CN101053587A - Medicinal composition for treating tumor and preparation method and quality control method thereof - Google Patents
Medicinal composition for treating tumor and preparation method and quality control method thereof Download PDFInfo
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Abstract
The invention discloses a medicine combination, especially a medicine combination treating tumor disease and the producing method and quality control method thereof, belonging to Chinese traditional medicine field. The Chinese traditional medicine combination has the astragalus root and blister beetle as material. The patent medicine is prepared by extracting the material with different crafts according to a certain compatible requirement and refining to obtain the extract, preferred is injection.
Description
Technical field
The present invention relates to a kind of pharmaceutical composition, particularly a kind of drug regimen that is used for the treatment of tumor disease and preparation method thereof and method of quality control belong to the field of Chinese medicines.
Background technology
Malignant tumor is the commonly encountered diseases and the frequently-occurring disease of serious threat human health, and according to World Health Organization's report, in more than 50 hundred million populations of the whole world, the tumor patient of annual new diagnosis is about 9,000,000 people, because of the dead person of tumor reached for 7,000,000 people/years, accounts for nearly 20% of total case fatality rate.Drug therapy occupies an important position in three big therapies of malignant tumor, and is with the fastest developing speed.The overwhelming majority is a lead compound with the natural anti-cancer active component in synthetic chemical classes cancer therapy drug, and the exploitation of cancer therapy drug comprises that computer mould fits Bionic Design all based on the natural anti-cancer active component.There is abundant resources of medicinal plant in China, the medical expert of China uses the experience of natural anti-cancer drugs according to various nationalities since the sixties, a collection of determined curative effect, the little natural anti-cancer drugs of untoward reaction from national medicine, have been researched and developed out, for due contribution has been made in the control of cancer.
Summary of the invention
One object of the present invention is to provide a kind of Chinese medicine composition for the treatment of tumor disease; The preparation method and the method for quality control that provide above-mentioned Chinese medicine composition to be prepared into various preparations is provided another object of the present invention.
The object of the present invention is achieved like this.
This pharmaceutical composition is to be made by the crude drug of weight ratio: the Radix Astragali 50～400, Mylabris 1～6.After preferred, the proportioning of each crude drug is: the Radix Astragali 200～350, Mylabris 3～5.Further preferred, the optimal proportion that can get each crude drug is: the Radix Astragali 300 weight portions, Mylabris 4 weight portions.
Mylabris is the dry body of Meloidae insecticide south mylabris phalerata or yellow black mylabris cichorii, is the medicine that China at first finds to have antitumor action, and its anticancer main effective ingredient is a cantharidin.Experiment showed, that cantharidin can suppress the metabolism of Hela cell and human esophagus cancer, carcinoma of gastric cardia, gastric cancer, breast carcinoma, fibroma, Hokdkin disease, hepatocarcinoma, pulmonary carcinoma and sarcoma of spleen cell.The antitumor mechanism of speckle huge legendary turtle element mainly is the protein synthesis of anticancer, reduces the tumor hormonal readiness, thereby influences the nucleic acid metabolism of tumor cell.Clinical practice and experimentation prove, the effect that it has stronger inhibition tumor and good leukocyte increasing can suppress the growth in vitro of kinds of tumor cells.But on the other hand, Mylabris also has bigger clinical adverse when there is significant curative effect treatment tumor aspect, and in light of this situation, the inventor has discovered the synergism of the Radix Astragali and Mylabris.Saponin that contains in the Radix Astragali and polysaccharide are fairly obvious in the effect aspect the raising human body immunity, and be better to the tumor treatment effect after using with proper proportion and Mylabris compatibility, and the clinical adverse of Mylabris can well be improved.Select Mylabris and the Radix Astragali two flavor medical materials right as medicine, be developed to various preparations, Mylabris is uncharmed, and the Radix Astragali is set upright, and plays the effect of Synergistic treatment.
Above drug regimen is except can also replacing with the effective part extract of these medical materials, i.e. Radix Astragali total saponins extract, Radix Astragali Mongolici total polysaccharide extract and cantharidin extract with feeding intake in proportion with crude drug.Convert by these compositions content ratio in crude drug, inventory is a basically identical.In addition, if feed intake with effective site, its purity should reach certain standard, such as: Radix Astragali total saponins accounts for more than 50% of total solid in the Radix Astragali total saponins extract, and Radix Astragali Mongolici total polysaccharide accounts for more than 50% of total solid in the Radix Astragali Mongolici total polysaccharide extract; The cantharidin extract then is the white crystalline powder that obtains with organic solvent extraction, and wherein cantharidin accounts for more than 80% of total solid.The method for detecting purity of these effective sites is consistent with used content assaying method in the quality control of final products.
Above crude drug can be made multiple dosage form as required, and optimum dosage form is capsule and injection.The preceding leaching process of these systems is:
A, get the Radix Astragali, decoct with water, after water liquid concentrates, add equivalent ethanol precipitate with ethanol, get supernatant and reclaim ethanol, surplus water liquid adds 3～5 times of amount ethanol secondary precipitate with ethanol, filters, and precipitates standby; Supernatant reclaims ethanol, adds water saturated n-butanol extraction 3～5 times in the surplus water liquid, merges n-butanol extracting liquid, be recycled to dried, residue with water dissolution after by strong base resin anion (R.A.) post, use the distilled water eluting, collect effluent, promptly obtain the Radix Astragali total saponins extract solution;
B, get precipitate standby among a, be dissolved in water, the activated carbon decolorizing that adds 0.2%～2% water liquid weight for several times, and is basicly stable to water liquid color, filters, and promptly obtains the Radix Astragali Mongolici total polysaccharide aqueous solution;
C, get Mylabris, be broken into fine powder, add volume ratio and be 1: 30～1: 50 hydrochloric acid acetone mixed liquor merceration 3～5 times, leachate reclaims acetone to saturation, cold put to make separate out crystallization, crystallization is dissolved in acetone after with petroleum ether, add alkaline dehydrated alcohol to muddy, cold preservation filters, get filtering residue, obtain Mylabris extract;
D, above three kinds of extracts are mixed after, add suitable adjuvant, make required dosage form.
