CN104739906A - Acanthopanax senticosus extract, preparation method and preparation thereof - Google Patents
Acanthopanax senticosus extract, preparation method and preparation thereof Download PDFInfo
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- CN104739906A CN104739906A CN201310743674.6A CN201310743674A CN104739906A CN 104739906 A CN104739906 A CN 104739906A CN 201310743674 A CN201310743674 A CN 201310743674A CN 104739906 A CN104739906 A CN 104739906A
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Abstract
The invention relates to a preparation method for an acanthopanax senticosus extract, the acanthopanax senticosus extract prepared by the method and a preparation containing the acanthopanax senticosus extract. The method includes: extracting an acanthopanax senticosus extract medicinal material with water, concentrating the extracted solution to obtain an acanthopanax senticosus water decoction paste; carrying out primary alcohol precipitation and concentration to obtain primary alcohol precipitation paste; adjusting the pH with lime milk and sulfuric acid, and then conducting standing and concentration to obtain a concentrated paste; then performing secondary alcohol precipitation and concentration to obtain secondary alcohol precipitation paste; diluting the secondary alcohol precipitation paste, then carrying out macroporous adsorbent resin adsorption and elution, subjecting the eluent to secondary ultrafiltration, and then conducting concentration to obtain the acanthopanax senticosus extract. The method provided by the invention can significantly reduce the content of impurities, especially nonpolar invalid impurities in the acanthopanax senticosus extract, improve the purity of effective components in the acanthopanax senticosus extract and the safety and stability of the extract, also reduces the energy consumption and greatly improves the extract yield, thus having huge application prospects 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 CN200710117640.0(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 comprising the steps of: (1) adopts 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, regulate PH to 4.5 ~ 6.5 with sulphuric acid 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 CN201010165556.8(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 CN201210049755.1(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 comprising the steps of: 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 application CN02125536.9(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.
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.If the preparation method of the Radix Et Caulis Acanthopanacis Senticosi extract made new advances therefore can be developed, especially carry out the optimization of subtractive process, most important for the stability and safety improving the preparation containing this Radix Et Caulis Acanthopanacis Senticosi extract.
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, 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 lime cream of obtaining of step (2) and sulfur acid for adjusting pH, then leave standstill, concentrated, obtain 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) the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream that obtains of step (4) is after dilution, and through absorption with macroporous adsorbent resin, eluting, eluent through two-stage ultrafiltering, then concentrates, and obtains Radix Et Caulis Acanthopanacis Senticosi extract.
Wherein, the model of described macroporous adsorbent resin is DM1180, ADS-F8, ADS-17, HPD750, D101, HPD100, HPD450, AB-8 or DM130.
Further, described DM1180 resin is phenylethylene resin series, is also nonpolar macroporous adsorption resin, specific surface area: 400 ~ 500m
2/ g, average pore size: 100-110A °.
Wherein, in step (2), regulate pH value to 10.0 ~ 12.0 of a Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream with lime cream, then regulate pH value to 5.0 ~ 6.0 of a Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream with sulphuric acid.
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 volumes times weight, 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 ethanol of more than 93% is added in the Radix Et Caulis Acanthopanacis Senticosi herbal decoction that step (1) obtains, 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 1.14 ~ 1.18(80 DEG C of mensuration), obtain Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream, for subsequent use;
(3) lime sulphur treatment: Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream step (2) obtained mixes with purified water, after stirring, filter, during liquid temp to be filtered 40 DEG C ~ 50 DEG C, with lime cream adjust ph to 10.0 ~ 12.0 of 20%, stir, use sulphuric acid adjust ph to 5.0 ~ 6.0 of 20% again, continue to stir, leave standstill, leaching supernatant also reclaims and is concentrated into relative density is 1.14 ~ 1.19(80 DEG C of survey), obtain condensed cream;
(4) secondary precipitate with ethanol: under agitation, more than 93% ethanol is added in the condensed cream that step (3) obtains, abundant stirring, 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 ~ 1.20(80 DEG C of mensuration), 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) absorption with macroporous adsorbent resin: get the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream that step (4) obtains appropriate, be diluted to general flavone content with water for injection and be about 7.5 ~ 10.0mg/ml, after stirring, filter, filtrate adjust pH 4.0 ~ 5.0, stir, 115 ~ 121 DEG C of sterilizings 30 ~ 40 minutes, cold preservation more than 12 hours;
Medicinal liquid after cold preservation through filtering with microporous membrane clarification after, adjust pH 4.6 ~ 5.0, filtrate crosses absorption with macroporous adsorbent resin, use 1 ~ 2 times of column volume purified water eluting again, collect eluent, stir, adjust pH 5.5 ± 0.2,115 ~ 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 ~ 1.20(80 DEG C of survey that filtrate is concentrated into relative density), namely obtain Radix Et Caulis Acanthopanacis Senticosi extract (i.e. Radix Et Caulis Acanthopanacis Senticosi extract B).
