, long or the too short extraction being all unfavorable for effective ingredient of ultrasonic time, such as, ultrasonic time is long, the dissolution of impurity can be caused, ultrasonic time is too short, affect again extraction ratio, supersonic frequency is excessive affects effective ingredient, the too small decline that can cause again extraction ratio of supersonic frequency, the present invention is exactly based on the consumption organically controlling Ramulus et folium taxi cuspidatae powder and extractant, the time of supersound extraction, and in conjunction with centrifugation and macroporous resin adsorption to reach to improve extraction ratio, ensure the purpose of the purity of effective ingredient.
In the present embodiment, in step b, adopt concentration to be the methanol of 60～99.5% or the ethanol of 60～99.5% carries out eluting.
In the present embodiment, in step b, in the tube centrifuge that rotating speed is 6000～20000r/min, it is centrifuged separating treatment obtains centrifugal clear liquid II; Centrifugal clear liquid II after macroporous resin treatment is collected filtrate after supersound extraction and is recycled as paclitaxel extractant.
In the present embodiment, then undertaken drying in the shade by Taxus media branch and leaf is crushed to 0.1～2mm, just prepares Ramulus et folium taxi cuspidatae powder; 10-DAB III extractum in step a and the paclitaxel in step b, Cephalomannine extractum purification are prepared paclitaxel, Cephalomannine and 10-DAB III. 10-DAB III extractum, paclitaxel, Cephalomannine extractum purification all adopt purification process of the prior art process all can realize the purpose of the present invention.
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment one
(1) extraction of 10-DAB III:
Undertaken drying in the shade by Taxus media branch and leaf and be then crushed to 0.1mm, just prepare Ramulus et folium taxi cuspidatae powder, by the quality (kg) of Ramulus et folium taxi cuspidatae powder: the ratio that ratio is 1: 5 of the volume (L) of 10-DAB III extractant (i.e. water), 10-DAB III extractant in Ramulus et folium taxi cuspidatae powder, then under the ul-trasonic irradiation that supersonic frequency is 20KHz, supersound extraction is carried out, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 6000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the macroporous resin column of AB-8, solution after absorption goes successively to extract in supersound extraction tank and is filtered, obtain filtrate and filtering residue, filtrate is as the extractant of next batch of material, filtering residue is placed in supersound extraction tank, resin column saturated rear eluant (i.e. the methanol of 40%) upon adsorption after absorption carries out eluting, collect eluent, resin eluant reuses after carrying out desorption, eluent concentrates, obtain the eluant of 10-DAB III extractum and recovery, the eluant circulation reclaimed utilizes, and in the present embodiment, the time of whole supersound extraction is 2 hours.
(2) extraction of paclitaxel and Cephalomannine
In the quality (kg) of the Ramulus et folium taxi cuspidatae powder that (1st) step prepares: the ratio that ratio is 1: 5 of the volume (L) of paclitaxel extractant (i.e. the methanol of 20%), equipped with the supersound extraction tank of filtering residue adds paclitaxel extractant in (1st) step, then under the ul-trasonic irradiation that supersonic frequency is 20KHz, supersound extraction is carried out, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 6000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in AB-8 resin column, solution after absorption enters and is again introduced in supersound extraction tank to be filtered after extraction, obtain filtrate and filtering residue, filtrate is as the extractant extracted next time, filtering residue is as Solid state fermentation,Resin column saturated rear eluant (i.e. the methanol of 60%) upon adsorption after absorption carries out eluting, collect eluent, resin eluant reuses after carrying out desorption, eluent concentrates, obtain the eluant containing paclitaxel, Cephalomannine extractum and recovery, the eluant circulation reclaimed utilizes, and in the present embodiment, the time of whole supersound process is 2 hours.
(3) process of extractum
10-DAB III extractum and paclitaxel, Cephalomannine extractum conventional purification methods purification can be obtained paclitaxel, Cephalomannine and 10-DAB III.
Embodiment two
(1) extraction of 10-DAB III:
Undertaken drying in the shade by Taxus media branch and leaf and be then crushed to 0.1mm, just prepare Ramulus et folium taxi cuspidatae powder, by the quality (kg) of Ramulus et folium taxi cuspidatae powder: the ratio that ratio is 1: 100 of the volume (L) of 10-DAB III extractant (i.e. water), 10-DAB III extractant in Ramulus et folium taxi cuspidatae powder, then under the ul-trasonic irradiation that supersonic frequency is 50KHz, supersound extraction is carried out, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 20000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the macroporous resin column of D101, solution after absorption goes successively in supersound extraction tank, the time of whole supersound extraction is 6 hours, then the material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant of next batch of material, filtering residue is placed in supersound extraction tank, resin column saturated rear eluant (i.e. the ethanol of 60%) upon adsorption after absorption carries out eluting, collecting eluent, resin eluant reuses after carrying out desorption, and eluent concentrates, obtaining the eluant of 10-DAB III extractum and recovery, the eluant circulation of recovery utilizes.
(2) extraction of paclitaxel and Cephalomannine
In the quality (kg) of the Ramulus et folium taxi cuspidatae powder that (1st) step prepares: the ratio that ratio is 1: 100 of the volume (L) of paclitaxel extractant (i.e. the ethanol of 50%), equipped with the supersound extraction tank of filtering residue adds paclitaxel extractant in (1st) step, then under the ul-trasonic irradiation that supersonic frequency is 50KHz, supersound extraction is carried out, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 20000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the resin column of D101, solution after absorption goes successively in supersound extraction tank and extracts, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant extracted next time, filtering residue is as Solid state fermentation, resin column saturated rear eluant (i.e. the ethanol of 99.5%) upon adsorption after absorption carries out eluting, collect eluent, resin eluant reuses after carrying out desorption, eluent concentrates, obtain the eluant containing paclitaxel, Cephalomannine extractum and recovery, the eluant circulation reclaimed utilizes, and in the present embodiment, the time of whole supersound extraction is 6 hours.
(3) process of extractum
10-DAB III extractum and paclitaxel, Cephalomannine extractum conventional purification methods purification can be obtained paclitaxel, Cephalomannine and 10-DAB III.
Embodiment three
(1) extraction of 10-DAB III:
Undertaken drying in the shade by Taxus media branch and leaf and be then crushed to 0.5mm, just prepare Ramulus et folium taxi cuspidatae powder;By the quality (kg) of Ramulus et folium taxi cuspidatae powder: the ratio that ratio is 1: 50 of the volume (L) of 10-DAB III extractant (i.e. water), 10-DAB III extractant in Ramulus et folium taxi cuspidatae powder, then under the ul-trasonic irradiation that supersonic frequency is 35KHz, supersound extraction is carried out, the total time of supersound process is 4 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 10000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the macroporous resin column of HPD300, solution after absorption enters and continues in supersound extraction tank to extract, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant of next batch of material, filtering residue is placed in supersound extraction tank, resin column saturated rear eluant (i.e. the methanol of 50%) upon adsorption after absorption carries out eluting, collecting eluent, resin eluant reuses after carrying out desorption, and eluent concentrates, obtaining the eluant of 10-DAB III extractum and recovery, the eluant circulation of recovery utilizes.
(2) extraction of paclitaxel and Cephalomannine
In the quality (kg) of the Ramulus et folium taxi cuspidatae powder that (1st) step prepares: the ratio that ratio is 1: 50 of the volume (L) of paclitaxel extractant (i.e. the methanol of 30%), equipped with the supersound extraction tank of filtering residue adds paclitaxel extractant in (1st) step, then under the ul-trasonic irradiation that supersonic frequency is 35KHz, supersound extraction is carried out 4 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 8000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the resin column of HPD300, solution after absorption enters and continues in supersound extraction tank to extract, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant extracted next time, filtering residue is as Solid state fermentation, resin column saturated rear eluant (i.e. the methanol of 70%) upon adsorption after absorption carries out eluting, collect eluent, resin eluant reuses after carrying out desorption, eluent concentrates, obtaining the eluant containing paclitaxel, Cephalomannine extractum and recovery, the eluant circulation of recovery utilizes.
(3) process of extractum
10-DAB III extractum and paclitaxel, Cephalomannine extractum conventional purification methods purification can be obtained paclitaxel, Cephalomannine and 10-DAB III.
Embodiment four
(1) extraction of 10-DAB III:
Undertaken drying in the shade by Taxus media branch and leaf and be then crushed to 1mm, just prepare Ramulus et folium taxi cuspidatae powder, by the quality (kg) of Ramulus et folium taxi cuspidatae powder: the ratio that ratio is 1: 25 of the volume (L) of 10-DAB III extractant (i.e. water), 10-DAB III extractant in Ramulus et folium taxi cuspidatae powder, then under the ul-trasonic irradiation that supersonic frequency is 25KHz, supersound extraction is carried out 3 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 7000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the macroporous resin column of AB-8, solution after absorption enters in supersound extraction tank and just extracts, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant of next batch of material, filtering residue is placed in supersound extraction tank, resin column saturated rear eluant (i.e. the ethanol of 48%) upon adsorption after absorption carries out eluting, collecting eluent, resin eluant reuses after carrying out desorption, and eluent concentrates, obtaining the eluant of 10-DAB III extractum and recovery, the eluant circulation of recovery utilizes.