Above-mentioned steps a also can realize by another kind of mode: get the Radix Astragali, decoct with water, after water liquid concentrates, add equivalent ethanol precipitate with ethanol, get supernatant and reclaim ethanol, surplus water liquid adds 3～5 times of amount ethanol secondary precipitate with ethanol, filters, and precipitates standby; Supernatant reclaims ethanol, surplus water liquid adds water saturated n-butanol extraction 3～5 times, merge n-butanol extracting liquid, be recycled to dried, residue with water dissolution after by the AB-8 macroporous adsorptive resins, it is colourless to be washed till effluent with distilled water, reuse 30% ethanol elution remove impurity, reuse 70% ethanol elution is collected 70% ethanol elution part to colourless, drying promptly obtains the Radix Astragali total saponins extract.
Just can make multiple dosage form easily with above extract, as make injection: get Mylabris extract and be dissolved in the Radix Astragali total saponins aqueous solution, ultrafilter membrane by molecular weight 10,000, collect filtration fraction water liquid, mix the Radix Astragali Mongolici total polysaccharide aqueous solution, adjust pH to 4.0～6.5, be dissolved into an amount of stabilizing agent, add the injection water to total amount, sterilization, promptly.
Because the dna purity of product of the present invention is higher, so the assay of its index components is a key technology.The inventor has formulated following several content assaying method through research, and these methods not only can be checked product, can be used for also checking whether the purity of each effective part extract reaches requirement simultaneously.
A, ultraviolet spectrophotometry are surveyed Radix Astragali total saponins content
The preparation precision of reference substance solution takes by weighing the astragaloside reference substance, adds methanol and quantitatively dissolves, and be diluted to scale, shakes up, promptly;
The accurate absorption of the preparation of standard allusion quotation line reference substance solution 20,40,60,80,100ul place 10ml tool plug test tube respectively, put and wave most solvent in the water-bath, take out immediately, put coldly, precision adds 5% vanillin-glacial acetic acid solution 0.2ml, perchloric acid 0.8ml, shake up, put in 60 ℃ of water-baths and heated 15 minutes, take out, immediately with circulating water cooling 2 minutes, precision adds glacial acetic acid 5ml, shaking up, is blank with the reagent corresponding, according to spectrophotography, wavelength place at 544nm measures trap, with the trap is vertical coordinate, and concentration is abscissa, the drawing standard curve;
The algoscopy precision is measured product of the present invention, and adding methanol extraction water changes molten or thin up, puts in the separatory funnel, add the chloroform jolting and extract 3 times, combined chloroform liquid also washes with water 2 times, discards chloroform solution, washing liquid and above-mentioned water layer merge, and put in the separatory funnel, with water saturated n-butanol extraction 5 times, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds methanol makes dissolving, and quantitatively shift in the measuring bottle, add methanol to scale, shake up, precision is measured and is put in the tool plug test tube, put and wave most solvent in the water-bath, take out immediately, put cold, precision adds 5% vanillin-glacial acetic acid solution 0.2ml, perchloric acid 0.8ml shakes up, and puts in 60 ℃ of water-baths and heats 15 minutes, take out, with circulating water cooling 2 minutes, precision added glacial acetic acid 5ml, shakes up immediately, with the reagent corresponding is blank, according to spectrophotography, measure trap at the wavelength place of 544nm, the weight of reading total Saponin the need testing solution from standard curve, calculate, promptly;
B, high-efficient liquid phase technique are surveyed the content of astragaloside
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Volume ratio is that 35: 65 acetonitrile-water is a mobile phase; Evaporative light scattering detector;
It is an amount of that the preparation precision of reference substance solution takes by weighing the astragaloside reference substance, adds methanol and make solution, promptly;
The preparation precision of need testing solution is measured the present invention's product, and adding methanol extraction water changes molten or thin up, puts in the separatory funnel, add the chloroform jolting and extract 3 times, combined chloroform liquid also washes with water 2 times, discards chloroform solution, washing liquid and above-mentioned water layer merge, and put in the separatory funnel, with water saturated n-butanol extraction 5 times, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds methanol makes dissolving, and quantitatively shift in the measuring bottle, add methanol to scale, shake up, promptly;
Accurate reference substance solution 5 μ l, the 15 μ l of drawing of algoscopy, need testing solution 10 μ l inject chromatograph of liquid, measure, promptly;
C, sulphuric acid anthrone method are surveyed Radix Astragali Mongolici total polysaccharide content
The preparation precision of reference substance solution takes by weighing the anhydrous glucose that is dried to constant weight through 80 ℃, puts in the measuring bottle, is dissolved in water and is diluted to scale, shakes up, and makes behind the thin up to contain anhydrous glucose 0.08mg among every 1ml, promptly;
The preparation precision of standard curve is measured reference substance solution 0.2,0.4,0.6,0.8 and 1.0ml, puts respectively in the 10ml tool plug test tube, and each is managed precision and adds water and make into 1ml, the accurate respectively sulphuric acid anthrone solution 4ml that adds in ice bath, shake up, put in the water-bath and heated 10 minutes, cool off after 40 minutes, with the corresponding reagent is blank, according to ultraviolet spectrophotometry, measure trap at the wavelength place of 625nm, be vertical coordinate with the trap, concentration is abscissa, the drawing standard curve; Wherein sulphuric acid anthrone solution is for getting anthrone 50mg, adds water 25ml and sulphuric acid 75ml makes dissolving, that is, face and use new system;
