CN101732466B - Method for controlling quality of Guipi granules - Google Patents
Method for controlling quality of Guipi granules Download PDFInfo
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Abstract
The invention relates to 'a method for controlling the quality of Guipi granules', which belongs to the field of medicament quality control. The method for controlling the quality of Guipi granules comprises the following steps: observing properties, identifying contents, checking the contents according to a method of pharmacopoeia, and measuring the content of ammonium glycyrrhizinate serving as an active ingredient. The quality of the Guipi granules is comprehensively controlled by using visual sense, the detection by using reference medicaments and the measuring of the ammonium glycyrrhizinate serving as an active ingredient, so that the potency of the product is controlled effectively.
Description
This application is that patent name is dividing an application of " a kind of spleen granule, oral liquid and concentrated pill and their method for preparing and method of quality control of returning ", application number are 200710143907.3, the applying date is on August 13rd, 2007 patent of invention.
Technical field
The present invention relates to the Chinese medicine field of pharmaceutical preparations, particularly a kind of have replenishing QI to invigorate the spleen, a nourishing blood to tranquillize the mind.Be used for deficiency of both the heart and spleen, the cardiopalmus of breathing hard, insomnia and dreamful sleep, dizzy dizzy, lassitude of the limbs and weakness, the Chinese medicine preparation of inappetence.Said preparation is to be processed by raw material of Chinese medicine such as Radix Codonopsis, the Rhizoma Atractylodis Macrocephalae, the Radix Astragali, Radix Glycyrrhizae, Poria, Radix Polygalae, Semen Ziziphi Spinosae, Arillus Longan, Radix Angelicae Sinensis, the Radix Aucklandiae, Fructus Jujubaes.
Background technology
GUIPI TANG comes from recipes for Saving Lives; GUIPI WAN is made up of Radix Codonopsis, the Rhizoma Atractylodis Macrocephalae (stir-fry), the Radix Astragali (processed with honey), Radix Glycyrrhizae (processed with honey), Poria, Radix Polygalae (system), Semen Ziziphi Spinosae (stir-fry), Arillus Longan, Radix Angelicae Sinensis, the Radix Aucklandiae, Fructus Jujubae Chinese medicines such as (enucleations); For one one of the Pharmacopoeia of the People's Republic of China (1995 editions) records; Be big honeyed pills, small honey pill or water-honeyed pill; Function with replenishing QI to invigorate the spleen, nourishing blood to tranquillize the mind, card such as be used for deficiency of both the heart and spleen, the cardiopalmus of breathing hard, insomnia and dreamful sleep, dizzy dizziness, lassitude of the limbs and weakness, inappetence, metrorrhagia are had blood in stool, because of former preparation big honeyed pills, small honey pill, water-honeyed pill and the watered pill etc. be Chinese herbal medicine directly pulverizing process; Quality is coarse, impurity content is many, dose is big, take inconvenience, absorb slow, difficult quality control, and curative effect is restricted.
The present invention provides a kind of spleen granule, oral liquid and concentrated pill preparation of returning, and using under the situation of original prescription, technology is improved, and makes through carrying out quality control in the production process that to reach product stable.
Through technological transformation, with modern Chinese medicine extractive technique and preparation technique, be equipped with special adjuvant and processed and return spleen granule, oral liquid and concentrated pill preparation, overcome the defective of prior art.And its curative effect and quality studied, obtained satisfied effect: dose is little, taking convenience, and mouthfeel is good, and patient compliance is good, and method of quality control is advanced, steady quality, curative effect obviously is superior to former pill.
Summary of the invention
The object of the present invention is to provide a kind of spleen granule, oral liquid and concentrated pill preparation and preparation method thereof of returning.
Spleen granule, oral liquid and the concentrated pill preparation of returning of the present invention is to be processed by following parts by weight of Chinese traditional medicine raw material:
Radix Codonopsis 70-280g Rhizoma Atractylodis Macrocephalae 140-560g Radix Astragali 70-280g Radix Glycyrrhizae 35-140g
Poria 140-560g Radix Polygalae 140-560g Semen Ziziphi Spinosae 70-280g Arillus Longan 140-560g
Radix Angelicae Sinensis 140-560g Radix Aucklandiae 35-140g Fructus Jujubae 35-140g
Its preparation method is following:
More than ten simply, pulverize or be chopped into suitable granule, the little dynamic reflux, extract, secondary that boils of water; Add for the first time 5-12 times of water gaging and extracted 1-2 hour, add 5-12 times of water gaging for the second time and extracted 0.5-1.5 hour, merge medicinal liquid; Filter; Filtrate decompression is concentrated into the extractum of relative density 1.05-1.15 (50 ℃), filters, and filtrating adds suitable adjuvant and is prepared into granule, oral liquid or concentrated pill preparation.
Preferred Recipe is following:
Radix Codonopsis 140g Rhizoma Atractylodis Macrocephalae 280g Radix Astragali 140g Radix Glycyrrhizae 70g
Poria 280g Radix Polygalae 280g Semen Ziziphi Spinosae 140g Arillus Longan 280g
Radix Angelicae Sinensis 280g Radix Aucklandiae 70g Fructus Jujubae 70g
More than ten simply, pulverize or be chopped into suitable granule, the little dynamic reflux, extract, secondary that boils of water; Add for the first time 10 times of water gagings and extracted 1 hour, add 5 times of water gagings for the second time and extracted 0.5 hour, merge medicinal liquid; Filter; Filtrate decompression is concentrated into the extractum of relative density 1.05-1.15 (50 ℃), filters, and filtrating adds suitable adjuvant and is prepared into granule, oral liquid or concentrated pill preparation.
Most preferred Recipe is following:
The Radix Codonopsis 140g Rhizoma Atractylodis Macrocephalae (stir-fry) the 280g Radix Astragali (processed with honey) 140g Radix Glycyrrhizae (processed with honey) 70g
Poria 280g Radix Polygalae (system) 280g Semen Ziziphi Spinosae (stir-fry) 140g Arillus Longan 280g
Radix Angelicae Sinensis 280g Radix Aucklandiae 70g Fructus Jujubae (enucleation) 70g
Suitable granule is pulverized or be chopped into to [technology] above ten, the little dynamic reflux, extract, secondary that boils of water simply; Add for the first time 10 times of water gagings and extracted 1 hour, add 5 times of water gagings for the second time and extracted 0.5 hour, merge medicinal liquid; Filter; Filtrate decompression is concentrated into the extractum of relative density 1.05-1.15 (50 ℃), filters, and filtrating adds suitable adjuvant and is prepared into granule, oral liquid or concentrated pill preparation.
More than in the prescription raw material of Chinese medicine like the Rhizoma Atractylodis Macrocephalae (stir-frys), the Radix Astragali (processed with honey), Radix Glycyrrhizae (processed with honey), Radix Polygalae (system), Semen Ziziphi Spinosae (stir-fry), employing such as Fructus Jujubae (enucleation) Chinese medicine processing technique is processed the process of preparing Chinese medicine to raw material and is obtained, and on market, can buy.
Adjuvant is selected from described in the above method for preparing: water, dextrin, Mel, sucrose, lactose, glycyrrhizic acid, stevioside, sorbic acid, benzoic acid, sodium benzoate, methyl hydroxybenzoate, ethyl hydroxybenzoate, propylparaben, butoben.
The present invention proposes new method for preparing, and this method adopts water to carry, under the prerequisite that adopts dynamic little reflux, extract, of boiling; With extraction time, water consumption, extraction time are factor, respectively establish three horizontal L9 (32) orthogonal experiment scheme; With dry extract put forward rate, ammonium glycyrrhizinate content is index, and extraction effect is compared, the result adds 10 times of water gagings with the granule medical material and soaked 1 hour; 98-99 ℃ of dynamic reflux, extract, 1 hour, leaching medicinal liquid, medicinal residues add 5 times of dynamic reflux, extract, of water gaging again and are best extraction process half an hour; Simultaneously relevant environmental condition and the granulation condition that is prepared into granule made an experiment, found preferred plan.
The present invention also according to the characteristics of returning spleen granule, oral liquid and concentrated pill preparation, has formulated product inspection method, and this method may further comprise the steps:
Character is observed, content is differentiated, official method is checked content, and the effective ingredient monoammonium glycyrrhizinate that contains is carried out assay.
For granule:
Wherein character is observed, step is:
[character] these article are brown or tan granule; Gas is fragrant, sweet in the mouth, little hardship.
Wherein content is differentiated, step is:
These article 10g is got in [discriminating] (1), adds methanol 30ml, and merceration spends the night, and supersound process 15 minutes filters; Residue adds methanol 10ml, and washing filters merging filtrate, evaporate to dryness; Residue adds water 15ml while hot makes dissolving, puts coldly, extracts 2 times each 15ml with the ether jolting; Merge ether solution, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material 1g, shines medical material solution in pairs with legal system.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With normal hexane-ethyl acetate (9: 1) is developing solvent, launches, and takes out; Dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.(2) get these article 20g, add methanol 50ml, merceration spends the night, and puts in the water-bath and refluxes 30 minutes, filters; The filtrating evaporate to dryness, residue adds water 20ml while hot makes dissolving, puts coldly, extracts 2 times with the ether jolting, at every turn 25ml; Combined ether liquid volatilizes, and residue adds methanol 0.5ml makes dissolving, as need testing solution.Other gets Radix Aucklandiae control medicinal material 0.2g, adds methanol 10ml, shines medical material solution in pairs with legal system.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw need testing solution 10 μ l, control medicinal material solution 2 μ l put respectively on same silica gel g thin-layer plate; With cyclohexane extraction-acetone (10: 3) is developing solvent, launches, and takes out; Dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.(3) in the chromatogram that under the assay item, writes down, the test sample main peak is consistent with the retention time of monoammonium glycyrrhizinate reference substance main peak.
Wherein official method checks that to content step is:
[inspection] granularity can not and can must not be crossed 15.0% (appendix XIB of Chinese Pharmacopoeia version in 2005) through the granule and the powder summation of No. five sieves through a sieve.
Moisture is measured according to aquametry (an appendix IXH of Chinese Pharmacopoeia version in 2005 three therapeutic methods of traditional Chinese medicine), must not cross 6.0%.
Other should meet each item regulation (an appendix I of Chinese Pharmacopoeia version in 2005 C) relevant under the granule item.
Wherein the effective ingredient monoammonium glycyrrhizinate that contains is carried out assay, step is:
[assay] measured according to HPLC (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filler, and methanol-water-acetic acid (69: 31: 0.5) is mobile phase; The detection wavelength is 254nm.Number of theoretical plate is pressed the monoammonium glycyrrhizinate peak and is calculated, and should be not less than 3500.
The preparation precision of reference substance solution takes by weighing through the monoammonium glycyrrhizinate reference substance of 80 ℃ of drying under reduced pressure to constant weights an amount of, adds 50% ethanol again and makes dissolving and process the solution that every 1ml contains monoammonium glycyrrhizinate 10 μ g, promptly gets.
These article porphyrize is got in the preparation of need testing solution, gets about 0.5g, and accurate the title decides, and puts in the 100ml round-bottomed flask, the accurate 50% ethanol 50ml that adds; Claim to decide weight, put in the water-bath reflux, extract, 2 hours, put coldly, weigh, supply the weight of loss with 50% ethanol; Shake up, filter, get subsequent filtrate, promptly get.
Algoscopy precision is respectively measured above-mentioned reference substance solution and is supplied each 20 μ l of examination solution, injects chromatograph of liquid, and the record chromatogram calculates, and promptly gets.
The every 1g of these article contains Radix Glycyrrhizae with monoammonium glycyrrhizinate (C
42H
63O
16N) meter must not be less than 1.17mg.
For oral liquid:
Wherein character is observed, step is:
[character] these article are brown or tan liquid; Gas is fragrant, sweet in the mouth, little hardship.
Wherein content is differentiated, step is:
These article 10ml is got in [discriminating] (1), adds methanol 30ml, and merceration spends the night, and supersound process 15 minutes filters; Residue adds methanol 10ml, and washing filters merging filtrate, evaporate to dryness; Residue adds water 15ml while hot makes dissolving, puts coldly, extracts 2 times each 15ml with the ether jolting; Merge ether solution, volatilize, residue adds methanol lml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material 1g, shines medical material solution in pairs with legal system.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With normal hexane-ethyl acetate (9: 1) is developing solvent, launches, and takes out; Dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.(2) get these article 20ml, add methanol 50ml, merceration spends the night, and puts in the water-bath and refluxes 30 minutes, filters; The filtrating evaporate to dryness, residue adds water 20ml while hot makes dissolving, puts coldly, extracts 2 times with the ether jolting, at every turn 25ml; Combined ether liquid volatilizes, and residue adds methanol 0.5ml makes dissolving, as need testing solution.Other gets Radix Aucklandiae control medicinal material 0.2g, adds methanol 10ml, shines medical material solution in pairs with legal system.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw need testing solution 10 μ l, control medicinal material solution 2 μ l put respectively on same silica gel g thin-layer plate; With cyclohexane extraction-acetone (10: 3) is developing solvent, launches, and takes out; Dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.(3) in the chromatogram that under the assay item, writes down, the test sample main peak is consistent with the retention time of monoammonium glycyrrhizinate reference substance main peak.
Wherein official method checks that to content step is:
[inspection] relative density should be not less than 1.02 (appendix VIIA)
Other should meet each item regulation (an appendix I of Chinese Pharmacopoeia version in 2005 J) relevant under the mixture item.
Wherein the effective ingredient monoammonium glycyrrhizinate that contains is carried out assay, step is:
[assay] measured according to HPLC (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filler, and methanol-water-acetic acid (69: 31: 0.5) is mobile phase; The detection wavelength is 254nm.Number of theoretical plate is pressed the monoammonium glycyrrhizinate peak and is calculated, and should be not less than 3500.The preparation precision of reference substance solution takes by weighing through the monoammonium glycyrrhizinate reference substance of 80 ℃ of drying under reduced pressure to constant weights an amount of, adds 50% ethanol again and makes dissolving and process the solution that every 1ml contains monoammonium glycyrrhizinate 10 μ g, promptly gets.
The preparation precision of need testing solution is measured these article 0.5ml, and accurate the title decides, and puts in the 100ml round-bottomed flask, and the accurate 50% ethanol 50ml that adds claims to decide weight; Put in the water-bath reflux, extract, 2 hours, and put coldly, weigh, supply the weight of loss with 50% ethanol; Shake up, filter, get subsequent filtrate, promptly get.
Algoscopy precision is respectively measured above-mentioned reference substance solution and is supplied each 20 μ l of examination solution, injects chromatograph of liquid, and the record chromatogram calculates, and promptly gets.
The every 1ml of these article contains Radix Glycyrrhizae with monoammonium glycyrrhizinate (C
42H
630
16N) meter must not be less than 1.17mg.
For concentrated pill:
Wherein character is observed, step is:
[character] these article are brown or tan concentrated pill; