CN104739908A - Acanthopanax senticosus extract and preparation method thereof - Google Patents
Acanthopanax senticosus extract and preparation method thereof Download PDFInfo
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- CN104739908A CN104739908A CN201310744469.1A CN201310744469A CN104739908A CN 104739908 A CN104739908 A CN 104739908A CN 201310744469 A CN201310744469 A CN 201310744469A CN 104739908 A CN104739908 A CN 104739908A
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Abstract
The invention relates to a preparation method of an acanthopanax senticosus extract, and the acanthopanax senticosus extract prepared by the preparation method and a preparation comprising the acanthopanax senticosus extract. The preparation method comprises the following steps: acanthopanax senticosus water decocted extract paste prepared by water extract of an acanthopanax senticosus medicinal material is precipitated by alcohol, then pass through macroporous resin for adsorption and elution, eluent is concentrated, then again precipitated by alcohol, and is refined to obtain the acanthopanax senticosus extract; the refining method comprises use of DM1180 resin for adsorption, elution and secondary ultrafiltration of the eluent. The method provided by the invention can significantly reduce the content of impurities and especially nonpolar invalid impurities in the acanthopanax senticosus extract, improve the purity of effective components in the acanthopanax senticosus extract and security and stability of the acanthopanax senticosus extract, can reduce energy consumption, greatly improves the extract yield, is superior in effect compared with the method in the prior art, and has great application prospect and market value.
Description
Technical field
The present invention relates to medicinal plants and extract field, particularly, relate to a kind of preparation method of Radix Et Caulis Acanthopanacis Senticosi extract, and the Radix Et Caulis Acanthopanacis Senticosi extract obtained by this preparation method and comprise the preparation of this Radix Et Caulis Acanthopanacis Senticosi extract.
Background technology
Radix Et Caulis Acanthopanacis Senticosi is dry root welding technology or the stem of Araliaceae Radix Et Caulis Acanthopanacis Senticosi Acanthopanax senticosus (Rupr.etMaxim.) Harms.There is replenishing QI to invigorate the spleen, effect of tonifying the kidney for tranquilization.Property pungent, micro-hardship, temperature.For deficiency of both the splenic and pulmonary QI, body void is weak, inappetence, deficiency of both the lung and kidney, chronic cough dyspnea due to deficiency, soreness of waist and knee joint of suffering from a deficiency of the kidney, deficiency of both the heart and spleen, insomnia and dreamful sleep.
Main active in Radix Et Caulis Acanthopanacis Senticosi is flavone, saponins and polysaccharide, and what glycoside content was the highest is syringoside and eleutheroside E.In recent years, the existing more research about Radix Et Caulis Acanthopanacis Senticosi extract method, target improves the content of total flavones, syringoside and eleutheroside E in Radix Et Caulis Acanthopanacis Senticosi, reduces the content of the impurity such as macromole, to improve the effectiveness and reliability of Acanthopanax preparations.
Chinese patent ZL200710117640.0(title: a kind of method preparing acanthopanax senticousus extracting liquid/extraction, publication number: CN101084953A, publication date: on December 12nd, 2007) disclose a kind of method preparing acanthopanax senticousus extracting liquid/extraction, the method comprises the steps: 1) adopt decoction and alcohol sedimentation technique to prepare Radix Et Caulis Acanthopanacis Senticosi drug extract; 2) by extractum thin up, regulate pH to 10.00 ~ 12.00 with lime cream, with sulfur acid for adjusting pH to 4.5 ~ 6.5 after stirring, leave standstill, extract supernatant liquid filtering, concentrated, precipitate with ethanol; 3) cold preservation leaves standstill remove impurity, obtains acanthopanax senticosus extract; Or concentrated drying under reduced pressure obtains Radix Et Caulis Acanthopanacis Senticosi extract.
Chinese patent ZL201010165556.8(title: a kind of Radix Et Caulis Acanthopanacis Senticosi extract and pharmaceutical composition thereof, publication number: CN101810656A, publication date: on August 25th, 2010) disclose a kind of Radix Et Caulis Acanthopanacis Senticosi extract and pharmaceutical composition thereof, this Radix Et Caulis Acanthopanacis Senticosi extract be by Radix Et Caulis Acanthopanacis Senticosi through water extract-alcohol precipitation, lime cream adjust pH to 10.0 ~ 12.0, leave standstill more than 4 hours, sulphuric acid tune pH to 5.0 ~ 6.0, again precipitate with ethanol after obtain.
Chinese patent ZL201210049755.1(title: a kind of acanthopanax combination, containing its preparation and detection method thereof, publication number: CN102579532A, publication date: on 07 18th, 2012) disclose a kind of preparation method of acanthopanax combination, the method comprises the steps: that Radix Et Caulis Acanthopanacis Senticosi is adjusted pH to 10.0 ~ 12.0, sulphuric acid adjust ph to 5.0 ~ 6.0, precipitate with ethanol through water extraction, lime cream, leave standstill more than 12 hours, concentrate and get final product.
Chinese patent ZL200810136879.7(title: high-purity syringin, preparation method and application, publication number: CN101643484A, publication date: on February 10th, 2010) provide a kind of preparation method and application of high-purity syringin, the method comprises the following steps: dissolve Radix Et Caulis Acanthopanacis Senticosi cream, macroporous adsorption resin chromatography, decolouring, macroporous adsorption resin chromatography, alcohol crystal or recrystallization, obtain highly purified syringoside.In this patent, resin is front without precipitate with ethanol, macroporous resin is carried and increases the weight of, affect purification effect.
Chinese patent ZL200710301682.X(title: the extract of acanthopanax senticosus effective fraction, its preparation method, its application, publication number: CN101214270A, publication date: on July 9th, 2008) disclose a kind of preparation method of extract of acanthopanax senticosus effective fraction: Radix Et Caulis Acanthopanacis Senticosi aqueous extract is dissolved, pH is adjusted to be 2 ~ 9, adsorbed by low pole or nonpolar macroporous adsorption resin chromatographic column, by water or the organic solvent eluting of low concentration that can mix with arbitrary proportion with water.The method is easy purification process, effectively can not remove the impurity such as macromole.
Chinese patent ZL02125536.9(title: manyprickle acanthopanax general saponin extractive and pharmaceutical composition thereof, publication number: CN1468860A, publication date: on January 21st, 2004) disclose a kind of method of Radix Et Caulis Acanthopanacis Senticosi total saponins abstract, the method comprises first with the lime cream that CaO makes, and is alkalescence by the water decoction furnishing pH value of Radix Et Caulis Acanthopanacis Senticosi; Then Radix Et Caulis Acanthopanacis Senticosi filtrate is made to be adsorbed by macroporous adsorptive resins and use ethanol elution under conditions of neutral ph; Finally make obtained eluate by weak acid ion exchange resin again and carry out routine decolouring.The method is applicable to desolventing technology, relatively poor to going deimpurity effect, and in decolorization, produce certain content loss.
Chinese patent application 03133441.5(title: the production technology manufacturing freeze-dried wilsonii powder for injection, publication number: CN1565535A, publication date: on January 19th, 2005) disclose a kind of production technology of freeze-dried wilsonii powder for injection, its extracting method comprises the following steps: alcohol reflux Caulis Et Caulis Acanthopanacis Senticosi, filter, reclaim under reduced pressure to relative density is that 1.02 ~ 1.03(20 ~ 30 DEG C are surveyed) aqueous solution, leave standstill 24 hours, filter.By filtrate by being equipped with the AB-8 type macroporous adsorptive resins handled well, eluting, collect eluent, being evaporated to relative density is that 1.04 ~ 1.06(50 ~ 60 DEG C are surveyed) solution, carries out spraying dry by this solution, obtains fine powder.The method is easy purification process, effectively can not remove the impurity such as macromole.
Great majority are all the macromolecular compounds removing instability a large amount of in extract about the research of Radix Et Caulis Acanthopanacis Senticosi, as tannin, resin, pigment etc., and the oxidizable decomposition of these macromolecular compounds, this is also one of reason causing Radix Et Caulis Acanthopanacis Senticosi extract and preparation instability thereof.In prior art, utilize DM1180 resin to yet there are no report to the research preparing Radix Et Caulis Acanthopanacis Senticosi extract, if corresponding technology can be developed, huge application prospect and economic worth certainly will be had.
Summary of the invention
In order to solve the problems of the technologies described above, the object of the invention is to, a kind of preparation method of Radix Et Caulis Acanthopanacis Senticosi extract is provided.The method significantly can reduce the content of impurity in Radix Et Caulis Acanthopanacis Senticosi extract, improves the purity of effective ingredient and the safety and stability of Radix Et Caulis Acanthopanacis Senticosi extract in Radix Et Caulis Acanthopanacis Senticosi extract.
Another object of the present invention is to, the Radix Et Caulis Acanthopanacis Senticosi extract prepared by described method is provided.
Another object of the present invention is, providing package is containing the preparation of described Radix Et Caulis Acanthopanacis Senticosi extract.
The preparation method of Radix Et Caulis Acanthopanacis Senticosi extract provided by the invention, comprising: with water extraction Radix Et Caulis Acanthopanacis Senticosi medical material, the Radix Et Caulis Acanthopanacis Senticosi herbal decoction obtained is after precipitate with ethanol, cross that macroporous resin carries out adsorbing, eluting, eluent precipitate with ethanol again after concentrated, and then through refining, obtain Radix Et Caulis Acanthopanacis Senticosi extract;
Described refining method comprises: with DM1180 resin carry out adsorbing, eluting, eluent is again through two-stage ultrafiltering.
The preparation method of Radix Et Caulis Acanthopanacis Senticosi extract provided by the invention, comprises the steps:
(1) with water extraction Radix Et Caulis Acanthopanacis Senticosi medical material, extracting solution, through concentrated, obtains Radix Et Caulis Acanthopanacis Senticosi herbal decoction;
(2) the Radix Et Caulis Acanthopanacis Senticosi herbal decoction that obtains of step (1) is through precipitate with ethanol, concentrated, obtains Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream;
(3) Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream of obtaining of step (2) is after dilution, crosses that macroporous resin carries out adsorbing, eluting, and concentrate eluant, obtains condensed cream;
(4) condensed cream that obtains of step (3) is through secondary precipitate with ethanol, concentrated, obtains Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream;
(5) Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream step (4) obtained after dilution, then through refining, obtains Radix Et Caulis Acanthopanacis Senticosi extract;
Described refining method comprises: the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream after dilution, crosses that DM1180 resin carries out adsorbing, eluting, and eluent through two-stage ultrafiltering, then concentrates, and to obtain final product.
Described DM1180 resin is non-polar macroporous resin, is also a kind of phenylethylene resin series, and specific surface area is 400 ~ 500m
2/ g, average pore size is 100 ~ 110A °.
Wherein, in step (3), the model of described macroporous resin can be ADS-F8, ADS-17, HPD750, D101, HPD100, HPD450, AB-8 or DM130, preferred ADS-F8, D101 or HPD100.
Wherein, in step (5), described refining method comprises:
Get the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream after dilution appropriate, filter, filtrate adjust pH 4.0 ~ 5.5, sterilizing, cold preservation, the medicinal liquid after cold preservation through filtering with microporous membrane clarification after, adjust pH 4.6 ~ 5.0, filtrate is crossed DM1180 resin and is adsorbed, use 1 ~ 2 times of column volume purified water eluting again, collect eluent, adjust pH 5.3 ~ 5.7, sterilizing, cold preservation; Medicinal liquid after cold preservation is after filtering with microporous membrane clarification, and successively carry out the two-stage ultrafiltering of 100,000,30,000 grades, it is 1.11 ~ 1.14(80 DEG C of survey that filtrate is concentrated into relative density), to obtain final product.
Wherein, in the process for purification of step (5), filtrate is crossed DM1180 resin and is adsorbed, and upper prop liquid (namely crossing the filtrate of DM1180) is (6 ~ 15) with the volume ratio of resin: 1.
Wherein, in the process for purification of step (5), with 1 ~ 2 times of column volume purified water eluting, elution flow rate is 2 ~ 4BV/h.
Wherein, in the process for purification of step (5), sterilizing (sterilizing of two places) condition is: 115 ~ 121 DEG C of sterilizings 30 ~ 40 minutes.
Wherein, in the process for purification of step (5), cold preservation (cold preservation of the two places) time is more than 12 hours, all preferably 12 ~ 18 hours.