The algoscopy precision is measured product of the present invention, extracting in water or dilution, and precision is measured and is put in the tool plug test tube, precision adds water makes into 1ml, and the accurate sulphuric acid anthrone solution 4ml that adds shakes up in ice bath, put in the water-bath and heated 10 minutes, cooling off after 40 minutes, is blank with the corresponding reagent, according to ultraviolet spectrophotometry, wavelength place at 625nm measures trap, from the weight that standard curve is read astragalus polysaccharides the need testing solution, calculate, promptly;
D, sulphuric acid phynol method are surveyed Radix Astragali Mongolici total polysaccharide content
The preparation precision of reference substance solution takes by weighing the anhydrous glucose that is dried to constant weight through 80 ℃, puts in the measuring bottle, is dissolved in water and is diluted to scale, shakes up, and makes behind the thin up to contain anhydrous glucose 0.6mg among every 1ml, promptly;
The preparation precision of standard curve is measured reference substance solution 0.5,1.0,1.5,2.0,2.5ml, puts respectively in the 50ml measuring bottle, adds water to scale, shakes up; Precision is measured above-mentioned solution 2ml respectively, puts in the tool plug test tube, respectively adds 4% phenol solution 1ml, and mixing adds sulphuric acid 7.0ml rapidly, shakes up, and puts in 40 ℃ of water-baths and is incubated 30 minutes, takes out in the rearmounted ice-water bath and places 5 minutes, takes out, and is blank with the corresponding reagent; According to ultraviolet spectrophotometry, measure trap at the wavelength place of 490nm, be vertical coordinate with the trap, concentration is abscissa, the drawing standard curve;
The algoscopy precision is measured product of the present invention, extracting in water or dilution, and precision is measured and is put in the tool plug test tube, add 4% phenol solution 1ml, mixing adds sulphuric acid 7.0ml rapidly, shake up, put in 40 ℃ of water-baths and be incubated 30 minutes, take out in the rearmounted ice-water bath and placed 5 minutes, taking out, is blank with the corresponding reagent, according to ultraviolet spectrophotometry, wavelength place at 490nm measures trap, from the weight that standard curve is read astragalus polysaccharides the need testing solution, calculate, promptly;
E, gas chromatography determination cantharidin content
Chromatographic condition and system suitability test are fixative with methyl silicone rubber SE-30, and coating concentration is 3.5%; Column temperature is 165 ± 10 ℃; Number of theoretical plate is pressed the cantharidin peak and is calculated, and should be not less than 2500;
It is an amount of that the cantharidin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and chlorination is copied into reference substance solution;
The preparation precision of need testing solution is measured product of the present invention, put in the separatory funnel, add water saturated chloroform jolting and extract 4 times, the filter paper of extracting solution through being covered with a small amount of anhydrous sodium sulfate filters combined chloroform liquid, put water-bath below 60 ℃ and boil off chloroform to surplus about 10ml, naturally wave and be dissipated to 2-3ml, quantitatively be transferred in the measuring bottle, add chloroform and be diluted to scale, shake up, promptly;
Algoscopy precision is respectively got reference substance solution, and need testing solution is annotated people's gas chromatograph, measures, and calculates, promptly.
Above method can be used separately, also can unite use, as long as can reach testing goal.
Pharmaceutical composition of the present invention has good anticancer antitumor action, the inventor is aspect the selection and compatibility thereof of crude drug, carried out series of experiment research, by the side's of tearing open experimental study, determined the crude drug composition of preparation medicine of the present invention, make it compared with prior art have significantly outstanding curative effect advantage, realized the potentiation purpose of compatible combination.
Verify that below by in-vitro pharmacological experiments this prescription injection is in the effect aspect the immunostimulant:
Medicine: injection of the present invention, make by oneself by optimum process of the present invention by invention.Ad pro injection, benefit hundred pharmaceutical Co. Ltds in Guizhou produce.
Laboratory animal: healthy, male, 6 week ages, closed colony KM Mus, body weight 18～22g in 6～8 ages in week, is provided by Beijing's animal center.
H22 hepatoma cell strain, H22 ascitic type cell strain are available from consonance medical university of Chinese Academy of Medical Sciences institute of materia medica.
Reagent and instrument: the flat Tissue Culture Plate of RPMI1640 culture fluid and 96 holes (the magnificent biological company limited in Shanghai); FCS (GIBCOBRL company); C02 constant temperature incubator (MODEL2300 SHELDOMANUFACTUERINGINC); MTT (the magnificent biological product in Shanghai engineering company), the flat Tissue Culture Plate in 96 holes.
Inoculation and grouping: aseptic extraction lotus hepatocarcinoma (H22) mouse peritoneal hydrops is diluted to PBS and contains oncocyte 1 * 10
7Ml, the right groin subcutaneous vaccination of every Mus 0.1ml is divided into lotus tumor model group, positive control (5-FU) group, Ai Di treatment group, injection group of the present invention and normal group, 6 every group at random with mice.
Begin administration behind the medication mouse inoculation oncocyte 24h, normal group and lotus tumor model group only gavage cold PBS0.5ml/ every day; Positive controls lumbar injection 5-FU0.2ml/ only, the next day 1 time; Ai Di treatment group lumbar injection every day ad pro injection 0.5ml/ only; Of the present invention group lumbar injection every day injection 0.5ml/ of the present invention, successive administration 12 days.
12h after the last administration of collection of specimens adopts and plucks eyeball depletion method execution mice, and body weight, the thymic weight of KM Mus respectively organized in weighing, peel off tumor tissues and weigh, and the aseptic spleen of getting weighed.
Monitoring index NK cytoactive is measured: the improvement mtt assay detects.
Statistical procedures SPSS10.0 statistical software carries out date processing, the t check, and P＜0.05 is the significance standard.
Table 1 injection of the present invention is to the influence of tumor-bearing mice NK cytoactive
| Group | N | The NK cytoactive |
| Normal group lotus tumor model group 5-FU group Ai Di treatment group | 6 6 6 6 | 34.42±3.53 32.75±3.14 17.89±2.47 40.09±3.25 △ |
| Of the present invention group | 6 | 44.88±2.94 △ |
Compare with normal group: Δ P＜0.05
Table 2 injection of the present invention is to the influence of tumor-bearing mice body weight, tumor weight, thymic weight and spleen weight
| Group | n | Body weight (g) | Thymus index (mg/g) | Index and spleen index (mg/g) | Tumor heavy (g) |
| Of the present invention group of normal group lotus knurl model group 5-FU group Ai Di treatment group | 6 6 6 6 6 | 20.55±1.76 21.67±3.12 19.48±2.54 △* 24.20±1.83 △* 22.97±1.66 △ | 3.44±1.27 2.62±0.54 1.70±0.19 △* 3.05±0.87 3.44±0.94 * | 8.22±3.28 7.78±2.53 6.45±2.53 △ 9.52±2.29 △* 9.45±2.02 △* | 0 1.66±0.43 0.74±0.34 * 0.90±0.47 * 0.93±0.22 * |
Compare with normal group: Δ P＜0.05; Compare with lotus tumor model group: * P＜0.05
Concrete case study on implementation
Embodiment 1:
Prescription: Radix Astragali 5kg Mylabris 600g
Method for making: get the Radix Astragali, decoct with water 3 times, after merging water liquid concentrates, add equivalent ethanol precipitate with ethanol, get supernatant and reclaim ethanol, surplus water liquid adds 4 times of amount ethanol secondary precipitate with ethanol, get supernatant and reclaim ethanol, add water saturated n-butanol extraction 5 times in the surplus water liquid, merge n-butanol extracting liquid, be recycled to dried, pass through strong base resin anion (R.A.) post behind the water dissolution, collect effluent, concentrate, add the starch drying.Get the precipitation of above-mentioned secondary precipitate with ethanol, be dissolved in water, the activated carbon decolorizing of adding 1.0% 5 times concentrates, and adds the starch drying; Get Mylabris, be broken into fine powder, add volume ratio and be 1: 30 hydrochloric acid acetone mixed liquor merceration 4 times, leachate reclaims acetone to saturation, cold put to make separate out crystallization, crystallization is dissolved in acetone after with petroleum ether, it is muddy to occurring to add alkaline dehydrated alcohol, cold preservation filters, and gets the filtering residue cold drying.Get cantharidin and be mixed to 300g with back and total saponin extracts, total polysaccharide extractive, incapsulate 1000 with 8 times of amount betacyclodextrin bags.
Embodiment 2:
Prescription: Radix Astragali 4kg Mylabris 10g
Method for making: get the Radix Astragali, decoct with water 3 times, after merging water liquid concentrates, add equivalent ethanol precipitate with ethanol, get supernatant and reclaim ethanol, surplus water liquid adds 4 times of amount ethanol secondary precipitate with ethanol, gets supernatant and reclaims ethanol, add water saturated n-butanol extraction 5 times in the surplus water liquid, merge n-butanol extracting liquid, be recycled to dried, behind the water dissolution by strong base resin anion (R.A.) post, collect effluent, standby.Get the precipitation of above-mentioned secondary precipitate with ethanol, be dissolved in water, add papain hydrolysis protein (40 ℃ of water temperatures, hydrolysis time 6 hours), boil enzyme extremely, add 4 times of amount dehydrated alcohol precipitation polysaccharide, the activated carbon decolorizing of adding 1.0% behind the water dissolution 5 times, standby; Get Mylabris, be broken into fine powder, add volume ratio and be 1: 40 hydrochloric acid acetone mixed liquor merceration 5 times, leachate reclaims acetone to saturation, cold put to make separate out crystallization, crystallization is dissolved in acetone after with petroleum ether, it is muddy to occurring to add alkaline dehydrated alcohol, cold preservation filters, and gets the filtering residue cold drying.Above-mentioned total saponins aqueous solution is added injection be diluted with water to the solution that every 1ml contains total saponins 0.5mg, add that Mylabris extract is warm to make dissolving,, collect filtered solution, as solution A by the ultrafilter membrane of molecular weight 10,000; Above-mentioned total polysaccharides extracting solution is added injection be diluted with water to the solution that every 1ml contains total polysaccharides 10mg, add 0.2% active carbon, boil, keep little and boiled 30 minutes, filter, take off charcoal, as solution B; Mixed in equal amounts solution A and B, adjust pH to 6.0, fill injection, every bottle of 10ml.
Embodiment 3:
Prescription: Radix Astragali 2kg Mylabris 50g
Method for making: get the Radix Astragali, decoct with water 2 times, after water liquid concentrates, add equivalent ethanol precipitate with ethanol, get supernatant and reclaim ethanol, surplus water liquid adds 3 times of amount ethanol secondary precipitate with ethanol, filters, and precipitates standby; Supernatant reclaims ethanol, surplus water liquid adds water saturated n-butanol extraction 4 times, merge n-butanol extracting liquid, be recycled to dried, residue with water dissolution after by the AB-8 macroporous adsorptive resins, it is colourless to be washed till effluent with distilled water, reuse 30% ethanol elution remove impurity, reuse 70% ethanol elution is collected 70% ethanol elution part to colourless, drying promptly obtains the Radix Astragali total saponins extract.Get the precipitation of above-mentioned secondary precipitate with ethanol, be dissolved in water, the activated carbon decolorizing of adding 1.5% 5 times gets total polysaccharide extractive, and is standby; Get Mylabris, be broken into fine powder, add volume ratio and be 1: 50 hydrochloric acid acetone mixed liquor merceration 5 times, leachate reclaims acetone to saturation, cold put to make separate out crystallization, crystallization is dissolved in acetone after with petroleum ether, it is muddy to occurring to add alkaline dehydrated alcohol, cold preservation filters, and gets the filtering residue cold drying.Above-mentioned total saponins is added injection be diluted with water to the solution that every 1ml contains total saponins 0.4mg, add that Mylabris extract is warm to make dissolving,, collect filtered solution, as solution A by the ultrafilter membrane of molecular weight 10,000; Above-mentioned total polysaccharides extracting solution is added injection be diluted with water to the solution that every 1ml contains total polysaccharides 8mg, add 0.2% active carbon, boil, keep little and boiled 30 minutes, filter, take off charcoal, as solution B; Mixed in equal amounts solution A and B, adjust pH to 6.0, fill injection, every bottle of 10ml.
Embodiment 4:
Prescription: Radix Astragali 3.5kg Mylabris 30g
Method for making: get the Radix Astragali, decoct with water 3 times, after merging water liquid concentrates, add equivalent ethanol precipitate with ethanol, get supernatant and reclaim ethanol, surplus water liquid adds 4 times of amount ethanol secondary precipitate with ethanol, gets supernatant and reclaims ethanol, add water saturated n-butanol extraction 5 times in the surplus water liquid, merge n-butanol extracting liquid, be recycled to dried, behind the water dissolution by strong base resin anion (R.A.) post, collect effluent, standby.Get the precipitation of above-mentioned secondary precipitate with ethanol, be dissolved in water, the activated carbon decolorizing of adding 2.0% 3 times, standby; Get Mylabris, be broken into fine powder, add volume ratio and be 1: 40 hydrochloric acid acetone mixed liquor merceration 3 times, leachate reclaims acetone to saturation, cold put to make separate out crystallization, crystallization is dissolved in acetone after with petroleum ether, it is muddy to occurring to add alkaline dehydrated alcohol, cold preservation filters, and gets the filtering residue cold drying.Above-mentioned total saponins aqueous solution is added injection be diluted with water to the solution that every 1ml contains total saponins 1mg, add that Mylabris extract is warm to make dissolving,, collect filtered solution, as solution A by the ultrafilter membrane of molecular weight 10,000; Above-mentioned total polysaccharides extracting solution is added injection be diluted with water to the solution that every 1ml contains total polysaccharides 15mg, add 0.5% active carbon, boil, keep little and boiled 30 minutes, filter, take off charcoal, as solution B; Mixed in equal amounts solution A and B, adjust pH to 6.0, fill injection, every bottle of 2ml.
Embodiment 5:
Prescription: Radix Astragali 3kg Mylabris 40g
Method for making: get the Radix Astragali, decoct with water 3 times, after merging water liquid concentrates, add equivalent ethanol precipitate with ethanol, get supernatant and reclaim ethanol, surplus water liquid adds 4 times of amount ethanol secondary precipitate with ethanol, get supernatant and reclaim ethanol, add water saturated n-butanol extraction 5 times in the surplus water liquid, merge n-butanol extracting liquid, be recycled to driedly, by AB-8 type macroporous resin column, distilled water is eluted to colourless behind the water dissolution, 30% ethanol elution is removed the flavonoid impurity component, collect 70% ethanol elution part, reclaim ethanol, water liquid is standby.Get the precipitation of above-mentioned secondary precipitate with ethanol, be dissolved in water, the activated carbon decolorizing of adding 1.0% 5 times, standby; Get Mylabris, be broken into fine powder, add volume ratio and be 1: 30～50 hydrochloric acid acetone mixed liquor merceration 3～5 times, leachate reclaims acetone to saturation, cold put to make separate out crystallization, crystallization is dissolved in acetone after with petroleum ether, it is muddy to occurring to add alkaline dehydrated alcohol, cold preservation filters, and gets the filtering residue cold drying.Above-mentioned total saponins aqueous solution is added injection be diluted with water to the solution that every 1ml contains total saponins 0.4mg,, collect filtered solution, add that Mylabris extract is warm to make dissolving, as solution A by the ultrafilter membrane of molecular weight 10,000; Above-mentioned total polysaccharides extracting solution is added injection be diluted with water to the solution that every 1ml contains total polysaccharides 8mg, add 0.2% active carbon, boil, keep little and boiled 30 minutes, filter, take off charcoal, as solution B; Mixed in equal amounts solution A and B, adjust pH to 6.0, fill injection, every bottle of 10ml.
Embodiment 6:
Ultraviolet spectrophotometry is surveyed Radix Astragali total saponins content in the injection
The preparation precision of reference substance solution takes by weighing the astragaloside reference substance, adds dissolve with methanol and makes the solution that every 1ml contains 0.5mg, promptly;
The accurate absorption of the preparation of standard allusion quotation line reference substance solution 20,40,60,80,100ul place 10ml tool plug test tube respectively, put and wave most solvent in the water-bath, take out immediately, put coldly, precision adds 5% vanillin-glacial acetic acid solution 0.2ml, perchloric acid 0.8ml, shake up, put in 60 ℃ of water-baths and heated 15 minutes, take out, immediately with circulating water cooling 2 minutes, precision adds glacial acetic acid 5ml, shaking up, is blank with the reagent corresponding, according to spectrophotography, wavelength place at 544nm measures trap, with the trap is vertical coordinate, and concentration is abscissa, the drawing standard curve;
The algoscopy precision is measured the present invention's product, and thin up is put in the separatory funnel, add the chloroform jolting and extract 3 times, combined chloroform liquid also washes with water 2 times, discards chloroform solution, washing liquid and above-mentioned water layer merge, and put in the separatory funnel, with water saturated n-butanol extraction 5 times, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds methanol makes dissolving, and quantitatively shift in the measuring bottle, add methanol to scale, shake up, precision is measured and is put in the tool plug test tube, put and wave most solvent in the water-bath, take out immediately, put cold, precision adds 5% vanillin-glacial acetic acid solution 0.2ml, perchloric acid 0.8ml shakes up, and puts in 60 ℃ of water-baths and heats 15 minutes, take out, with circulating water cooling 2 minutes, precision added glacial acetic acid 5ml, shakes up immediately, with the reagent corresponding is blank, according to spectrophotography, measure trap at the wavelength place of 544nm, the weight (μ g) of reading total Saponin the need testing solution from standard curve, calculate, promptly;
The every 1ml of this product contains total Saponin should be less than 0.4mg with astragaloside e calculating.
Embodiment 7:
High-efficient liquid phase technique is surveyed the content of astragaloside
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-water (35: 65) is a mobile phase; Evaporative light scattering detector.
It is an amount of that the preparation precision of reference substance solution takes by weighing the astragaloside reference substance, adds methanol and make the solution that every ml contains 0.1mg, promptly.
The preparation precision of need testing solution is measured the present invention's product, and adding methanol extraction water changes molten or thin up, puts in the separatory funnel, add the chloroform jolting and extract 3 times, combined chloroform liquid also washes with water 2 times, discards chloroform solution, washing liquid and above-mentioned water layer merge, and put in the separatory funnel, with water saturated n-butanol extraction 5 times, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds methanol makes dissolving, and quantitatively shift in the measuring bottle, add methanol to scale, shake up, promptly.
Accurate reference substance solution 5 μ l, the 15 μ l of drawing of algoscopy, need testing solution 10 μ l inject chromatograph of liquid, measure, promptly.
Embodiment 8:
The sulphuric acid anthrone method is surveyed Radix Astragali Mongolici total polysaccharide content
The preparation precision of reference substance solution takes by weighing the anhydrous glucose 80mg that is dried to constant weight through 80 ℃, puts in the 100ml measuring bottle, is dissolved in water, and is diluted to scale, shake up, precision is measured 5ml, puts in the 50ml measuring bottle, thin up shakes up to scale, makes among every 1ml to contain anhydrous glucose 0.08mg promptly.
The preparation precision of standard curve is measured reference substance solution 0.2,0.4,0.6,0.8 and 1.0ml, puts respectively in the 10ml tool plug test tube, and each is managed precision and adds water and make into 1ml, the accurate respectively sulphuric acid anthrone solution 4ml that adds in ice bath, shake up, put in the water-bath and heated 10 minutes, cool off after 40 minutes, with the corresponding reagent is blank, according to spectrophotography, measure trap at the wavelength place of 625nm, be vertical coordinate with the trap, concentration is abscissa, the drawing standard curve.Sulphuric acid anthrone solution is for getting anthrone 50mg, adds water 25ml and sulphuric acid 75ml makes dissolving, that is, face and use new system.
The algoscopy precision is measured the present invention's product, extracting in water or dilution, precision is measured and is put in the tool plug test tube, the sighting target directrix curve get under the preparation method, from " respectively manage precision add water make into 1ml ", measure absorbance, the weight (μ g) of reading astragalus polysaccharides the need testing solution from standard curve in accordance with the law, calculate, promptly.
The every 1ml of this product contains polysaccharide should be no less than 2.5mg in anhydrous glucose.
Embodiment 9:
The sulphuric acid phynol method is surveyed Radix Astragali Mongolici total polysaccharide content
The preparation precision of reference substance solution takes by weighing the anhydrous glucose that is dried to constant weight through 80 ℃, puts in the measuring bottle, is dissolved in water and is diluted to scale, shakes up, and makes behind the thin up to contain anhydrous glucose 0.6mg among every 1ml, promptly;
The preparation precision of standard curve is measured reference substance solution 0.5,1.0,1.5,2.0,2.5ml, puts respectively in the 50ml measuring bottle, adds water to scale, shakes up.Precision is measured above-mentioned solution 2ml respectively, puts in the tool plug test tube, respectively adds 4% phenol solution 1ml, and mixing adds sulphuric acid 7.0ml rapidly, shakes up, and puts in 40 ℃ of water-baths and is incubated 30 minutes, takes out in the rearmounted ice-water bath and places 5 minutes, takes out, and is blank with the corresponding reagent.According to ultraviolet spectrophotometry, measure trap at the wavelength place of 490nm, be vertical coordinate with the trap, concentration is abscissa, the drawing standard curve.
The algoscopy precision is measured the present invention's product, extracting in water or dilution, precision is measured and is put in the tool plug test tube, the sighting target directrix curve get under the preparation method, from " respectively adding 4% phenol solution 1ml ", measure absorbance, the weight (μ g) of reading astragalus polysaccharides the need testing solution from standard curve in accordance with the law, calculate, promptly.
The every 1ml of this product contains polysaccharide should be no less than 2.5mg in anhydrous glucose.
Embodiment 10:
The assay of cantharidin
According to gas chromatography determination.
Chromatographic condition and system suitability test are fixative with methyl silicone rubber SE-30, and coating concentration is 3.5%; Column temperature is 165 ± 10 ℃; Number of theoretical plate is pressed the cantharidin peak and is calculated, and should be not less than 2500.
It is an amount of that the cantharidin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and chlorination is copied into 1ml and contained the 0.5mg reference substance solution.
The preparation precision of need testing solution is measured this product 50ml, put in the separatory funnel, add 1.8mol/L sulfuric acid solution 5ml, extract 4 times with water saturated chloroform jolting, the filter paper of extracting solution through being covered with a small amount of anhydrous sodium sulfate filters, combined chloroform liquid is put water-bath below 60 ℃ and is boiled off chloroform to surplus about 10ml, waves naturally and is dissipated to 2-3ml, quantitatively be transferred in the 5ml measuring bottle, add chloroform and be diluted to scale, shake up, promptly.
Algoscopy precision is respectively got reference substance solution, and need testing solution is annotated people's gas chromatograph, measures, and calculates, promptly.
The every 1ml of this product contains cantharidin (C10H12O4), should be 0.8～8 μ g.
Claims (10)
1, a kind of pharmaceutical composition that is used for the treatment of tumor disease is characterized in that this pharmaceutical composition made by following raw material medicaments: the Radix Astragali 50～400 weight portions, Mylabris 1～6 weight portion.
2, pharmaceutical composition as claimed in claim 1 is characterized in that the optimum ratio of each crude drug is: the Radix Astragali 200～350 weight portions, Mylabris 3～5 weight portions.
3, pharmaceutical composition as claimed in claim 2 is characterized in that the optimal proportion of each crude drug is: the Radix Astragali 300 weight portions, Mylabris 4 weight portions.
4, as pharmaceutical composition as described in the claim 1,2 or 3, it is characterized in that the extract that each crude drug also can identical conversion amount feeds intake, wherein Radix Astragali total saponins accounts for more than 50% of total solid in the Radix Astragali total saponins extract, and Radix Astragali Mongolici total polysaccharide accounts for more than 50% of total solid in the Radix Astragali Mongolici total polysaccharide extract; Mylabris extract then is the white crystalline powder that obtains with organic solvent extraction, and wherein cantharidin accounts for more than 80% of total solid.