In the present invention, the pH value of purified water is 3.0.
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), all stir 15 minutes.
In step (3), leave standstill 4 ~ 8 hours.
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), time of repose preferably 12 ~ 16 hours.
In step (5), all preferably 12 ~ 18 hours cold preservation (cold preservation of two places) time.
In step (5), filtrate crosses absorption with macroporous adsorbent resin, and the volume ratio of upper prop liquid and resin is (6 ~ 15): 1.
In step (5), with 1 ~ 2 times of column volume purified water eluting, elution flow rate is 2 ~ 4BV/h.
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 that described method prepares.
Containing total flavones 50 ~ 65mg/g, syringoside 5.5 ~ 7.5mg/g and eleutheroside E 4.5 ~ 6.0mg/g in described Radix Et Caulis Acanthopanacis Senticosi extract.
Preferably, total flavones 53 ~ 63mg/g, syringoside 5.7 ~ 6.7mg/g and eleutheroside E 4.5 ~ 5.2mg/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 containing 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 3.0 ~ 6.5mg/ml, syringoside 0.2 ~ 2.0mg/ml and eleutheroside E 0.1 ~ 1.0mg/ml in described Ci Wu Jia type.
Preferably, total flavones 5.20 ~ 5.40mg/ml, syringoside 0.38 ~ 0.55mg/ml and eleutheroside E 0.25 ~ 0.35mg/ml is contained in the little aqueous injection of described Radix Et Caulis Acanthopanacis Senticosi.
Preferably, total flavones 5.00 ~ 5.15mg/ml, syringoside 0.40 ~ 0.50mg/ml and eleutheroside E 0.28 ~ 0.35mg/ml is contained in described Radix Et Caulis Acanthopanacis Senticosi lyophilized preparation.
Preferably, total flavones 3.10 ~ 3.15mg/ml, syringoside 0.25 ~ 0.30mg/ml and eleutheroside E 0.18 ~ 0.22mg/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) in the middle of ethanol precipitation twice, add a step stone vulcanizing treatment, and coordinate macroporous adsorbent resin to adsorb, reduce nonpolar invalid impurity content simultaneously, can also energy consumption be reduced.
(2) adopt the enrichment of macroporous adsorbent resin effective ingredient, eliminate water-solubility impurity and non polar impurities, alleviate ultrafilter membrane burden.
(3) adopt two-stage ultrafiltering, macromolecular substances is removed in segmentation, improves and comprises the safety of the preparation of gained Radix Et Caulis Acanthopanacis Senticosi extract, reduces loss of effective components, extends ultrafilter membrane service life.
(4) 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.
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, comprise the preparation method etc. 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 nonpolar macroporous adsorption 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 amount of alcohol content, eluent, and Calx and the percentage sign involved by sulphuric acid " % " refer 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.
Detailed description of the invention
Embodiment 1: prepare Radix Et Caulis Acanthopanacis Senticosi extract
(1) extract: extract Radix Et Caulis Acanthopanacis Senticosi medical material (8kg) 3 times with 6 times of water gagings (48L), 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, slowly 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 1.18(80 DEG C of mensuration), obtain Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream, for subsequent use;
(3) stone sulfur method: get Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream that step (2) obtains and add in the tank filling appropriate purified water in right amount, add the purified water of purified water to time precipitate with ethanol cream 10 times amount (v/v), stir after 15min, filter, liquid temp to be filtered reaches 45 DEG C, by 20% lime cream adjust ph to 11.0, stir 15min, use 20% sulphuric acid adjust ph to 5.5 again, continue to stir 15min, leave standstill 4 hours, beginning leaching supernatant reclaims and is concentrated into relative density is 1.16(80 DEG C of survey);
(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 (residue medicinal residues centrifugal rear cross leaching supernatant), filtrate recycling ethanol is to without alcohol taste, and to be concentrated into relative density be 1.12(80 DEG C of mensuration), receive cream and obtain Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream (i.e. Radix Et Caulis Acanthopanacis Senticosi extract A0.648kg), for subsequent use;
(5) absorption with macroporous adsorbent resin 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 to be diluted to 1ml containing total flavones and to be about 10.0mg/ml, after stirring, filter, filtrate surveys adjust pH 5.0, stir, 115 DEG C of pressure sterilizings 40 minutes, cold preservation 12 hours; Medicinal liquid after cold preservation is after 0.45 μm of filtering with microporous membrane clarification, with the NaOH solution adjust pH 4.8 of 40%, filtrate is crossed DM-1180 macroporous adsorbent resin (upper prop liquid and resin volume ratio are 10:1) and is adsorbed, and after upper complete sample, then uses 1 times of column volume purified water eluting, elution flow rate is 3BV/h, collect eluent, stir, with the NaOH solution adjust pH 5.5 of 40%, 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 1.12(80 DEG C of survey that filtrate is concentrated into relative density), obtain Radix Et Caulis Acanthopanacis Senticosi extract B0.6kg.
Containing total flavones 53mg/g, syringoside 5.7mg/g and eleutheroside E 4.5mg/g in the Radix Et Caulis Acanthopanacis Senticosi extract B prepared in the present embodiment.
Embodiment 2: prepare Radix Et Caulis Acanthopanacis Senticosi extract
(1) extract: extract Radix Et Caulis Acanthopanacis Senticosi medical material (6kg) 2 times with 8 volumes times water gaging (48L), 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, slowly add 93% ethanol (making alcohol content reach 74.5%), fully stir in the Radix Et Caulis Acanthopanacis Senticosi herbal decoction that step (1) obtains, and leave standstill 12 hours; Filter, filtrate recycling ethanol is extremely without alcohol taste, and continuing to be concentrated into relative density is 1.16(80 DEG C of mensuration), obtain Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream, for subsequent use;
(3) stone sulfur method: get Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream that step (2) obtains and add in the tank filling appropriate purified water in right amount, add the purified water of purified water to time precipitate with ethanol cream 8 times amount (v/v), stir after 15min, liquid temp to be filtered 45 DEG C, by 20% lime cream adjust ph to 12.0, stirs 15min, use 20% sulphuric acid adjust ph to 6.0 again, continue to stir 15min, leave standstill 6 hours, beginning leaching supernatant reclaims and is concentrated into relative density is 1.19(80 DEG C of survey);
(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 1.13(80 DEG C of mensuration), receipts cream obtains Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream (i.e. Radix Et Caulis Acanthopanacis Senticosi extract A0.456kg), for subsequent use;
(5) absorption with macroporous adsorbent resin 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 to be diluted to 1ml containing total flavones and to be about 7.5mg/ml, after stirring, filter, filtrate surveys adjust pH 4.0, stir, 115 DEG C of pressure sterilizings 40 minutes, cold preservation 16 hours; Medicinal liquid after cold preservation is after 0.45 μm of filtering with microporous membrane clarification, with the NaOH solution adjust pH 4.6 of 40%, filtrate crosses AB-8 macroporous adsorbent resin (upper prop liquid: resin 6:1) absorption, after upper complete sample, then uses 2 times of column volume purified water eluting, elution flow rate is 2BV/h, collect eluent, stir, with the NaOH solution adjust pH 5.3 of 40%, 115 DEG C of pressure sterilizings 40 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 1.13(80 DEG C of survey that filtrate is concentrated into relative density), obtain Radix Et Caulis Acanthopanacis Senticosi extract B0.414kg.
Containing total flavones 56mg/g, syringoside 6.0mg/g and eleutheroside E 4.8mg/g in the Radix Et Caulis Acanthopanacis Senticosi extract B prepared in the present embodiment.
Embodiment 3: prepare Radix Et Caulis Acanthopanacis Senticosi extract
(1) extract: extract Radix Et Caulis Acanthopanacis Senticosi medical material (10kg) 2 times with 12 volumes times water gaging (120L), 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, slowly add 95% ethanol (making alcohol content reach 75.5%), fully stir in the Radix Et Caulis Acanthopanacis Senticosi herbal decoction that step (1) obtains, and 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 mensuration), obtain Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream, for subsequent use;
(3) stone sulfur method: get Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream that step (2) obtains and add in the tank filling appropriate purified water in right amount, add the purified water of purified water to time precipitate with ethanol cream 12 times amount (v/v), stir after 15min, liquid temp to be filtered 45 DEG C, by 20% lime cream adjust ph to 10.0, stirs 15min, use 20% sulphuric acid adjust ph to 5.0 again, continue to stir 15min, leave standstill 8 hours, beginning leaching supernatant reclaims and is concentrated into relative density is 1.14(80 DEG C of survey);
(4) secondary precipitate with ethanol: under agitation, adds 95% ethanol (making alcohol content reach 85.5%) 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 1.14(80 DEG C of mensuration), receipts cream obtains Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream (i.e. Radix Et Caulis Acanthopanacis Senticosi extract A0.71kg), for subsequent use;
(5) absorption with macroporous adsorbent resin 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 to be diluted to 1ml containing total flavones and to be about 8mg/ml, after stirring, filter, filtrate surveys adjust pH 5.0, stir, 115 DEG C of pressure sterilizings 40 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 5.0 of 40%, filtrate crosses DM-1180 macroporous adsorbent resin (upper prop liquid: resin 15:1) absorption, after having gone up sample, use 1 times of column volume purified water eluting again, elution flow rate is 4BV/h, collects and eluent, stir, NaOH solution adjust pH with 40% 5.7,115 DEG C of pressure sterilizings 40 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 1.14(80 DEG C of survey that filtrate is concentrated into relative density), obtain Radix Et Caulis Acanthopanacis Senticosi extract B0.66kg.
Containing total flavones 63mg/g, syringoside 6.7mg/g and eleutheroside E 5.2mg/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 5.37mg/ml, syringoside 0.51mg/ml and eleutheroside E 0.34mg/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 5.28mg/ml, syringoside 0.46mg/ml and eleutheroside E 0.30mg/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 3.15mg/ml, syringoside 0.28mg/ml and eleutheroside E 0.21mg/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, sterilizing through 0.22 μm of membrane filtration, and packaging, obtains Radix Et Caulis Acanthopanacis Senticosi lyophilized preparation.
Containing total flavones 5.14mg/ml, syringoside 0.47mg/ml and eleutheroside E 0.32mg/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 201010165556.8 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, adds a step stone vulcanizing treatment, and coordinates macroporous adsorbent resin to adsorb, significantly can reduce the content of impurity in Radix Et Caulis Acanthopanacis Senticosi extract, especially nonpolar invalid impurity in the middle of ethanol precipitation twice; Can effectively remove resin residue thing, 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
Sample embodiment 4-7 and comparative example being obtained the little aqueous injection that extract obtains by the embodiment of the present application 4 method is placed in 40 DEG C ± 2 DEG C, carries 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
Sample embodiment 4-7 and comparative example being obtained the little aqueous injection that extract obtains by the embodiment of the present application 4 method is placed in temperature 25 ± 2 DEG C, places 30 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
Accelerated test and long-term test results show: the preparation stability that the Radix Et Caulis Acanthopanacis Senticosi extract prepared by embodiment of the present invention 1-3 is made is better, pH value change is less, this shows to add a step stone vulcanizing treatment in the middle of ethanol precipitation twice, and coordinate macroporous adsorbent resin to adsorb, significantly can reduce the content of impurity in Radix Et Caulis Acanthopanacis Senticosi extract, especially nonpolar invalid 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 (12)
1. a preparation method for Radix Et Caulis Acanthopanacis Senticosi extract, 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 lime cream of obtaining of step (2) and sulfur acid for adjusting pH, then leave standstill, concentrated, obtain 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) the Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream that obtains of step (4) is after dilution, and through absorption with macroporous adsorbent resin, eluting, eluent through two-stage ultrafiltering, then concentrates, and obtains Radix Et Caulis Acanthopanacis Senticosi extract.