(2) extraction of paclitaxel and Cephalomannine
In the quality (kg) of the Ramulus et folium taxi cuspidatae powder that (1st) step prepares: the ratio that ratio is 1: 80 of the volume (L) of paclitaxel extractant (i.e. the methanol of 40%), equipped with the supersound extraction tank of filtering residue adds paclitaxel extractant in (1st) step, then under the ul-trasonic irradiation that supersonic frequency is 45KHz, supersound extraction is carried out 3 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 15000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the resin column of HPD300, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant extracted next time, filtering residue is as Solid state fermentation, resin column saturated rear eluant (i.e. the methanol of 75%) upon adsorption after absorption carries out eluting, collect eluent, resin eluant reuses after carrying out desorption, eluent concentrates, obtaining the eluant containing paclitaxel, Cephalomannine extractum and recovery, the eluant circulation of recovery utilizes.
(3) process of extractum
10-DAB III extractum and paclitaxel, Cephalomannine extractum conventional purification methods purification can be obtained paclitaxel, Cephalomannine and 10-DAB III.
Embodiment five
(1) extraction of 10-DAB III:
Undertaken drying in the shade by Taxus media branch and leaf and be then crushed to 1.5mm, just prepare Ramulus et folium taxi cuspidatae powder, by the quality (kg) of Ramulus et folium taxi cuspidatae powder: the ratio that ratio is 1: 65 of the volume (L) of 10-DAB III extractant (i.e. water), 10-DAB III extractant in Ramulus et folium taxi cuspidatae powder, then under the ul-trasonic irradiation that supersonic frequency is 28KHz, supersound extraction is carried out 5 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 12000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the macroporous resin column of D101, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant of next batch of material, filtering residue is placed in supersound extraction tank, resin column saturated rear eluant (i.e. the ethanol of 45%) upon adsorption after absorption carries out eluting, collecting eluent, resin eluant reuses after carrying out desorption, and eluent concentrates, obtaining the eluant of 10-DAB III extractum and recovery, the eluant circulation of recovery utilizes.
(2) extraction of paclitaxel and Cephalomannine
In the quality (kg) of the Ramulus et folium taxi cuspidatae powder that (1st) step prepares: the ratio that ratio is 1: 12 of the volume (L) of paclitaxel extractant (i.e. the ethanol of 48%), equipped with the supersound extraction tank of filtering residue adds paclitaxel extractant in (1st) step, then under the ul-trasonic irradiation that supersonic frequency is 42KHz, supersound extraction is carried out 5 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 10800r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the resin column of HPD300, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant extracted next time, filtering residue is as Solid state fermentation, resin column saturated rear eluant (i.e. the ethanol of 99%) upon adsorption after absorption carries out eluting, collect eluent, resin eluant reuses after carrying out desorption, eluent concentrates, obtaining the eluant containing paclitaxel, Cephalomannine extractum and recovery, the eluant circulation of recovery utilizes.
(3) process of extractum
10-DAB III extractum and paclitaxel, Cephalomannine extractum conventional purification methods purification can be obtained paclitaxel, Cephalomannine and 10-DAB III.
Embodiment six
(1) extraction of 10-DAB III:
Undertaken drying in the shade by Taxus media branch and leaf and be then crushed to 0.8mm, just prepare Ramulus et folium taxi cuspidatae powder, by the quality (kg) of Ramulus et folium taxi cuspidatae powder: the ratio that ratio is 1: 65 of the volume (L) of 10-DAB III extractant (i.e. water), 10-DAB III extractant in Ramulus et folium taxi cuspidatae powder, then under the ul-trasonic irradiation that supersonic frequency is 32KHz, supersound extraction is carried out 3 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 18000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the macroporous resin column of D101, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant of next batch of material, filtering residue is placed in supersound extraction tank, resin column saturated rear eluant (i.e. the ethanol of 55%) upon adsorption after absorption carries out eluting, collecting eluent, resin eluant reuses after carrying out desorption, and eluent concentrates, obtaining the eluant of 10-DAB III extractum and recovery, the eluant circulation of recovery utilizes.