5, compositions as claimed in claim 4 is characterized in that being made in capsule, the injection any.
6, as preparation of drug combination method as described in the claim 5, it is characterized in that this method realizes by following technical process:
A, get the Radix Astragali, decoct with water, after water liquid concentrates, add equivalent ethanol precipitate with ethanol, get supernatant and reclaim ethanol, surplus water liquid adds 3～5 times of amount ethanol secondary precipitate with ethanol, filters, and precipitates standby; Supernatant reclaims ethanol, adds water saturated n-butanol extraction 3～5 times in the surplus water liquid, merges n-butanol extracting liquid, be recycled to dried, residue with water dissolution after by strong base resin anion (R.A.) post, use the distilled water eluting, collect effluent, promptly obtain the Radix Astragali total saponins extract solution;
B, get precipitate standby among a, be dissolved in water, the activated carbon decolorizing that adds 0.2%～2% water liquid weight for several times, and is basicly stable to water liquid color, filters, and promptly obtains the Radix Astragali Mongolici total polysaccharide aqueous solution;
C, get Mylabris, be broken into fine powder, add volume ratio and be 1: 30～1: 50 hydrochloric acid acetone mixed liquor merceration 3～5 times, leachate reclaims acetone to saturation, cold put to make separate out crystallization, crystallization is dissolved in acetone after with petroleum ether, add alkaline dehydrated alcohol to muddy, cold preservation filters, get filtering residue, obtain Mylabris extract;
D, above three kinds of extracts are mixed after, add suitable adjuvant, make required dosage form.
7, as preparation method as described in the claim 6, it is characterized in that step a also can be: get the Radix Astragali, decoct with water, after water liquid concentrates, add equivalent ethanol precipitate with ethanol, get supernatant and reclaim ethanol, surplus water liquid adds 3～5 times of amount ethanol secondary precipitate with ethanol, filters, and precipitates standby; Supernatant reclaims ethanol, surplus water liquid adds water saturated n-butanol extraction 3～5 times, merge n-butanol extracting liquid, be recycled to dried, residue with water dissolution after by the AB-8 macroporous adsorptive resins, it is colourless to be washed till effluent with distilled water, reuse 30% ethanol elution remove impurity, reuse 70% ethanol elution is collected 70% ethanol elution part to colourless, drying promptly obtains the Radix Astragali total saponins extract.
8, as preparation of drug combination method as described in claim 6 or 7, the preparation process that it is characterized in that injection is: get Mylabris extract and be dissolved in the Radix Astragali total saponins aqueous solution, ultrafilter membrane by molecular weight 10,000, collect filtration fraction water liquid, mix the Radix Astragali Mongolici total polysaccharide aqueous solution, adjust pH to 4.0～6.5, be dissolved into an amount of stabilizing agent, add the injection water to total amount, sterilization, promptly.
9,, it is characterized in that this method contains following each or several as the method for quality control of pharmaceutical composition as described in the claim 5:
A, ultraviolet spectrophotometry are surveyed Radix Astragali total saponins content
The preparation precision of reference substance solution takes by weighing the astragaloside reference substance, adds methanol and quantitatively dissolves, and be diluted to scale, shakes up, promptly;
The accurate absorption of the preparation of standard allusion quotation line reference substance solution 20,40,60,80,100ul place 10ml tool plug test tube respectively, put and wave most solvent in the water-bath, take out immediately, put coldly, precision adds 5% vanillin-glacial acetic acid solution 0.2ml, perchloric acid 0.8ml, shake up, put in 60 ℃ of water-baths and heated 15 minutes, take out, immediately with circulating water cooling 2 minutes, precision adds glacial acetic acid 5ml, shaking up, is blank with the reagent corresponding, according to spectrophotography, wavelength place at 544nm measures trap, with the trap is vertical coordinate, and concentration is abscissa, the drawing standard curve;
The algoscopy precision is measured product of the present invention, and adding methanol extraction water changes molten or thin up, puts in the separatory funnel, add the chloroform jolting and extract 3 times, combined chloroform liquid also washes with water 2 times, discards chloroform solution, washing liquid and above-mentioned water layer merge, and put in the separatory funnel, with water saturated n-butanol extraction 5 times, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds methanol makes dissolving, and quantitatively shift in the measuring bottle, add methanol to scale, shake up, precision is measured and is put in the tool plug test tube, put and wave most solvent in the water-bath, take out immediately, put cold, precision adds 5% vanillin-glacial acetic acid solution 0.2ml, perchloric acid 0.8ml shakes up, and puts in 60 ℃ of water-baths and heats 15 minutes, take out, with circulating water cooling 2 minutes, precision added glacial acetic acid 5ml, shakes up immediately, with the reagent corresponding is blank, according to spectrophotography, measure trap at the wavelength place of 544nm, the weight of reading total Saponin the need testing solution from standard curve, calculate, promptly;
B, high-efficient liquid phase technique are surveyed the content of astragaloside
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Volume ratio is that 35: 65 acetonitrile-water is a mobile phase; Evaporative light scattering detector;
It is an amount of that the preparation precision of reference substance solution takes by weighing the astragaloside reference substance, adds methanol and make solution, promptly;
The preparation precision of need testing solution is measured the present invention's product, and adding methanol extraction water changes molten or thin up, puts in the separatory funnel, add the chloroform jolting and extract 3 times, combined chloroform liquid also washes with water 2 times, discards chloroform solution, washing liquid and above-mentioned water layer merge, and put in the separatory funnel, with water saturated n-butanol extraction 5 times, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds methanol makes dissolving, and quantitatively shift in the measuring bottle, add methanol to scale, shake up, promptly;
Accurate reference substance solution 5 μ l, the 15 μ l of drawing of algoscopy, need testing solution 10 μ l inject chromatograph of liquid, measure, promptly;
C, sulphuric acid anthrone method are surveyed Radix Astragali Mongolici total polysaccharide content
The preparation precision of reference substance solution takes by weighing the anhydrous glucose that is dried to constant weight through 80 ℃, puts in the measuring bottle, is dissolved in water and is diluted to scale, shakes up, and makes behind the thin up to contain anhydrous glucose 0.08mg among every 1ml, promptly;
The preparation precision of standard curve is measured reference substance solution 0.2,0.4,0.6,0.8 and 1.0ml, puts respectively in the 10ml tool plug test tube, and each is managed precision and adds water and make into 1ml, the accurate respectively sulphuric acid anthrone solution 4ml that adds in ice bath, shake up, put in the water-bath and heated 10 minutes, cool off after 40 minutes, with the corresponding reagent is blank, according to ultraviolet spectrophotometry, measure trap at the wavelength place of 625nm, be vertical coordinate with the trap, concentration is abscissa, the drawing standard curve; Wherein sulphuric acid anthrone solution is for getting anthrone 50mg, adds water 25ml and sulphuric acid 75ml makes dissolving, that is, face and use new system;
The algoscopy precision is measured product of the present invention, extracting in water or dilution, and precision is measured and is put in the tool plug test tube, precision adds water makes into 1ml, and the accurate sulphuric acid anthrone solution 4ml that adds shakes up in ice bath, put in the water-bath and heated 10 minutes, cooling off after 40 minutes, is blank with the corresponding reagent, according to ultraviolet spectrophotometry, wavelength place at 625nm measures trap, from the weight that standard curve is read astragalus polysaccharides the need testing solution, calculate, promptly;
D, sulphuric acid phynol method are surveyed Radix Astragali Mongolici total polysaccharide content
The preparation precision of reference substance solution takes by weighing the anhydrous glucose that is dried to constant weight through 80 ℃, puts in the measuring bottle, is dissolved in water and is diluted to scale, shakes up, and makes behind the thin up to contain anhydrous glucose 0.6mg among every 1ml, promptly;
The preparation precision of standard curve is measured reference substance solution 0.5,1.0,1.5,2.0,2.5ml, puts respectively in the 50ml measuring bottle, adds water to scale, shakes up; Precision is measured above-mentioned solution 2ml respectively, puts in the tool plug test tube, respectively adds 4% phenol solution 1ml, and mixing adds sulphuric acid 7.0ml rapidly, shakes up, and puts in 40 ℃ of water-baths and is incubated 30 minutes, takes out in the rearmounted ice-water bath and places 5 minutes, takes out, and is blank with the corresponding reagent; According to ultraviolet spectrophotometry, measure trap at the wavelength place of 490nm, be vertical coordinate with the trap, concentration is abscissa, the drawing standard curve;
The algoscopy precision is measured product of the present invention, extracting in water or dilution, and precision is measured and is put in the tool plug test tube, add 4% phenol solution 1ml, mixing adds sulphuric acid 7.0ml rapidly, shake up, put in 40 ℃ of water-baths and be incubated 30 minutes, take out in the rearmounted ice-water bath and placed 5 minutes, taking out, is blank with the corresponding reagent, according to ultraviolet spectrophotometry, wavelength place at 490nm measures trap, from the weight that standard curve is read astragalus polysaccharides the need testing solution, calculate, promptly;
E, gas chromatography determination cantharidin content
Chromatographic condition and system suitability test are fixative with methyl silicone rubber SE-30, and coating concentration is 3.5%; Column temperature is 165 ± 10 ℃; Number of theoretical plate is pressed the cantharidin peak and is calculated, and should be not less than 2500;
It is an amount of that the cantharidin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and chlorination is copied into reference substance solution;
The preparation precision of need testing solution is measured product of the present invention, put in the separatory funnel, add 1.8mol/L sulfuric acid solution 5ml, extract 4 times with water saturated chloroform jolting, the filter paper of extracting solution through being covered with a small amount of anhydrous sodium sulfate filters, combined chloroform liquid is put water-bath below 60 ℃ and is boiled off chloroform to surplus about 10ml, waves naturally and is dissipated to 2-3ml, quantitatively be transferred in the measuring bottle, add chloroform and be diluted to scale, shake up, promptly;
Algoscopy precision is respectively got reference substance solution, and need testing solution is annotated people's gas chromatograph, measures, and calculates, promptly.
10, be used for the treatment of application in the medicine of tumor disease as pharmaceutical composition as described in arbitrary in the claim 1 to 4 in preparation.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101940793B (en) * | 2009-07-03 | 2012-10-31 | 中国医学科学院药用植物研究所 | Hydroxypropyl-beta-cyclodextrin clathrate compound of cantharidin and cantharis extractive and preparation method thereof |
| CN105606556A (en) * | 2016-01-28 | 2016-05-25 | 广西壮族自治区中医药研究院 | Ultraviolet spectrophotometry for polysaccharide content in medicine material fokien angiopteris rhizomes |
| CN111257254A (en) * | 2020-03-19 | 2020-06-09 | 中国水产科学研究院黄海水产研究所 | Method for measuring glycogen content in oyster tissue |
-
2006
- 2006-04-13 CN CNA2006100769673A patent/CN101053587A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101940793B (en) * | 2009-07-03 | 2012-10-31 | 中国医学科学院药用植物研究所 | Hydroxypropyl-beta-cyclodextrin clathrate compound of cantharidin and cantharis extractive and preparation method thereof |
| CN105606556A (en) * | 2016-01-28 | 2016-05-25 | 广西壮族自治区中医药研究院 | Ultraviolet spectrophotometry for polysaccharide content in medicine material fokien angiopteris rhizomes |
| CN105606556B (en) * | 2016-01-28 | 2018-09-21 | 广西壮族自治区中医药研究院 | The ultraviolet spectrophotometry of polyoses content in fokien angiopteris rhizome medicinal material |
| CN111257254A (en) * | 2020-03-19 | 2020-06-09 | 中国水产科学研究院黄海水产研究所 | Method for measuring glycogen content in oyster tissue |
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