Particularly, the preparation method of Radix Et Caulis Acanthopanacis Senticosi extract provided by the invention, comprises the following steps:
(1) extract: with the water extraction Radix Et Caulis Acanthopanacis Senticosi medical material 2 ~ 3 times of 6 ~ 12 volume times amount, extract 1 ~ 2 hour, merge extractive liquid, at every turn, concentrate, obtain Radix Et Caulis Acanthopanacis Senticosi herbal decoction, for subsequent use;
(2) precipitate with ethanol: under agitation, the Radix Et Caulis Acanthopanacis Senticosi herbal decoction obtained to step (1) with more than 93% ethanol mix, abundant stirring, leave standstill more than 6 hours, filter, filtrate recycling ethanol is to without alcohol taste, and to be concentrated into relative density be 1.11 ~ 1.14(80 DEG C of survey), obtain Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream, for subsequent use;
(3) macroporous resin adsorption: get Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream that step (2) obtains appropriate, being diluted to general flavone content with water for injection is 7.5 ~ 10.0mg/ml, after stirring, filter, filtrate adjust pH 4.0 ~ 5.5, stirs, cold preservation more than 12 hours; Medicinal liquid after cold preservation through filtering with microporous membrane clarification after, adjust pH 2.0 ± 0.2, filtrate with macroporous resin column on 1.5 ~ 2BV/h flow velocity, then with same flow velocity (1.5 ~ 2BV/h) 0.3 ~ 0.5 times of column volume purified water eluting, collection eluent, for subsequent use; Then use 50% ethanol elution of 4 ~ 6 volume times amount, collect eluent, adjust pH to be 5.5,50% eluent being concentrated into relative density is 1.11 ~ 1.14(80 DEG C of survey), obtain condensed cream, for subsequent use;
(4) secondary precipitate with ethanol: under agitation, more than 93% ethanol is added in the condensed cream that step (3) obtains, stir, leave standstill more than 12 hours, leaching supernatant (residue medicinal residues centrifugal rear cross leaching supernatant), filtrate recycling ethanol is to without alcohol taste, and to be concentrated into relative density be 1.11 ~ 1.14(80 DEG C of survey), obtain Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream (i.e. Radix Et Caulis Acanthopanacis Senticosi extract A), for subsequent use;
(5) DM1180 resin elution and two-stage ultrafiltering: get the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream (i.e. Radix Et Caulis Acanthopanacis Senticosi extract A) that step (4) obtains appropriate, being diluted to general flavone content with water for injection is 6 ~ 15mg/ml, filter, filtrate adjust pH 4.0 ~ 5.5,115 ~ 121 DEG C of sterilizings 30 ~ 40 minutes, cold preservation more than 12 hours;
Medicinal liquid after cold preservation is after filtering with microporous membrane clarification, adjust pH 4.6 ~ 5.0, filtrate is crossed DM1180 resin and is adsorbed, use the purified water eluting of 1 ~ 2 times of column volume again, elution flow rate is 2 ~ 4BV/h, collects eluent, adjust pH 5.3 ~ 5.7,115 ~ 121 DEG C of sterilizings 30 ~ 40 minutes, cold preservation more than 12 hours; Medicinal liquid after cold preservation is after filtering with microporous membrane clarification, and successively carry out the two-stage ultrafiltering of 100,000,30,000 grades, it is 1.11 ~ 1.14(80 DEG C of survey that filtrate is concentrated into relative density), obtain (obtaining Radix Et Caulis Acanthopanacis Senticosi extract B).
In step (2), concentration of alcohol preferably 93 ~ 95%, makes alcohol content reach 74.5 ~ 75.5%.
In step (2), time of repose preferably 6 ~ 18 hours.
In step (3), cold preservation time preferably 12 ~ 18 hours.
In step (3) and step (5), the pH value of purified water is 3.0.
In step (4), concentration of alcohol preferably 93 ~ 95%, makes alcohol content reach 84.5 ~ 85.5%.
In step (4), after adding more than 93% ethanol, stir 15 minutes.
In step (4), cold preservation time preferably 12 ~ 16 hours.
In step (5), all preferably 12 ~ 18 hours cold preservation (cold preservation of two places) time.
In step (5), filtrate is crossed DM1180 resin and is adsorbed, and upper prop liquid (namely crossing the filtrate of DM1180) is (6 ~ 15) with the volume ratio of resin: 1.
In above-mentioned preparation method, the aperture of microporous filter membrane used is 0.45 μm.
Present invention also offers the Radix Et Caulis Acanthopanacis Senticosi extract prepared by described method.
Containing total flavones 60 ~ 75mg/g, syringoside 7.0 ~ 8.5mg/g and eleutheroside E 4.5 ~ 7.0mg/g in described Radix Et Caulis Acanthopanacis Senticosi extract.
Preferably, total flavones 60 ~ 68mg/g, syringoside 7.2 ~ 7.8mg/g and eleutheroside E 4.9 ~ 6.3mg/g is contained in described Radix Et Caulis Acanthopanacis Senticosi extract.Here Radix Et Caulis Acanthopanacis Senticosi extract refers to above-mentioned Radix Et Caulis Acanthopanacis Senticosi extract B.
Present invention also offers the preparation comprising above-mentioned Radix Et Caulis Acanthopanacis Senticosi extract.
The preparation comprising above-mentioned Radix Et Caulis Acanthopanacis Senticosi extract can be made up of separately Radix Et Caulis Acanthopanacis Senticosi extract, also can be made up of above-mentioned Radix Et Caulis Acanthopanacis Senticosi extract and pharmaceutically acceptable carrier or diluent.
Described pharmaceutically acceptable carrier or diluent are the conventional material of this area.
Described preparation is injection type, comprising: the little aqueous injection of Radix Et Caulis Acanthopanacis Senticosi, Radix Et Caulis Acanthopanacis Senticosi lyophilized preparation or Radix Et Caulis Acanthopanacis Senticosi injection.
Containing total flavones 3 ~ 6.5mg/ml, syringoside 0.2 ~ 2.2mg/ml and eleutheroside E 0.1 ~ 1.0mg/ml in described Ci Wu Jia type.
Preferably, total flavones 5.25 ~ 5.46mg/ml, syringoside 0.38 ~ 0.47mg/ml and eleutheroside E 0.20 ~ 035mg/ml is contained in the little aqueous injection of described Radix Et Caulis Acanthopanacis Senticosi.
Preferably, total flavones 5.05 ~ 5.15mg/ml, syringoside 0.35 ~ 0.45mg/ml and eleutheroside E 0.15 ~ 0.25mg/ml is contained in described Radix Et Caulis Acanthopanacis Senticosi lyophilized preparation.
Preferably, total flavones 3.05 ~ 3.20mg/ml, syringoside 0.20 ~ 0.35mg/ml and eleutheroside E 0.15 ~ 0.20mg/ml is contained in described Radix Et Caulis Acanthopanacis Senticosi injection.
The method that the present invention prepares Radix Et Caulis Acanthopanacis Senticosi extract has the following advantages:
(1) DM1180 macroporous adsorbent resin is nonpolar macroporous adsorbent, be suitable for the separation and Extraction of medium molecule organic compound, the unstable macromolecular substances of main removal is as tannin, resin residue thing, pigment etc., effective, extract yield promotes greatly, and improves the content of effective ingredient, ensure that the stability of the preparation comprising Radix Et Caulis Acanthopanacis Senticosi extract of the present invention, pH value change is less, and easy to operate.
(2) DM1180 macroporous adsorbent resin physicochemical property is stablized, the process of acid and alkali resistance and organic solvent, has larger specific surface area and intermediate pore size, can bear the temperature of less than 150 DEG C and not destroy.
(3), in the preparation method of Radix Et Caulis Acanthopanacis Senticosi extract of the present invention, adopt step (3) described macroporous adsorbent resin and DM1180 resin use in conjunction, the while of active constituent-enriched, remove invalid impurity to greatest extent.
(4) in the preparation method of Radix Et Caulis Acanthopanacis Senticosi extract of the present invention, process for purification also comprises two-stage ultrafiltering, it is advantageous that macromolecular substances is removed in segmentation, improves the safety comprising the preparation of gained Radix Et Caulis Acanthopanacis Senticosi extract, reduce loss of effective components, extend ultrafilter membrane service life.
(5) preparation method of many Radix Et Caulis Acanthopanacis Senticosi extracts uses stone sulphuring treatment, and the present invention utilizes resin to substitute stone sulphuring treatment step, effectively can improve effective ingredient purity in finished product, also can remove the inorganic salt that a large amount of impact comprises the preparation security of gained Radix Et Caulis Acanthopanacis Senticosi extract simultaneously.
(6) the present invention's material used (as resin, ultrafilter membrane) all can reuse, and not only can improve the quality of products, and can reduce resource consumption.
(7) the present invention is good through the purification effect of ethanol precipitation twice.
In a word, method provided by the invention, significantly can reduce the content of impurity in Radix Et Caulis Acanthopanacis Senticosi extract, especially nonpolar invalid impurity, improve the purity of effective ingredient and the safety and stability of Radix Et Caulis Acanthopanacis Senticosi extract in Radix Et Caulis Acanthopanacis Senticosi extract, energy consumption can be reduced again simultaneously, and extract yield improves greatly, effect is better than prior art, has huge application prospect and market value.
Detailed description of the invention
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.Without departing from the spirit and substance of the case in the present invention, the amendment do the inventive method, step or condition or replacement, all belong to scope of the present invention.
If do not specialize, experiment material used in the embodiment of the present invention, reagent and instrument etc. are all commercially available.If specifically do not indicate, the technological means do not write exactly in embodiment all adopts conventional means well-known to those skilled in the art, as the detection method of extract, comprises the preparation method of the preparation of Radix Et Caulis Acanthopanacis Senticosi extract, the means etc. of adjust pH, all can adopt the conventional method of this area.
DM1180 resin used in the present invention is non-polar macroporous resin, and specific surface area is 400 ~ 500m
2/ g, average pore size is 100 ~ 110A °.
In the present invention, effective ingredient in Detection and Extraction thing, syringoside, eleutheroside E high performance liquid chromatography, total flavones spectrophotography.
In the present invention, the concentration of ethanol, the percentage sign " % " involved by the amount of alcohol content and eluent refers to percent by volume.Two-stage ultrafiltering of the present invention, 100,000,30,000 grades is in ultra-filtration process, the unit of ultrafilter membrane used: molecular cut off.
In the present invention, the multiple of water used is the weight multiple of Radix Et Caulis Acanthopanacis Senticosi medical material, and water used can be purified water or distilled water etc.
Embodiment 1: prepare Radix Et Caulis Acanthopanacis Senticosi extract
In the present embodiment, the preparation method of Radix Et Caulis Acanthopanacis Senticosi extract comprises the steps:
(1) extract: extract Radix Et Caulis Acanthopanacis Senticosi medical material 6kg3 time with the water (72L) of 12 volume times amount, each extraction 1 hour, merge extractive liquid, concentrated, obtain Radix Et Caulis Acanthopanacis Senticosi herbal decoction, for subsequent use;
(2) precipitate with ethanol: under agitation, add 95% ethanol (making alcohol content reach 75%), fully stir in the Radix Et Caulis Acanthopanacis Senticosi herbal decoction that step (1) obtains, and leave standstill 6 hours; Filter, filtrate recycling ethanol is extremely without alcohol taste, and continuing to be concentrated into relative density is 1.13(80 DEG C of survey), obtain Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream, for subsequent use;
(3) macroporous resin adsorption: get Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream that step (2) obtains appropriate, add water for injection and be diluted to general flavone content 10.0mg/ml, after stirring, filter, filtrate adjust pH 5.0, stirs, cold preservation 12 hours; Medicinal liquid after cold preservation is after 0.45 μm of filtering with microporous membrane clarification, with rare HCl adjust pH 2.0, filtrate with D101 macroporous resin column on 1.5BV/h flow velocity, then with same flow velocity 0.3 times of column volume purified water (pH value is for 3.0) eluting, collect eluent, for subsequent use; Then use 50% ethanol elution of 4 volume times amount, collect eluent, adjust pH to be 5.5,50% eluent being concentrated into relative density is 1.13(80 DEG C of survey), obtain condensed cream, for subsequent use;
(4) secondary precipitate with ethanol: under agitation, 95% ethanol (making alcohol content reach 85%) is added in the condensed cream that step (3) obtains, stir 15min, leave standstill 12 hours, leaching supernatant (the centrifugal rear leaching supernatant excessively of residue medicinal residues), filtrate recycling ethanol to without alcohol taste and to be concentrated into relative density be 1.13(80 DEG C of survey), receipts cream obtains Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream (i.e. Radix Et Caulis Acanthopanacis Senticosi extract A) 0.3kg, for subsequent use;
(5) DM1180 resin elution and two-stage ultrafiltering: get the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream (i.e. Radix Et Caulis Acanthopanacis Senticosi extract A) that step (4) obtains appropriate, add water for injection and be diluted to 1ml containing total flavones 15.0mg/ml, after stirring, filter, filtrate adjust pH 5.0, stir, 115 DEG C of pressure sterilizings 40 minutes, cold preservation 12 hours; Take out the medicinal liquid after cold preservation, after the clarification of 0.45 μm of filtering with microporous membrane, with the NaOH solution adjust pH 4.8 of 40%, filtrate is crossed DM1180 resin (upper prop liquid and resin volume ratio are 10:1) and is adsorbed, after having gone up sample, use 1 times of column volume purified water (pH value is 3.0) eluting again, elution flow rate is 3BV/h, collects eluent, stir, NaOH solution adjust pH with 40% 5.5,115 DEG C of pressure sterilizings 40 minutes, cold preservation 12 hours; Take out the medicinal liquid after cold preservation, after 0.45 μm of filtering with microporous membrane clarification, successively carry out the two-stage ultrafiltering of 100,000,30,000 grades, when filter does not have flow to permeate, push up water in right amount, stop ultrafiltration, it is 1.13(80 DEG C of survey that filtrate is concentrated into relative density), obtain Radix Et Caulis Acanthopanacis Senticosi extract B0.252kg.
Containing total flavones 68mg/g, syringoside 7.6mg/g and eleutheroside E 5.4mg/g in the Radix Et Caulis Acanthopanacis Senticosi extract B prepared in the present embodiment.
Embodiment 2: prepare Radix Et Caulis Acanthopanacis Senticosi extract
In the present embodiment, the preparation method of Radix Et Caulis Acanthopanacis Senticosi extract comprises the steps:
(1) extract: extract Radix Et Caulis Acanthopanacis Senticosi medical material 8kg2 time with the water (64L) of 8 volume times amount, each extraction 2 hours, merge extractive liquid, concentrated, obtain Radix Et Caulis Acanthopanacis Senticosi herbal decoction, for subsequent use;
(2) precipitate with ethanol: under agitation, 93% ethanol (making alcohol content reach 74.5%) is added in the Radix Et Caulis Acanthopanacis Senticosi herbal decoction that step (1) obtains, abundant stirring, leave standstill 12 hours, filter, filtrate recycling ethanol is extremely without alcohol taste, and continuing to be concentrated into relative density is 1.11(80 DEG C of survey), obtain Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream, for subsequent use;
(3) macroporous resin adsorption: get Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream that step (2) obtains appropriate, adding water for injection, to be diluted to general flavone content be 7.5mg/ml, and after stirring, filter, filtrate adjust pH 4.0, stirs, cold preservation 16 hours; Medicinal liquid after cold preservation is after 0.45 μm of filtering with microporous membrane clarification, with rare HCl adjust pH 2.0, filtrate with HPD100 macroporous resin column on 1.5BV/h flow velocity, then with same flow velocity 0.3 times of column volume purified water (pH value is for 3.0) eluting, collect eluent, for subsequent use; Then use 50% ethanol elution of 6 volume times amount, collect eluent, adjust pH to be 5.5,50% eluent being concentrated into relative density is 1.11(80 DEG C of survey), obtain condensed cream, for subsequent use;
(4) secondary precipitate with ethanol: under agitation, adds 93% ethanol (making alcohol content reach 84.5%) in the condensed cream that step (3) obtains, and stirs 15min, leaves standstill 16 hours; Leaching supernatant (residue medicinal residues centrifugal rear cross leaching supernatant), filtrate recycling ethanol to without alcohol taste and to be concentrated into relative density be 1.11(80 DEG C of survey), receipts cream obtains Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream (i.e. Radix Et Caulis Acanthopanacis Senticosi extract A) 0.456kg, for subsequent use;
(5) DM1180 resin elution and two-stage ultrafiltering: get the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream (i.e. Radix Et Caulis Acanthopanacis Senticosi extract A) that step (4) obtains appropriate, adding water for injection, to be diluted to general flavone content be 6mg/ml, after stirring, filter, filtrate adjust pH 4.0, stir, 120 DEG C of pressure sterilizings 30 minutes, cold preservation 16 hours, take out the medicinal liquid after cold preservation, after 0.45 μm of filtering with microporous membrane clarification, with the NaOH solution adjust pH 4.6 of 40%, filtrate crosses DM1180 resin (upper prop liquid: resin (V/V) is 6:1) absorption, after having gone up sample, with 2 times of column volume purified water (pH value is 3.0) eluting, elution flow rate is 2BV/h, collect eluent, stir, with the NaOH solution adjust pH 5.3 of 40%, 120 DEG C of pressure sterilizings 30 minutes, cold preservation 16 hours, take out the medicinal liquid after cold preservation, after 0.45 μm of filtering with microporous membrane clarification, successively carry out the two-stage ultrafiltering of 100,000,30,000 grades, when filter does not have flow to permeate, push up water in right amount, stop ultrafiltration, it is 1.12(80 DEG C of survey that filtrate is concentrated into relative density), obtain Radix Et Caulis Acanthopanacis Senticosi extract B0.368kg.
Containing total flavones 60mg/g, syringoside 7.2mg/g and eleutheroside E 4.9mg/g in the Radix Et Caulis Acanthopanacis Senticosi extract B prepared in the present embodiment.
