CN104095924A - Preparation method for traditional Chinese medicine gel for treating gynaecological tumors - Google Patents
Preparation method for traditional Chinese medicine gel for treating gynaecological tumors Download PDFInfo
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Abstract
The invention discloses a preparation method for a traditional Chinese medicine gel for treating gynaecological tumors. The gel is prepared from four kinds of chemical compositions such as total saponins, total polysaccharides, magnolia officinalis total phenols and norcantharidin which are obtained through extraction and purification from three medicinal materials such as ginseng, radix astragali and acanthopanax senticosus. In a dry product of the total saponins composition, the content of ginsenoside Rg1 is not less than 3.0%, the content of ginsenoside Re is not less than 1.0%, the content of ginsenoside Rb1 is not less than 4.0%, the content of astragaloside is not less than 3.0%, the content of acanthopanax senticosus saponins E is not less than 2%; in a dry product of the total polysaccharides composition, the content calculated according to glucose is not less than 80%; in a dry product of magnolia officinalis total phenols, the content of the sum of magnolol and honokiol is not less than 80%; and in a dry product of the norcantharidin composition, the content of norcantharidin is not less than 96%. Magnolia officinalis total phenols and norcantharidin are both included by hydroxypropyl-beta-cyclodextrin. The above four kinds of compositions are mixed uniformly and pharmaceutic adjuvants are added for preparing a gel preparation, and the gel preparation is used to treat gynaecological uterus myoma, cervical carcinoma, herpes, condyloma and the like.
Description
Technical field
The invention belongs to pharmaceutical field, relate to the preparation method of a kind of total saponins that derives from Radix Ginseng, the Radix Astragali, Radix Et Caulis Acanthopanacis Senticosi, the total magnolol of total polysaccharides magnolia obovata, 4 kinds of component gel preparations of norcantharidin.
Background technology
Gynecological's kinds of tumor disease comprises hysteromyoma, cervical cancer, breast carcinoma etc., and sickness rate is in rising trend.Wherein cervical cancer is the 3rd the common malignant tumor that is only second to breast carcinoma and colorectal cancer in global women, is to be only second to breast carcinoma to occupy the 2nd common malignant tumor in developing country, is modal female genital tract malignant tumor.Within 2008, new cases of cervical cancer 52.98 ten thousand is estimated in the whole world, death 25.51 ten thousand people, and wherein 85% new cases are in developing country.
Gel means that medicine and suitable adjuvant make evenly or the transparent or semitransparent semi-solid preparation of suspendible.For for oral administration or external.The gel being formed by organic compound of topical application means single-phase gels, is divided into again aqueous gel and oil-base gel.Applying clinically more is that hydrogel is the gel of substrate.Chinese medicine gel means what extract and appropriate substrate were made, has semisolid or the glop preparation of gel characteristic, can be from oral cavity, the number of ways administration such as nasal cavity, eye mucosa, alimentary canal mucous membrane, vagina, rectum, skin.
Chinese medicine gel is a kind of novel external preparation, be applicable to skin, mucosa and tract, not only avoid the first-pass effect such as enzyme, acid in gastrointestinal tract that oral administration exists, and the untoward reaction that can alleviate medicine, met the theory of " inner disease outer treat " of the traditional Chinese medical science.There is the multiple advantages such as easy to use, comfortable, good biocompatibility simultaneously, superfine medicated powder, the extract etc. that can hold Chinese medicine compound, process conditions are not harsh, are applicable to the production status of compound Chinese medicinal preparation, easy to utilize, can be used as improved a kind of selection of Chinese medicine tradition external preparation.In recent years, new pharmaceutical technology is as the application in gel such as cyclodextrin clathrate, liposome, not only expand the range of application of Chinese medicine gel, and the combination of new technologies and methods makes, and Chinese medicine gel quality is more stable, effect is more lasting, improve drug bioavailability, and there is skin targeting function.
Vagina gel is in recent years to obtain paying close attention to and fast-developing a kind of novel form, and the advantage showing in skin, mucosal drug delivery dosage form is just progressively familiar with by people, this dosage form convenient drug administration, and intravaginal anelasticity is good, and drug treating time is long.