2. the preparation method of Radix Et Caulis Acanthopanacis Senticosi extract according to claim 1, is characterized in that, the model of described macroporous adsorbent resin is DM1180, ADS-F8, ADS-17, HPD750, D101, HPD100, HPD450, AB-8 or DM130.
3. the preparation method of Radix Et Caulis Acanthopanacis Senticosi extract according to claim 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. the preparation method of Radix Et Caulis Acanthopanacis Senticosi extract according to claim 1, is characterized in that, in step (2), regulates pH value to 10.0 ~ 12.0 of a Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream, then regulate its pH value to 5.0 ~ 6.0 with sulphuric acid with lime cream.
5. the preparation method of the Radix Et Caulis Acanthopanacis Senticosi extract according to Claims 1 to 4 any one, is characterized in that, the method comprises the following steps:
(1) extract: with the water extraction Radix Et Caulis Acanthopanacis Senticosi medical material 2 ~ 3 times of 6 ~ 12 volumes times weight, 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 ethanol of more than 93% is added in the Radix Et Caulis Acanthopanacis Senticosi herbal decoction that step (1) obtains, 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 1.14 ~ 1.18, obtain Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream, for subsequent use;
(3) lime sulphur treatment: Radix Et Caulis Acanthopanacis Senticosi extract precipitate with ethanol cream step (2) obtained mixes with purified water, after stirring, filter, during liquid temp to be filtered 40 DEG C ~ 50 DEG C, with lime cream adjust ph to 10.0 ~ 12.0 of 20%, stir, use sulphuric acid adjust ph to 5.0 ~ 6.0 of 20% again, continue to stir, leave standstill, leaching supernatant also reclaims and is concentrated into relative density is 1.14 ~ 1.19, obtains condensed cream;
(4) secondary precipitate with ethanol: under agitation, more than 93% ethanol is added in the condensed cream that step (3) obtains, abundant stirring, 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 ~ 1.20, obtain Radix Et Caulis Acanthopanacis Senticosi extract secondary precipitate with ethanol cream, for subsequent use;
(5) absorption with macroporous adsorbent resin: 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 7.5 ~ 10.0mg/ml, after stirring, filter, filtrate adjust pH 4.0 ~ 5.0, stir, 115 ~ 121 DEG C of sterilizings 30 ~ 40 minutes, cold preservation more than 12 hours;
Medicinal liquid after cold preservation through filtering with microporous membrane clarification after, adjust pH 4.6 ~ 5.0, filtrate crosses absorption with macroporous adsorbent resin, use 1 ~ 2 times of column volume purified water eluting again, collect eluent, stir, adjust pH 5.5 ± 0.2,115 ~ 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 ~ 1.20 that filtrate is concentrated into relative density, namely obtains Radix Et Caulis Acanthopanacis Senticosi extract.
6. the preparation method of Radix Et Caulis Acanthopanacis Senticosi extract according to claim 5, is characterized in that, in step (2), concentration of alcohol is 93 ~ 95%, makes alcohol content reach 74.5 ~ 75.5%; In step (4), concentration of alcohol is 93 ~ 95%, makes alcohol content reach 84.5 ~ 85.5%.
7. the preparation method of Radix Et Caulis Acanthopanacis Senticosi extract according to claim 5, is characterized in that, in step (5), filtrate crosses absorption with macroporous adsorbent resin, 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.
8. the preparation method of the Radix Et Caulis Acanthopanacis Senticosi extract according to claim 5 ~ 8 any one, is characterized in that, the aperture of microporous filter membrane used is 0.45 μm.
9. the Radix Et Caulis Acanthopanacis Senticosi extract prepared by method described in claim 1 ~ 8 any one; Wherein, containing total flavones 50 ~ 65mg/g, syringoside 5.5 ~ 7.5mg/g and eleutheroside E 4.5 ~ 6.0mg/g; Preferably, total flavones 53 ~ 63mg/g, syringoside 5.7 ~ 6.7mg/g and eleutheroside E 4.5 ~ 5.2mg/g is contained in described Radix Et Caulis Acanthopanacis Senticosi extract.
10. the preparation containing Radix Et Caulis Acanthopanacis Senticosi extract described in claim 8, is made up of separately described Radix Et Caulis Acanthopanacis Senticosi extract, or is made up of Radix Et Caulis Acanthopanacis Senticosi extract and pharmaceutically acceptable carrier or diluent.
11. preparations according to claim 10, is characterized in that, described preparation is injection type, the little aqueous injection of preferred Radix Et Caulis Acanthopanacis Senticosi, Radix Et Caulis Acanthopanacis Senticosi lyophilized preparation or Radix Et Caulis Acanthopanacis Senticosi injection.
12. preparations according to claim 11, is characterized in that, containing total flavones 3.0 ~ 6.5mg/ml, syringoside 0.2 ~ 2.0mg/ml and eleutheroside E 0.1 ~ 1.0mg/ml in described Ci Wu Jia type;
Preferably, total flavones 5.20 ~ 5.40mg/ml, syringoside 0.38 ~ 0.55mg/ml and eleutheroside E 0.25 ~ 0.35mg/ml is contained in the little aqueous injection of described Radix Et Caulis Acanthopanacis Senticosi;
Preferably, total flavones 5.00 ~ 5.15mg/ml, syringoside 0.40 ~ 0.50mg/ml and eleutheroside E 0.28 ~ 0.35mg/ml is contained in described Radix Et Caulis Acanthopanacis Senticosi lyophilized preparation;
Preferably, total flavones 3.10 ~ 3.15mg/ml, syringoside 0.25 ~ 0.30mg/ml and eleutheroside E 0.18 ~ 0.22mg/ml is contained in described Radix Et Caulis Acanthopanacis Senticosi injection.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105395583A (en) * | 2015-11-25 | 2016-03-16 | 哈尔滨珍宝制药有限公司 | Preparing method for acanthopanax senticosus extract |
| CN105726947A (en) * | 2016-02-02 | 2016-07-06 | 王知斌 | Acanthopanax senticosus leaf and polygonatum odoratum leaf extract for improving sleeping and reducing blood sugar and preparing method and application thereof |
| CN108434152A (en) * | 2018-03-26 | 2018-08-24 | 黑龙江珍宝岛药业股份有限公司 | A kind of pharmaceutical composition and its preparation method and application for improving sleep |
| CN109010398A (en) * | 2018-09-28 | 2018-12-18 | 黑龙江省格润药业有限责任公司 | A kind of Radix Et Caulis Acanthopanacis Senticosi injection and its preparation process |
| CN112763639A (en) * | 2020-12-30 | 2021-05-07 | 四川新绿色药业科技发展有限公司 | Preparation process and quality control method of radix Acanthopanacis Senticosi reference extract |
-
2013
- 2013-12-30 CN CN201310743674.6A patent/CN104739906A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105395583A (en) * | 2015-11-25 | 2016-03-16 | 哈尔滨珍宝制药有限公司 | Preparing method for acanthopanax senticosus extract |
| CN105726947A (en) * | 2016-02-02 | 2016-07-06 | 王知斌 | Acanthopanax senticosus leaf and polygonatum odoratum leaf extract for improving sleeping and reducing blood sugar and preparing method and application thereof |
| CN105726947B (en) * | 2016-02-02 | 2019-08-16 | 黑龙江中医药大学 | A kind of improvement sleep, hypoglycemic acanthopanax radix polygonati officinalis leaf extract and its preparation method and application |
| CN108434152A (en) * | 2018-03-26 | 2018-08-24 | 黑龙江珍宝岛药业股份有限公司 | A kind of pharmaceutical composition and its preparation method and application for improving sleep |
| CN109010398A (en) * | 2018-09-28 | 2018-12-18 | 黑龙江省格润药业有限责任公司 | A kind of Radix Et Caulis Acanthopanacis Senticosi injection and its preparation process |
| CN112763639A (en) * | 2020-12-30 | 2021-05-07 | 四川新绿色药业科技发展有限公司 | Preparation process and quality control method of radix Acanthopanacis Senticosi reference extract |
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Application publication date: 20150701 |