Embodiment 3: prepare Radix Et Caulis Acanthopanacis Senticosi extract
In the present embodiment, the preparation method of Radix Et Caulis Acanthopanacis Senticosi extract comprises the steps:
(1) extract: extract Radix Et Caulis Acanthopanacis Senticosi medical material 10kg2 time with the water (120L) of 12 volume times amount, each extraction 1.5 hours, merge extractive liquid, concentrated, obtain Radix Et Caulis Acanthopanacis Senticosi herbal decoction, for subsequent use;
(2) precipitate with ethanol: under agitation, 95% ethanol (making alcohol content reach 75.5%) is added in the Radix Et Caulis Acanthopanacis Senticosi herbal decoction that step (1) obtains, abundant stirring, leave standstill 18 hours, filter, filtrate recycling ethanol is extremely without alcohol taste, and continuing to be concentrated into relative density is 1.14(80 DEG C of survey), obtain Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream, for subsequent use;
(3) macroporous resin adsorption: get Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream that step (2) obtains appropriate, adding water for injection, to be diluted to general flavone content be 10.0mg/ml, and after stirring, filter, filtrate adjust pH 5.5, stirs, cold preservation 18 hours; Medicinal liquid after cold preservation is after 0.45 μm of filtering with microporous membrane clarification, with rare HCl adjust pH 2.0, filtrate with ADS-F8 macroporous resin column on 2BV/h flow velocity, then with same flow velocity 0.5 times of column volume purified water (pH value is for 3.0) eluting, collect eluent, for subsequent use; Then use 50% ethanol elution of 6 volume times amount, collect eluent, adjust pH to be 5.5,50% eluent being concentrated into relative density is 1.14(80 DEG C of survey), obtain condensed cream, for subsequent use;
(4) secondary precipitate with ethanol: under agitation, 95% ethanol (making alcohol content reach 85.5%) is added in the condensed cream that step (3) obtains, stir 15min, leave standstill 16 hours, leaching supernatant (the centrifugal rear leaching supernatant excessively of residue medicinal residues), filtrate recycling ethanol to without alcohol taste and to be concentrated into relative density be 1.14(80 DEG C of survey), receipts cream obtains Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream (i.e. Radix Et Caulis Acanthopanacis Senticosi extract A) 0.44kg, for subsequent use;
(5) DM1180 resin elution and two-stage ultrafiltering: get the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream (i.e. Radix Et Caulis Acanthopanacis Senticosi extract A) that step (4) obtains appropriate, adding water for injection, to be diluted to general flavone content be 8mg/ml, after stirring, filter, filtrate adjust pH 5.5, stir, 115 DEG C of pressure sterilizings 30 minutes, cold preservation 18 hours; Take out the medicinal liquid after cold preservation, after 0.45 μm of filtering with microporous membrane clarification, with the NaOH solution adjust pH 5.0 of 40%, filtrate crosses DM1180 resin (upper prop liquid: resin (V/V) is 15:1) absorption, after having gone up sample, with 1 times of column volume purified water (pH value is 3.0) eluting, elution flow rate is 4BV/h, collects eluent, stir, NaOH solution adjust pH with 40% 5.7,115 DEG C of pressure sterilizings 30 minutes, cold preservation 18 hours; Take out the medicinal liquid after cold preservation, after 0.45 μm of filtering with microporous membrane clarification, successively carry out the two-stage ultrafiltering of 100,000,30,000 grades, when filter does not have flow to permeate, push up water in right amount, stop ultrafiltration, it is 1.14(80 DEG C of survey that filtrate is concentrated into relative density), obtain Radix Et Caulis Acanthopanacis Senticosi extract B0.39kg.
Containing total flavones 62mg/g, syringoside 7.8mg/g and eleutheroside E 6.3mg/g in the Radix Et Caulis Acanthopanacis Senticosi extract B prepared in the present embodiment.
Embodiment 4: prepare the little aqueous injection of Radix Et Caulis Acanthopanacis Senticosi
The preparation method of the injection type (little aqueous injection) containing Radix Et Caulis Acanthopanacis Senticosi extract in the present embodiment comprising:
The Radix Et Caulis Acanthopanacis Senticosi extract B74g of Example 1, is diluted to total flavones 6.0mg/ml with water for injection, adds 10g active carbon, backflow boil absorption 15min(refer to add charcoal after, reflux to boiling, start timing 15min, lower with), cooling, through 0.45 μm of membrane filtration to clarification; With 10,000 ultrafiltration membrance filters, filter when there is no flow to permeate, push up water in right amount, be diluted to total flavones 5.0mg/ml according to content, with 20% sodium hydroxide solution adjust pH 5.5; Medicinal liquid is through 0.22 μm of filter element fine straining, and fill 20ml, seals; Through high-temp steam sterilizing, cooling, obtains Ci Wu Jia type (little aqueous injection).
Containing total flavones 5.34mg/ml, syringoside 0.42mg/ml and eleutheroside E 0.28mg/ml in the little aqueous injection of the Radix Et Caulis Acanthopanacis Senticosi prepared in the present embodiment.
Embodiment 5: prepare the little aqueous injection of Radix Et Caulis Acanthopanacis Senticosi
The Radix Et Caulis Acanthopanacis Senticosi extract B88g of Example 2, is diluted to total flavones 7.0mg/ml with water for injection, adds 15g active carbon, and absorption 30min is boiled in backflow, cooling, through 0.45 μm of membrane filtration to clarification; With 10,000 ultrafiltration membrance filters, filter when there is no flow to permeate, push up water in right amount, be diluted to total flavones 5.3mg/ml according to content, with 20% sodium hydroxide solution adjust pH 5.7; Medicinal liquid is through 0.22 μm of filter element fine straining, and fill 20ml, seals; Through high-temp steam sterilizing, cooling, obtains Ci Wu Jia type (little aqueous injection).
Containing total flavones 5.45mg/ml, syringoside 0.47mg/ml and eleutheroside E 0.25mg/ml in the little aqueous injection of the Radix Et Caulis Acanthopanacis Senticosi prepared in the present embodiment.
Embodiment 6: prepare Radix Et Caulis Acanthopanacis Senticosi injection
The Radix Et Caulis Acanthopanacis Senticosi extract B140g of Example 3, is diluted to total flavones 6.5mg/ml with water for injection, adds 10g active carbon, and absorption 20min is boiled in backflow, cooling, through 0.45 μm of membrane filtration to clarification; With 10,000 ultrafiltration membrance filters, filter when there is no flow to permeate, push up water in right amount, be diluted to total flavones 3.2mg/ml according to content, with 20% sodium hydroxide solution adjust pH 5.6; Medicinal liquid is through 0.22 μm of filter element fine straining, and fill 100ml, seals; Through high-temp steam sterilizing, cooling, obtains Radix Et Caulis Acanthopanacis Senticosi injection.