This gel preparation formula is made up of norcantharidin, total magnolol, Radix Ginseng, the Radix Astragali, Radix Et Caulis Acanthopanacis Senticosi, for gynecological's hysteroma, cervical cancer, herpes etc.There is following functions:
(1) antitumor, has direct killing effect to mice S180 cell, H22 cell; S180, H22, EAC are to the tumor-inhibiting action of dose dependent.
(2) strengthen immunologic function and can improve the phagocytic activity of tumor-bearing mice reticuloendothelial system to carbon granules, enhancing non-specific immunity function; Can increase the weight of normal mouse and tumor-bearing mice immune organ; Promote tumor-bearing mice T lymphocyte propagation and transformation function, strengthen DNCB and cause tumor-bearing mice delayed hypersensitivity; Improve tumor-bearing mice Hemolysin level; Show that this product can obviously strengthen mouse cell immunity and humoral immune function.
(3) significant anti-fatigue effect, can obviously extend tumor-bearing mice swimming time; Obviously strengthen the hypoxia-bearing capability under mice normal pressure.
(4) potentiation to Radiotherapy chemotherapy, share with small dose chemotherapy medicine CTX or 5-FU, and tumour inhibiting rate, higher than alone chemotherapeutic or alone ad pro injection, illustrates that both combine use and have anticancer synergism.Irradiate therapeutic alliance with Co60, EAC mice life span is extended compared with radiation alone group, prove that this product has certain potentiation to radiotherapy.
(5) in Cortex Magnoliae Officinalis, magnolol compounds has inducing apoptosis of tumour cell, suppresses neoplasm metastasis, suppresses the effects such as tumor vessel formation and inducing tumor cell differentiation kinds of tumors in vivo and in vitro.
(6) Attenuation: the leukopenia that treatment Radiotherapy chemotherapy causes, antagonism bone marrow inhibition.
In research process, medical material chemical composition is conducted in-depth research:
(1), by fitochemical studies and inside and outside pharmacological effect study on mechanism, clear and definite active ingredient, determines the best prescription of effective chemical constituent by Pharmacological Activity Screening;
(2) adopt modern Chinese medicine chemical composition purification technique, as the advanced technology such as resin purification, fractional extraction, crystallization, high speed centrifugation, membrane permeation, ultrafiltration, purity is reached more than 80%, so both retained composition and effectiveness, removed again the impurity that affects stability; Increase the research of finger printing and related substance simultaneously, ensure the steady quality between each batch, medicine is safer controlled.
(3) dosage form selection: vagina gel has suitable stickiness, can make medicine and vaginal mucosa have good bioadhesive, long and difficult loss, has preparation process simple with the suppository comparative drug holdup time, release is fast, not the feature of pollution clothes.This gel preparation can act on skin surface administration, for prevention and the treatment of mastopathy, again can vagina administration, and be used for the treatment of hysteromyoma, cervical cancer, herpesvirus infection etc.
Summary of the invention
Each medical material composition and effectiveness and each chemical composition pharmacologically active in prescription:
1, the contained cantharidin composition of Mylabris has adjusting immunologic function, inducing apoptosis of tumour cell effect, anticancer while leukocyte increasing, be mainly used in the adjuvant drug of cancer operation front and back and associating chemicotherapy front and back, also have the antivirus actions such as anti-hepatitis, liver cirrhosis, inhibition hepatitis B virus duplication, pharmacological toxicology evidence norcantharidin toxicity is less than cantharidin.
2, the contained multiple saponin of Radix Ginseng and polysaccharide all have certain anti-tumor activity, and structure activity relationship is clear and definite.Research shows that ginsenoside can the cell growth inhibiting factor, the infiltration of anticancer, and the sticking and invade of inhibition tumor cell and fibronectin splicing variants and laminin，LN, anti-tumor neovascularization formation, thus reach the effect of neoplasm growth transfer; Wherein representative composition ginsenoside Rg3, ginsenoside Rh1 all have stronger entirety and in vitro antitumor action.Current research report, ginsenoside Rg3 not only has the effect of the tumor growth of inhibition, and suppresses in addition tumor-blood-vessel growth, anti metastasis and recurrence effect.
3, the contained saponin of the Radix Astragali and polysaccharide component have stronger immunocompetence, and Radix Astragali extract can improve the phagocytic function of reticuloendothelial cell, strengthen the active anticancer of cell; Wherein saponin component also has antiinflammatory, antioxidation, resisting fatigue, protects the liver isoreactivity.