(2) extraction of paclitaxel and Cephalomannine
In the quality (kg) of the Ramulus et folium taxi cuspidatae powder that (1st) step prepares: the ratio that ratio is 1: 88 of the volume (L) of paclitaxel extractant (i.e. the ethanol of 50%), equipped with the supersound extraction tank of filtering residue adds paclitaxel extractant in (1st) step, then under the ul-trasonic irradiation that supersonic frequency is 30KHz, supersound extraction is carried out 3 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 15000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the resin column of D101, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant extracted next time, filtering residue is as Solid state fermentation, resin column saturated rear eluant (i.e. the ethanol of 60%) upon adsorption after absorption carries out eluting, collect eluent, resin eluant reuses after carrying out desorption, eluent concentrates, obtaining the eluant containing paclitaxel, Cephalomannine extractum and recovery, the eluant circulation of recovery utilizes.
(3) process of extractum
10-DAB III extractum and paclitaxel, Cephalomannine extractum conventional purification methods purification can be obtained paclitaxel, Cephalomannine and 10-DAB III.
Embodiment seven
(1) extraction of 10-DAB III:
Undertaken drying in the shade by Taxus media branch and leaf and be then crushed to 1.8mm, just prepare Ramulus et folium taxi cuspidatae powder, by the quality (kg) of Ramulus et folium taxi cuspidatae powder: the ratio that ratio is 1: 98 of the volume (L) of 10-DAB III extractant (i.e. water), 10-DAB III extractant in Ramulus et folium taxi cuspidatae powder, then under the ul-trasonic irradiation that supersonic frequency is 20～50KHz, supersound extraction is carried out 4 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 20000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the macroporous resin column of AB-8, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant of next batch of material, filtering residue is placed in supersound extraction tank,Resin column saturated rear eluant (i.e. the ethanol of 60%) upon adsorption after absorption carries out eluting, collecting eluent, resin eluant reuses after carrying out desorption, and eluent concentrates, obtaining the eluant of 10-DAB III extractum and recovery, the eluant circulation of recovery utilizes.
(2) extraction of paclitaxel and Cephalomannine
In the quality (kg) of the Ramulus et folium taxi cuspidatae powder that (1st) step prepares: the ratio that ratio is 1: 20 of the volume (L) of paclitaxel extractant (i.e. the ethanol of 50%), equipped with the supersound extraction tank of filtering residue adds paclitaxel extractant in (1st) step, then under the ul-trasonic irradiation that supersonic frequency is 50KHz, supersound extraction is carried out 4 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 6000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the resin column of AB-8, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant extracted next time, filtering residue is as Solid state fermentation, resin column saturated rear eluant (i.e. the ethanol of 80%) upon adsorption after absorption carries out eluting, collect eluent, resin eluant reuses after carrying out desorption, eluent concentrates, obtaining the eluant containing paclitaxel, Cephalomannine extractum and recovery, the eluant circulation of recovery utilizes.
(3) process of extractum
10-DAB III extractum and paclitaxel, Cephalomannine extractum conventional purification methods purification can be obtained paclitaxel, Cephalomannine and 10-DAB III.
Embodiment eight
(1) extraction of 10-DAB III:
Undertaken drying in the shade by Taxus media branch and leaf and be then crushed to 0.65mm, just prepare Ramulus et folium taxi cuspidatae powder, by the quality (kg) of Ramulus et folium taxi cuspidatae powder: the ratio that ratio is 1: 10 of the volume (L) of 10-DAB III extractant (i.e. water), 10-DAB III extractant in Ramulus et folium taxi cuspidatae powder, then under the ul-trasonic irradiation that supersonic frequency is 20～50KHz, supersound extraction is carried out 2 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 20000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the macroporous resin column of HPD300, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant of next batch of material, filtering residue is placed in supersound extraction tank, resin column saturated rear eluant (i.e. the ethanol of 55%) upon adsorption after absorption carries out eluting, collecting eluent, resin eluant reuses after carrying out desorption, and eluent concentrates, obtaining the eluant of 10-DAB III extractum and recovery, the eluant circulation of recovery utilizes.