Containing total flavones 3.17mg/ml, syringoside 0.29mg/ml and eleutheroside E 0.19mg/ml in the Radix Et Caulis Acanthopanacis Senticosi injection prepared in the present embodiment.
Embodiment 7: prepare Radix Et Caulis Acanthopanacis Senticosi lyophilized preparation
The Radix Et Caulis Acanthopanacis Senticosi extract B83g of Example 2, is diluted to total flavones 20.0mg/ml with water for injection, adds 18g active carbon, and absorption 20min is boiled in backflow, cooling, through 0.22 μm of membrane filtration to clarification; With 10,000 ultrafiltration membrance filters, filter when there is no flow to permeate, push up water in right amount, be diluted to total flavones 5.2mg/ml according to content, with 20% sodium hydroxide solution adjust pH 5.9, medicinal liquid to clarification, filtrate fill, fills nitrogen, sealing by fusing through 0.22 μm of membrane filtration, sterilizing, packaging, obtains Radix Et Caulis Acanthopanacis Senticosi lyophilized preparation.
Containing total flavones 5.14mg/ml, syringoside 0.41mg/ml and eleutheroside E 0.23mg/ml in the Radix Et Caulis Acanthopanacis Senticosi lyophilized preparation prepared in the present embodiment.
Experimental example 1: the inspection of extract
Comparative example: the embodiment 1 being the patent of 200710301682.X with reference to application number prepares Radix Et Caulis Acanthopanacis Senticosi extract.
The Radix Et Caulis Acanthopanacis Senticosi extract testing data of table 1: the embodiment of the present application 1-3 and comparative example
Experimental result shows, the application uses DM1180 resin to carry out the refining of Radix Et Caulis Acanthopanacis Senticosi extract, can effectively remove resin residue thing, and resin item is checked and becomes qualified from defective, and loss of effective components amount is very little, and extract yield improves greatly.
Experimental example 2: stability test
The embodiment of the present application 4-7 and above-mentioned comparative example are obtained extract to be placed in 40 DEG C ± 2 DEG C by the little aqueous injection sample that the embodiment of the present application 4 method is obtained, to carry out acceleration test in 6 months under relative humidity 75% ± 5% condition; Inspection target is detected respectively at 0,1,2,3,6 sampling at the end of month.
Table 2: embodiment 4-7 and comparative example accelerated test investigate data
The embodiment of the present application 4-7 and above-mentioned comparative example are obtained extract and be placed in temperature 25 ± 2 DEG C by the little aqueous injection sample that the embodiment of the present application 4 method is obtained, place 24 months under the condition of relative humidity 60 ± 10%; Respectively at 0,3,6,9,12,18,24,30 month, detect by stability high spot reviews project.
The long term test of table 3: embodiment 4-7 and comparative example investigates data
Above-mentioned accelerated test and long-term test results show: each preparation stability that the Radix Et Caulis Acanthopanacis Senticosi extract prepared by the embodiment of the present application 1-3 is made is better, pH value change is less, be better than prior art, this shows that DM1180 resin effectively can remove impurity, ensure that stability and the safety of preparation.
Although above with general explanation, detailed description of the invention and test, the present invention is described in detail, and on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (13)
1. a preparation method for Radix Et Caulis Acanthopanacis Senticosi extract, comprising: with water extraction Radix Et Caulis Acanthopanacis Senticosi medical material, the Radix Et Caulis Acanthopanacis Senticosi herbal decoction obtained is after precipitate with ethanol, cross that macroporous resin carries out adsorbing, eluting, eluent precipitate with ethanol again after concentrated, and then through refining, obtain Radix Et Caulis Acanthopanacis Senticosi extract;
Described refining method comprises: with DM1180 resin carry out adsorbing, eluting, eluent is again through two-stage ultrafiltering.
2. preparation method according to claim 1, is characterized in that, described method comprises the steps:
(1) with water extraction Radix Et Caulis Acanthopanacis Senticosi medical material, extracting solution, through concentrated, obtains Radix Et Caulis Acanthopanacis Senticosi herbal decoction;
(2) the Radix Et Caulis Acanthopanacis Senticosi herbal decoction that obtains of step (1) is through precipitate with ethanol, concentrated, obtains Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream;
(3) Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream of obtaining of step (2) is after dilution, crosses that macroporous resin carries out adsorbing, eluting, and concentrate eluant, obtains condensed cream;
(4) condensed cream that obtains of step (3) is through secondary precipitate with ethanol, concentrated, obtains Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream;
(5) Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream step (4) obtained after dilution, then through refining, obtains Radix Et Caulis Acanthopanacis Senticosi extract;
Described refining method comprises: the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream after dilution, crosses that DM1180 resin carries out adsorbing, eluting, and eluent through two-stage ultrafiltering, then concentrates, and to obtain final product.
3. preparation method according to claim 1 and 2, is characterized in that, the specific surface area of described DM1180 resin is 400 ~ 500m
2/ g, average pore size is 100 ~ 110A °.
4. preparation method according to claim 2, is characterized in that, in step (3), the model of described macroporous resin is ADS-F8, ADS-17, HPD750, D101, HPD100, HPD450, AB-8 or DM130.
5. the preparation method according to Claims 1 to 4 any one, it is characterized in that, described refining method comprises: get the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream after dilution, filter, filtrate adjust pH 4.0 ~ 5.5, sterilizing, cold preservation, medicinal liquid after cold preservation through filtering with microporous membrane clarification after, adjust pH 4.6 ~ 5.0; Filtrate is crossed DM1180 resin and is adsorbed, then uses 1 ~ 2 times of column volume purified water eluting, collects eluent, adjust pH 5.3 ~ 5.7, sterilizing, cold preservation; Medicinal liquid after cold preservation is after filtering with microporous membrane clarification, and successively carry out the two-stage ultrafiltering of 100,000,30,000 grades, it is 1.11 ~ 1.14 that filtrate is concentrated into relative density, to obtain final product.
6. preparation method according to claim 5, is characterized in that, filtrate is crossed DM1180 resin and adsorbed, and the volume ratio of upper prop liquid and resin is (6 ~ 15): 1; With 1 ~ 2 times of column volume purified water eluting, elution flow rate is 2 ~ 4BV/h.
7. the preparation method according to claim 5 or 6, is characterized in that, the condition of two places sterilizing is: 115 ~ 121 DEG C of sterilizings 30 ~ 40 minutes; The time of two places cold preservation is more than 12 hours.
8. the preparation method according to claim 1 ~ 7 any one, is characterized in that, described in comprise the following steps:
(1) extract: with the water extraction Radix Et Caulis Acanthopanacis Senticosi medical material 2 ~ 3 times of 6 ~ 12 volume times amount, extract 1 ~ 2 hour, merge extractive liquid, at every turn, concentrate, obtain Radix Et Caulis Acanthopanacis Senticosi herbal decoction, for subsequent use;
(2) precipitate with ethanol: under agitation, the Radix Et Caulis Acanthopanacis Senticosi herbal decoction obtained to step (1) with more than 93% ethanol mix, abundant stirring, leave standstill more than 6 hours, filter, filtrate recycling ethanol is to without alcohol taste, and to be concentrated into relative density be 1.11 ~ 1.14, obtain Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream, for subsequent use;
(3) macroporous resin adsorption: get Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream that step (2) obtains, being diluted to general flavone content with water for injection is 7.5 ~ 10.0mg/ml, after stirring, filter, filtrate adjust pH 4.0 ~ 5.5, stirs, cold preservation more than 12 hours; Medicinal liquid after cold preservation through filtering with microporous membrane clarification after, adjust pH 2.0 ± 0.2, filtrate with macroporous resin column on 1.5 ~ 2BV/h flow velocity, then with same flow velocity 0.3 ~ 0.5 times of column volume purified water eluting, collection eluent, for subsequent use; Then use 50% ethanol elution of 4 ~ 6 volume times amount, collect eluent, adjust pH to be 5.5, it is 1.11 ~ 1.14 that 50% eluent is concentrated into relative density, obtains condensed cream, for subsequent use;
(4) secondary precipitate with ethanol: under agitation, more than 93% ethanol is added in the condensed cream that step (3) obtains, stir, leave standstill more than 12 hours, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, and to be concentrated into relative density be 1.11 ~ 1.14, obtain Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream, for subsequent use;
(5) DM1180 resin elution and two-stage ultrafiltering: get the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream that step (4) obtains, being diluted to general flavone content with water for injection is 6 ~ 15mg/ml, filters, filtrate adjust pH 4.0 ~ 5.5,115 ~ 121 DEG C of sterilizings 30 ~ 40 minutes, cold preservation more than 12 hours;
Medicinal liquid after cold preservation is after filtering with microporous membrane clarification, adjust pH 4.6 ~ 5.0, filtrate is crossed DM1180 resin and is adsorbed, use 1 ~ 2 times of column volume purified water eluting again, elution flow rate is 2 ~ 4BV/h, collects eluent, adjust pH 5.3 ~ 5.7,115 ~ 121 DEG C of sterilizings 30 ~ 40 minutes, cold preservation more than 12 hours; Medicinal liquid after cold preservation is after filtering with microporous membrane clarification, and successively carry out the two-stage ultrafiltering of 100,000,30,000 grades, it is 1.11 ~ 1.14 that filtrate is concentrated into relative density, to obtain final product.
9. the preparation method according to claim 5 or 8, is characterized in that, the aperture of described microporous filter membrane is 0.45 μm.
10. the Radix Et Caulis Acanthopanacis Senticosi extract prepared by method described in claim 1 ~ 9 any one, wherein, containing total flavones 60 ~ 75mg/g, syringoside 7.0 ~ 8.5mg/g and eleutheroside E 4.5 ~ 7.0mg/g; Preferably, total flavones 60 ~ 68mg/g, syringoside 7.2 ~ 7.8mg/g and eleutheroside E 4.9 ~ 6.3mg/g is contained in described Radix Et Caulis Acanthopanacis Senticosi extract.
11. 1 kinds of preparations comprising Radix Et Caulis Acanthopanacis Senticosi extract according to claim 10, are made up of separately Radix Et Caulis Acanthopanacis Senticosi extract, or are made up of Radix Et Caulis Acanthopanacis Senticosi extract and pharmaceutically acceptable carrier or diluent.
12. preparations according to claim 11, is characterized in that, said preparation is injection type, are preferably the little aqueous injection of Radix Et Caulis Acanthopanacis Senticosi, Radix Et Caulis Acanthopanacis Senticosi lyophilized preparation or Radix Et Caulis Acanthopanacis Senticosi injection.
13. preparations according to claim 12, is characterized in that, containing total flavones 3 ~ 6.5mg/ml, syringoside 0.2 ~ 2.2mg/ml and eleutheroside E 0.1 ~ 1.0mg/ml in described Ci Wu Jia type;
Preferably, total flavones 5.25 ~ 5.46mg/ml, syringoside 0.38 ~ 0.47mg/ml and eleutheroside E 0.20 ~ 0.35mg/ml is contained in the little aqueous injection of described Radix Et Caulis Acanthopanacis Senticosi;
Preferably, total flavones 5.05 ~ 5.15mg/ml, syringoside 0.35 ~ 0.45mg/ml and eleutheroside E 0.15 ~ 0.25mg/ml is contained in described Radix Et Caulis Acanthopanacis Senticosi lyophilized preparation;
Preferably, total flavones 3.05 ~ 3.20mg/ml, syringoside 0.20 ~ 0.35mg/ml and eleutheroside E 0.15 ~ 0.20mg/ml is contained in described Radix Et Caulis Acanthopanacis Senticosi injection.
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| CN105311075A (en) * | 2015-11-25 | 2016-02-10 | 哈尔滨珍宝制药有限公司 | Preparation method of manyprickle acanthopanax root extract |
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| CN106727797A (en) * | 2016-11-11 | 2017-05-31 | 哈尔滨珍宝制药有限公司 | A kind of method for extracting wilsonii |
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| CN110302224A (en) * | 2019-08-06 | 2019-10-08 | 广东工业大学 | The extracting method and its application of chromocor extract in a kind of wilsonii |
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Application publication date: 20150701 |