4, Radix Et Caulis Acanthopanacis Senticosi has definite antitumaous effect, and main anticancer component is saponin and polysaccharide.Transfer and the spontaneous leukemia of mice of transplanted tumor to zoopery of the extract of Radix Acanthopanacis Senticosi root and total glycosides, drug-induced tumor, cancer have certain inhibitory action, can also alleviate the toxicity of cancer therapy drug.
5, Cortex Magnoliae Officinalis pharmacological action is extensive, has antibacterial, antiulcer, spasmolytic, antiallergic, the effect such as of flaccid muscles, and toxic and side effects is few, and clinical application range is more and more wider.The antitumor action of magnolol compound and mechanism of action mainly contain inducing apoptosis of tumour cell, inhibition neoplasm metastasis, the formation of inhibition tumor vessel, inhibition tumor cell propagation, and inducing tumor cell breaks up, blocks nuclear factor NF-kB activation, reversing tumor drug resistance.The mouse skin tumor that Cortex Magnoliae Officinalis methanolic extract honokiol causes the second stage of carcinogenic test in body has obvious inhibitory action.
The research of total sugar glycosides effective part raw material extraction and purification process:
Saponin: medical material is adopted to temperature control thermal cycle reflux, extract, technology, then use the multistage Purification of traditional Chinese herbs technology such as macroporous adsorption resin chromatography, solvent extraction and separation purification, high speed centrifugation, ultrafiltration, saponin content is all reached more than 80%, greatly improved validity of products, quality controllability and safety.
Mylabris: adopt chemical synthetic drug norcantharidin to replace and extract composition and effectiveness from animal drugs, solved animal material source, extraction and purification process and Quality Control problem, greatly improved safety, reduced cost.
Polysaccharide: adopt step ethanol precipitation remove impurity, adopt membrane permeation technology to remove impurity after precipitate with ethanol, adopt ultrafiltration membrance filter to intercept the polysaccharide of certain molecular weight, ensure the control of the molecular weight distribution of polysaccharide.
Cortex Magnoliae Officinalis: magnolol, honokiol can adopt the extraction of co_2 supercritical fluid extraction technology, extract obtains method by molecular distillation again and obtains the higher total magnolol of purity.
Dosage form selection and research
Aqueous gel substrate is mostly swelled into aqueous gel and does not dissolve in water.The general easy painting exhibition of this class substrate and eccysis, without greasy feeling, can not hinder skin normal function by absorptive tissue transudate.Also because viscosity is compared with the release of the little medicine that is beneficial to, particularly water soluble drug.
The general method for making of hydrogel adhesive, the water-soluble person of medicine is often first dissolved in part water or glycerol, heating if desired, all the other prescription compositions are made hydrogel matrix by preparation method of base material, then mix to add water to drug solution and enoughly stir evenly and get final product.The water insoluble person of medicine, can be first with a small amount of water or glycerol porphyrize, disperses, then is mixed in substrate and stirs evenly and get final product.
Carbomer is the crosslinked high molecular polymer of acrylic acid and acrylic sucrose, and commodity are called carbomer, is often divided into 934,940,941 equal-specifications by viscosity difference, and this product is a kind of moist very strong white bulky powder that draws.Owing to there being a large amount of hydroxy-acid groups in molecule, there is very similarly physicochemical property with polyacrylic acid, can be swelling rapidly in water, but do not dissolve.Hydroxy-acid group in its molecular structure makes its aqueous dispersions be acid, and the pH value of 1% aqueous dispersions is about 3.11, and viscosity is lower.When with in alkali and time, dissolve gradually with macromole, viscosity also rises gradually, forms clear and bright solution in the time of low concentration, forms translucent gel in the time that concentration is larger.There are maximum viscosity and denseness in pH6～11, the alkali that neutralization is used and the concentration difference of carbopol, the viscosity of its solution changes also difference to some extent.Generally, in and 1g carbopol approximately consume 1.35g triethanolamine or 400mg sodium hydroxide, the substrate that this product is made is without greasy feeling, is coated with lubricated comfortable, is particularly suitable for treating seborrheic dermatosis.
Gel is by medicine and substrate composed, and substrate is the carrier of medicine, again the release of medicine is had to important impact, and therefore, the selection of substrate is particularly important to the preparation of gel.Gel can be divided into aqueous gel and oil-base gel agent according to the difference of substrate.Aqueous gel substrate is generally by water, glycerol, propylene glycol, cellulose derivative, carbomer and alginate, tragacanth, gelatin; Non-cellulosic polysaccharide is as formations such as chitin, ethene polymers, acrylic resin, polyvinyl alcohol and carbopol.