(2) extraction of paclitaxel and Cephalomannine
In the quality (kg) of the Ramulus et folium taxi cuspidatae powder that (1st) step prepares: the ratio that ratio is 1: 70 of the volume (L) of paclitaxel extractant (i.e. the ethanol of 45%), equipped with the supersound extraction tank of filtering residue adds paclitaxel extractant in (1st) step, then under the ul-trasonic irradiation that supersonic frequency is 25KHz, supersound extraction is carried out 3 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 6000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the resin column of HPD300, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant extracted next time, filtering residue is as Solid state fermentation,Resin column saturated rear eluant (i.e. the ethanol of 80%) upon adsorption after absorption carries out eluting, collect eluent, resin eluant reuses after carrying out desorption, eluent concentrates, obtaining the eluant containing paclitaxel, Cephalomannine extractum and recovery, the eluant circulation of recovery utilizes.
(3) process of extractum
10-DAB III extractum and paclitaxel, Cephalomannine extractum conventional purification methods purification can be obtained paclitaxel, Cephalomannine and 10-DAB III.
Embodiment nine
(1) extraction of 10-DAB III:
Undertaken drying in the shade by Taxus media branch and leaf and be then crushed to 0.7mm, just prepare Ramulus et folium taxi cuspidatae powder, by the quality (kg) of Ramulus et folium taxi cuspidatae powder: the ratio that ratio is 1: 44 of the volume (L) of 10-DAB III extractant (i.e. water), 10-DAB III extractant in Ramulus et folium taxi cuspidatae powder, then under the ul-trasonic irradiation that supersonic frequency is 50KHz, supersound extraction is carried out 3 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 20000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the macroporous resin column of AB-8, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant of next batch of material, filtering residue is placed in supersound extraction tank, resin column saturated rear eluant (i.e. the methanol of 60%) upon adsorption after absorption carries out eluting, collecting eluent, resin eluant reuses after carrying out desorption, and eluent concentrates, obtaining the eluant of 10-DAB III extractum and recovery, the eluant circulation of recovery utilizes.
(2) extraction of paclitaxel and Cephalomannine
In the quality (kg) of the Ramulus et folium taxi cuspidatae powder that (1st) step prepares: the ratio that ratio is 1: 100 of the volume (L) of paclitaxel extractant (i.e. the methanol of 50%), equipped with the supersound extraction tank of filtering residue adds paclitaxel extractant in (1st) step, then under the ul-trasonic irradiation that supersonic frequency is 20KHz, supersound extraction is carried out 2 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 6000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the resin column of AB-8, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant extracted next time, filtering residue is as Solid state fermentation, resin column saturated rear eluant (i.e. the methanol of 99.5%) upon adsorption after absorption carries out eluting, collect eluent, resin eluant reuses after carrying out desorption, eluent concentrates, obtaining the eluant containing paclitaxel, Cephalomannine extractum and recovery, the eluant circulation of recovery utilizes.
(3) process of extractum
10-DAB III extractum and paclitaxel, Cephalomannine extractum conventional purification methods purification can be obtained paclitaxel, Cephalomannine and 10-DAB III.
Embodiment ten
(1) extraction of 10-DAB III:
Undertaken drying in the shade by Taxus media branch and leaf and be then crushed to 1.2mm, just prepare Ramulus et folium taxi cuspidatae powder, by the quality (kg) of Ramulus et folium taxi cuspidatae powder: the ratio that ratio is 1: 70 of the volume (L) of 10-DAB III extractant (i.e. water), 10-DAB III extractant in Ramulus et folium taxi cuspidatae powder, then under the ul-trasonic irradiation that supersonic frequency is 20KHz, supersound extraction is carried out 5 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 20000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the macroporous resin column of AB-8, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant of next batch of material, filtering residue is placed in supersound extraction tank,Resin column saturated rear eluant (i.e. the methanol of 50%) upon adsorption after absorption carries out eluting, collecting eluent, resin eluant reuses after carrying out desorption, and eluent concentrates, obtaining the eluant of 10-DAB III extractum and recovery, the eluant circulation of recovery utilizes.
(2) extraction of paclitaxel and Cephalomannine
In the quality (kg) of the Ramulus et folium taxi cuspidatae powder that (1st) step prepares: the ratio that ratio is 1: 60 of the volume (L) of paclitaxel extractant (i.e. the ethanol of 50%), equipped with the supersound extraction tank of filtering residue adds paclitaxel extractant in (1st) step, then under the ul-trasonic irradiation that supersonic frequency is 30KHz, supersound extraction is carried out 4 hours, extracting solution filter plate under supersound extraction tank enters in the tube centrifuge that rotating speed is 20000r/min after being filtered and is centrifuged, obtain centrifugal clear liquid and precipitum, precipitum is as Solid state fermentation, centrifugal clear liquid enters and adsorbs equipped with in the resin column of AB-8, solution after absorption enters in supersound extraction tank and continues with, material in supersound extraction tank is filtered, obtain filtrate and filtering residue, filtrate is as the extractant extracted next time, filtering residue is as Solid state fermentation, resin column saturated rear eluant (i.e. the ethanol of 99.5%) upon adsorption after absorption carries out eluting, collect eluent, resin eluant reuses after carrying out desorption, eluent concentrates, obtaining the eluant containing paclitaxel, Cephalomannine extractum and recovery, the eluant circulation of recovery utilizes.
(3) process of extractum
10-DAB III extractum and paclitaxel, Cephalomannine extractum conventional purification methods purification can be obtained paclitaxel, Cephalomannine and 10-DAB III.
What finally illustrate is, above example is only in order to illustrate technical scheme and unrestricted, although the present invention being described in detail with reference to preferred embodiment, it will be understood by those within the art that, technical scheme can be modified or equivalent replacement, without deviating from objective and the scope of technical solution of the present invention, it all should be encompassed in the middle of scope of the presently claimed invention.
Claims (10)
1. the method for efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae, it is characterised in that: comprise the following steps:
A. Ramulus et folium taxi cuspidatae powder is dissolved in after 10-DAB III extractant carries out supersound extraction and collects centrifugal clear liquid I through centrifugation, centrifugal clear liquid I carries out eluting collection eluent I after the saturated absorption of macroporous resin concentrate, obtaining 10-DAB III extractum, the centrifugal clear liquid I after macroporous resin treatment collects filtering residue and filtrate after supersound extraction;
B. the filtering residue collected in step a is dissolved in paclitaxel extractant and after first, after supersound extraction and centrifugation, collects centrifugal clear liquid II, centrifugal clear liquid II carries out eluting collection eluent II after the saturated absorption of macroporous resin concentrate, obtain the extractum containing paclitaxel, Cephalomannine.
2. the method for efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae according to claim 1, it is characterised in that: in step a, the mass volume ratio of Ramulus et folium taxi cuspidatae powder and 10-DAB III extractant is 1: 5～100.
3. the method for efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae according to claim 2, it is characterised in that: in step a, the supersonic frequency of supersound extraction is 20～50KHz, and extraction time is 2-6 hour.
4. the method for efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae according to claim 3, it is characterised in that: filtrate in step a is recycled as 10-DAB III extractant.
5. the method for efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae according to claim 1, it is characterised in that: in step a, described 10-DAB III extractant is water; Adopt concentration to be the methanol of 40～60% or the ethanol of 40～60% carries out eluting as eluant; The tube centrifuge that rotating speed is 6000～20000r/min is centrifuged separating treatment.
6. the method for efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae according to claim 1, it is characterized in that: in step b, the ratio that mass volume ratio is 1: 5～100 according to Ramulus et folium taxi cuspidatae powder Yu paclitaxel extractant, adding paclitaxel extractant to filtering residue, described paclitaxel extractant is the ethanol of the methanol of concentration 20～50% or 20～50%.
7. the method for efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae according to claim 6, it is characterised in that: in step b, supersound extraction frequency is 20～50KHz, and extraction time is 2-6 hour.
8. the method for efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae according to claim 7, it is characterised in that: in step b, adopt concentration to be the methanol of 60～99.5% or the ethanol of 60～99.5% carries out eluting.
9. the method for efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae according to claim 1, it is characterized in that: in step b, in the tube centrifuge that rotating speed is 6000～20000r/min, be centrifuged separating treatment obtain centrifugal clear liquid II; Centrifugal clear liquid II after macroporous resin treatment is collected filtrate after ultrasonic and is recycled as paclitaxel extractant.
10. the method for efficient rapid extraction paclitaxel, Cephalomannine and 10-DAB III from Ramulus et folium taxi cuspidatae according to claim 1, it is characterised in that: then undertaken drying in the shade by Taxus media branch and leaf is crushed to 0.1～2mm, just prepares Ramulus et folium taxi cuspidatae powder; 10-DAB III extractum in step a and the paclitaxel in step b, Cephalomannine extractum purification are prepared paclitaxel, Cephalomannine and 10-DAB III.
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| CN113845496A (en) * | 2021-10-12 | 2021-12-28 | 华中科技大学 | Method for synchronously and efficiently separating various taxanes |
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