Magnolol and norcantharidin are little polar compounds, and water solublity is poor, also easily scatter and disappear unstable, and by can effectively solving problems after hydroxypropyl level betacyclodextrin enclose, and because gentle release is beneficial to the mucosa irritation that reduces medicine.
Detailed description of the invention
Embodiment 1
Radix Ginseng 1000g, Radix Astragali 2000g, tri-kinds of medical materials of Radix Et Caulis Acanthopanacis Senticosi 3000g are thinly sliced, added 15 times of amount soak with ethanol 1 hour, adopt thermal cycle reflux, extract, method, collect extracting solution.Extracting solution is evaporated to without ethanol taste, lets cool, and adds the dilution of 12000ml water, and cold preservation, filters.Filtrate adds 20% sodium hydroxide solution (weight ratio) adjust pH to 12, macroporous adsorptive resins absorption on medicinal liquid.First wash with water to eluent as neutral, use again 80% ethanol elution complete to saponin eluting, collect ethanol elution, reclaim ethanol and be concentrated into without ethanol taste, aqueous solution adds 20% sodium hydroxide solution (weight ratio) adjust pH to 12, with equivalent water-saturated n-butanol extraction 4 times.Collect butanol extraction liquid, reclaim under reduced pressure n-butyl alcohol is to dry, and residue adds absolute ethyl alcohol and stirring and dissolves, and filters, and reclaims ethanol, and evaporate to dryness gets dry extract, and pulverizes, and obtains total saponins 101.5g.
By medical material residue after above-mentioned ethanol extraction, add 8 times of water gagings and make solvent, reflux, extract, 2 times, collects extracting solution, is evaporated to 2 times of crude drug amounts, let cool, high speed centrifugation remove impurity, rotating speed 12000-16000 turns, and adds ethanol and makes concentration of alcohol to 30%, the centrifugal precipitation of going, solution is concentrated into 1.5 times of crude drug amounts, adds ethanol and makes concentration of alcohol to 85%, quiet heavy 24 hours, get and precipitate the dissolving of blunging, add Sevag reagent (chloroform: n-butyl alcohol=4: 1), stir centrifugal (15min, 4000r/min), repeatedly extract 3 times.Gained supernatant is evaporated to small size, water dialysis 3 days, the interior solution of bag filter adds ethanol makes concentration of alcohol reach 85% ethanol, and quiet heavy 24 hours, filter, precipitation absolute ethanol washing, vacuum drying, must refine total polysaccharides 304g.
The total magnolol HYDROXYPROPYL BETA-CYCLODEXTRIN of Cortex Magnoliae Officinalis enclose: get the total magnolol 2g of Cortex Magnoliae Officinalis, add 25ml ethanol, tepor makes to dissolve, and splashes in 500ml, the HYDROXYPROPYL BETA-CYCLODEXTRIN saturated aqueous solution of 75 DEG C, stir 45 minutes, stop heating and continue to stir 5 hours again, obtain white precipitate, room temperature leaves standstill 12 hours, filter, precipitate is dried at 40 DEG C, crosses 80 mesh sieves, obtain total magnolol clathrate.
Norcantharidin HYDROXYPROPYL BETA-CYCLODEXTRIN enclose: remove norcantharidin 0.5g, add 25ml ethanol, tepor makes to dissolve, and splashes in 500ml, the HYDROXYPROPYL BETA-CYCLODEXTRIN saturated aqueous solution of 75 DEG C, stir 45 minutes, stop heating and continue to stir 5 hours again, obtain white precipitate, room temperature leaves standstill 12 hours, filter, precipitate is dried at 40 DEG C, crosses 80 mesh sieves, obtain norcantharidin clathrate.
The preparation of gel: total saponins 10g, total polysaccharides 30g, total magnolol cyclodextrin clathrate 10g, norcantharidin cyclodextrin clathrate 2g, carbomer 26g, triethanolamine 32g, glycerol 200g, the about 500g of propylene glycol 200g purified water; Take carbomer in prescription ratio, make to be scattered in purified water, placing spends the night makes it fully swelling.Add glycerol and propylene glycol to stir evenly, slowly add triethanolamine, limit edged stirs to obtain transparence gel-type vehicle.Separately get total saponins, total polysaccharides, total magnolol and norcantharidin and be dissolved in suitable quantity of water, stir, until completely dissolved, slowly add and in people's substrate, constantly stir and get final product, finally add water to 1000g, stir.
Embodiment 2
Radix Ginseng 1000g is thinly sliced, mix and add in extraction pot, add 18 times of amount soak with ethanol 1 hour, adopt thermal cycle reflux, extract, method, collect extracting solution.Extracting solution is evaporated to without ethanol taste, lets cool, and adds the dilution of 2000ml water, and cold preservation, filters.Filtrate adds 10% sodium hydroxide solution (weight ratio) adjust pH to 10, macroporous adsorptive resins absorption on medicinal liquid.First wash with water to eluent as neutral, use again 80% ethanol elution complete to saponin eluting, collect ethanol elution, reclaim ethanol and be concentrated into without ethanol taste, aqueous solution adds 10% sodium hydroxide solution (weight ratio) adjust pH to 10, with equivalent water-saturated n-butanol extraction 4 times.Collect butanol extraction liquid, reclaim under reduced pressure n-butyl alcohol is to dry, and residue adds absolute ethyl alcohol and stirring and dissolves, and filters, and reclaims ethanol, and evaporate to dryness gets dry extract, and pulverizes, and obtains total saponins 32.0g.
Radix Astragali 2000g is thinly sliced, mix and add in extraction pot, add 18 times of amount soak with ethanol 1 hour, adopt thermal cycle reflux, extract, method, collect extracting solution.Extracting solution is evaporated to without ethanol taste, lets cool, and adds the dilution of 3000ml water, and cold preservation, filters.Filtrate adds 20% sodium hydroxide solution (weight ratio) adjust pH to 12, macroporous adsorptive resins absorption on medicinal liquid.First wash with water to eluent as neutral, use again 80% ethanol elution complete to saponin eluting, collect ethanol elution, reclaim ethanol and be concentrated into without ethanol taste, aqueous solution adds 20% sodium hydroxide solution (weight ratio) adjust pH to 12, with equivalent water-saturated n-butanol extraction 4 times.Collect butanol extraction liquid, reclaim under reduced pressure n-butyl alcohol is to dry, and residue adds absolute ethyl alcohol and stirring and dissolves, and filters, and reclaims ethanol, and evaporate to dryness gets dry extract, and pulverizes, and obtains total saponins 31.0g.
Radix Et Caulis Acanthopanacis Senticosi 3000g is thinly sliced, mix and add in extraction pot, add 18 times of amount soak with ethanol 1 hour, adopt thermal cycle reflux, extract, method, collect extracting solution.Extracting solution is evaporated to without ethanol taste, lets cool, and adds the dilution of 4000ml water, and cold preservation, filters.Filtrate adds 20% sodium hydroxide solution (weight ratio) adjust pH to 10, macroporous adsorptive resins absorption on medicinal liquid.First wash with water to eluent as neutral, use again 80% ethanol elution complete to saponin eluting, collect ethanol elution, reclaim ethanol and be concentrated into without ethanol taste, aqueous solution adds 20% sodium hydroxide solution (weight ratio) adjust pH to 10, with equivalent water-saturated n-butanol extraction 4 times.Collect butanol extraction liquid, reclaim under reduced pressure n-butyl alcohol is to dry, and residue adds absolute ethyl alcohol and stirring and dissolves, and filters, and reclaims ethanol, and evaporate to dryness gets dry extract, and pulverizes, and obtains total saponins 34.5g.
By medical material residue after above-mentioned ethanol extraction, add 8 times of water gagings and make solvent, reflux, extract, 2 times, collects extracting solution, is evaporated to 2 times of crude drug amounts, let cool, high speed centrifugation remove impurity, rotating speed 12000-16000 turns, and adds ethanol and makes concentration of alcohol to 30%, the centrifugal precipitation of going, solution is concentrated into 1.5 times of crude drug amounts, adds ethanol and makes concentration of alcohol to 85%, quiet heavy 24 hours, get and precipitate the dissolving of blunging, add Sevag reagent (chloroform: n-butyl alcohol=4: 1), stir centrifugal (15min, 4000r/min), repeatedly extract 3 times.Gained supernatant is evaporated to small size, water dialysis 3 days, the interior solution of bag filter adds ethanol makes concentration of alcohol reach 85% ethanol, and quiet heavy 24 hours, filter, precipitation absolute ethanol washing, vacuum drying, must refine total polysaccharides 315g.
The total magnolol of Cortex Magnoliae Officinalis, norcantharidin HYDROXYPROPYL BETA-CYCLODEXTRIN enclose: get the total magnolol of Cortex Magnoliae Officinalis and norcantharidin mixture 2.5g, add 25ml ethanol, tepor makes to dissolve, and splashes in 500ml, the HYDROXYPROPYL BETA-CYCLODEXTRIN saturated aqueous solution of 75 DEG C, stir 45 minutes, stop heating and continue to stir 5 hours again, obtain white precipitate, room temperature leaves standstill 12 hours, filter, precipitate is dried at 40 DEG C, crosses 80 mesh sieves, obtain total magnolol clathrate.
The preparation of gel: total saponins 10g, total polysaccharides 30g, total magnolol norcantharidin cyclodextrin clathrate 10g, carbomer 30g, triethanolamine 30g, glycerol 200g, the about 500g of propylene glycol 200g purified water; Take carbomer in prescription ratio, make to be scattered in purified water, placing spends the night makes it fully swelling.Add glycerol and propylene glycol to stir evenly, slowly add triethanolamine, limit edged stirs to obtain transparence gel-type vehicle.Separately get total saponins, total polysaccharides, total magnolol and norcantharidin and be dissolved in suitable quantity of water, stir, until completely dissolved, slowly add and in people's substrate, constantly stir and get final product, finally add water to 1000g, stir.
Embodiment 3
Radix Ginseng 1000g, Radix Astragali 2000g, tri-kinds of medical materials of Radix Et Caulis Acanthopanacis Senticosi 3000g are thinly sliced, added 15 times of amount soak with ethanol 1 hour, adopt thermal cycle reflux, extract, method, collect extracting solution.Extracting solution is evaporated to without ethanol taste, lets cool, and adds the dilution of 12000ml water, and cold preservation, filters.Filtrate adds 20% sodium hydroxide solution (weight ratio) adjust pH to 10-12, macroporous adsorptive resins absorption on medicinal liquid.First wash with water to eluent as neutral, use again 80% ethanol elution complete to saponin eluting, collect ethanol elution, reclaim ethanol and be concentrated into without ethanol taste, aqueous solution adds 20% sodium hydroxide solution (weight ratio) adjust pH to 10-12, with equivalent water-saturated n-butanol extraction 4 times.Collect butanol extraction liquid, reclaim under reduced pressure n-butyl alcohol is to dry, and residue adds absolute ethyl alcohol and stirring and dissolves, and filters, and reclaims ethanol, and evaporate to dryness gets dry extract, and pulverizes, and obtains total saponins 101.5g.
By medical material residue after above-mentioned ethanol extraction, add 8 times of water gagings and make solvent, reflux, extract, 2 times, collects extracting solution, is evaporated to 2 times of crude drug amounts, let cool, high speed centrifugation remove impurity, rotating speed 12000-16000 turns, and adds ethanol and makes concentration of alcohol to 30%, the centrifugal precipitation of going, solution is concentrated into 1.5 times of crude drug amounts, adds ethanol and makes concentration of alcohol to 85%, quiet heavy 24 hours, get and precipitate the dissolving of blunging, add Sevag reagent (chloroform: n-butyl alcohol=4: 1), stir centrifugal (15min, 4000r/min), repeatedly extract 3 times.Gained supernatant is evaporated to small size, water dialysis 3 days, the interior solution of bag filter adds ethanol makes concentration of alcohol reach 85% ethanol, and quiet heavy 24 hours, filter, precipitation absolute ethanol washing, vacuum drying, must refine total polysaccharides 304g.
Total magnolol, norcantharidin HYDROXYPROPYL BETA-CYCLODEXTRIN enclose: get the total magnolol of Cortex Magnoliae Officinalis and norcantharidin mixture 2.5g, add 25ml ethanol, tepor makes to dissolve, and splashes in 500ml, the HYDROXYPROPYL BETA-CYCLODEXTRIN saturated aqueous solution of 75 DEG C, stir 45 minutes, stop heating and continue to stir 5 hours again, obtain white precipitate, room temperature leaves standstill 12 hours, filter, precipitate is dried at 40 DEG C, crosses 80 mesh sieves, obtain HYDROXYPROPYL BETA-CYCLODEXTRIN clathrate.
The preparation of gel: total saponins 10g, total polysaccharides 30g, total magnolol norcantharidin cyclodextrin clathrate 10g, carbomer 27g, triethanolamine 33g, glycerol 200g, the about 500g of propylene glycol 200g purified water; Take carbomer in prescription ratio, make to be scattered in purified water, placing spends the night makes it fully swelling.Add glycerol and propylene glycol to stir evenly, slowly add triethanolamine, limit edged stirs to obtain transparence gel-type vehicle.Separately get total saponins, total polysaccharides, total magnolol and norcantharidin and be dissolved in suitable quantity of water, stir, until completely dissolved, slowly add and in people's substrate, constantly stir and get final product, finally add water to 1000g, stir.
Claims (6)
1. the gel that the total saponins that derives from Radix Ginseng, the Radix Astragali, Radix Et Caulis Acanthopanacis Senticosi, the total magnolol of total polysaccharides magnolia obovata, norcantharidin four constituents that are used for the treatment of gynecological tumor are made.
2. preparation according to claim 1, is characterized in that:
(1) wherein total saponin extracts is pressed dry product calculating, must not be less than 3.0% containing ginsenoside Rg1, ginsenoside Re must not be less than 1.0%, and ginsenoside Rb1 must not be less than 4.0%, astragaloside must not be less than 3.0%, and acanthopanax senticosus saponins E is no less than 2.0%;
(2) wherein total polysaccharide extractive calculates and must not be less than 80% with glucose meter content by dry product;
(3) wherein the total magnolol of Cortex Magnoliae Officinalis is pressed dry product calculating, must not be less than 80% containing magnolol, honokiol total amount;
(4) wherein norcantharidin must not be less than 96% by dry product calculating content;
(5) wherein the total magnolol of Cortex Magnoliae Officinalis, norcantharidin are used respectively HYDROXYPROPYL BETA-CYCLODEXTRIN enclose.
3. preparation according to claim 1, the preparation method of its total saponins is:
By Radix Ginseng, the Radix Astragali, three kinds of medical materials of Radix Et Caulis Acanthopanacis Senticosi, cut into the thin slice of 2～3mm, add 15-20 and doubly measure soak with ethanol 1 hour, adopt thermal cycle reflux, extract, method, collect extracting solution; Extracting solution is evaporated to without ethanol taste, lets cool, and adds 1-2 times of water gaging dilution, and cold preservation, filters; Filtrate adds 10%-20% sodium hydroxide solution (weight ratio) adjust pH to 10-12, macroporous adsorptive resins absorption on medicinal liquid.First wash with water to eluent as neutral, use again 60%-85% ethanol elution complete to saponin eluting, collect ethanol elution, reclaim ethanol and be concentrated into without ethanol taste, aqueous solution adds 10%-20% sodium hydroxide solution (weight ratio) adjust pH to 10-12, with equivalent water-saturated n-butanol extraction 4-6 time; Collect butanol extraction liquid, reclaim under reduced pressure n-butyl alcohol is to dry, and residue adds absolute ethyl alcohol and stirring and dissolves, and filters, and reclaims ethanol, and evaporate to dryness gets dry extract, and pulverizes, and obtains total saponins.
4. preparation according to claim 1, the preparation method of its total polysaccharides is:
By medical material residue after the ethanol extraction described in the claims 3, add 6-12 times of water gaging and make solvent, reflux, extract, 2-3 time, collect extracting solution, be evaporated to 1.5-2.5 times of crude drug amount, let cool, high speed centrifugation remove impurity, rotating speed 12000-16000 turns, add ethanol and make concentration of alcohol to 30%, the centrifugal precipitation of going, solution is concentrated into 1 times of crude drug amount, add ethanol and make concentration of alcohol to 85%, quiet heavy 24 hours, get and precipitate the dissolving of blunging, add Sevag reagent (chloroform: n-butyl alcohol=4: 1, volume ratio), stir, centrifugal (15min, 4000r/min), repeatedly extract 3-5 time, gained supernatant is evaporated to small size, water dialysis 3 days, the interior solution of bag filter adds ethanol makes concentration of alcohol reach 85% ethanol, and quiet heavy 24 hours, filter, precipitation absolute ethanol washing, vacuum drying, obtains refining total polysaccharides.
5. preparation according to claim 1, the total magnolol of its Cortex Magnoliae Officinalis, norcantharidin HYDROXYPROPYL BETA-CYCLODEXTRIN inclusion method are:
(1) get the total magnolol 1g-3g of Cortex Magnoliae Officinalis, add 15ml-30ml ethanol, tepor makes to dissolve, and splashes in 300ml-500ml, the HYDROXYPROPYL BETA-CYCLODEXTRIN saturated aqueous solution of 75 DEG C, stir 45-60 minute, stop heating and continue to stir 4-6 hour again, obtain white precipitate, room temperature leaves standstill 12 hours, filter, precipitate is dried at 40 DEG C, crosses 80 mesh sieves, obtain total magnolol clathrate;
(2) remove norcantharidin 0.5g-1g, add 15ml-30ml ethanol, tepor makes to dissolve, and splashes in 300ml-500ml, the HYDROXYPROPYL BETA-CYCLODEXTRIN saturated aqueous solution of 75 DEG C, stir 45 minutes, stop heating and continue to stir 4-6 hour again, obtain white precipitate, room temperature leaves standstill 12 hours, filter, precipitate is dried at 40 DEG C, crosses 80 mesh sieves, obtain norcantharidin clathrate.
6. preparation according to claim 1, the preparation method of its gel is:
(1) raw material adjuvant composition: total saponins 8-12 part, total polysaccharides 25-40 part, total magnolol cyclodextrin clathrate 8-15 part, norcantharidin cyclodextrin clathrate 2-5 part, carbomer 20-35 part, triethanolamine 25-40 part, glycerol 180-240 part, propylene glycol 150-220 part purified water adds to 1000 parts;
(2) preparation: take carbomer in prescription ratio, make to be scattered in purified water, placing spends the night makes it fully swelling.Add glycerol and propylene glycol to stir evenly, slowly add triethanolamine, limit edged stirs to obtain transparence gel-type vehicle; Separately get total saponins, total polysaccharides, total magnolol and norcantharidin and be dissolved in suitable quantity of water, stir, until completely dissolved, slowly add and in people's substrate, constantly stir and get final product, finally add water to 1000 parts, stir.
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| CN201310128148.9A Pending CN104095924A (en) | 2013-04-15 | 2013-04-15 | Preparation method for traditional Chinese medicine gel for treating gynaecological tumors |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105560292A (en) * | 2014-10-16 | 2016-05-11 | 张继旭 | Drug capable of killing herpes simplex virus and chicken pox-herpes zoster virus |
| CN111700858A (en) * | 2020-07-30 | 2020-09-25 | 欧迪玛(湖北)生物科技有限公司 | Gel composition for treating cervical cancer and preparation method thereof |
| CN111808210A (en) * | 2020-09-01 | 2020-10-23 | 江西业力医疗器械有限公司 | Lumbrugua burclover polysaccharide, extraction method and application thereof |
| CN116350668A (en) * | 2023-03-29 | 2023-06-30 | 广州通泽医疗科技有限公司 | Gynecological gel and preparation method and application thereof |
-
2013
- 2013-04-15 CN CN201310128148.9A patent/CN104095924A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105560292A (en) * | 2014-10-16 | 2016-05-11 | 张继旭 | Drug capable of killing herpes simplex virus and chicken pox-herpes zoster virus |
| CN111700858A (en) * | 2020-07-30 | 2020-09-25 | 欧迪玛(湖北)生物科技有限公司 | Gel composition for treating cervical cancer and preparation method thereof |
| CN111808210A (en) * | 2020-09-01 | 2020-10-23 | 江西业力医疗器械有限公司 | Lumbrugua burclover polysaccharide, extraction method and application thereof |
| CN111808210B (en) * | 2020-09-01 | 2021-01-19 | 西藏甘露藏药股份有限公司 | Lumbrugua burclover polysaccharide, extraction method and application thereof |
| CN116350668A (en) * | 2023-03-29 | 2023-06-30 | 广州通泽医疗科技有限公司 | Gynecological gel and preparation method and application thereof |
| CN116350668B (en) * | 2023-03-29 | 2024-03-19 | 广州通泽医疗科技有限公司 | Gynecological gel and preparation method and application thereof |
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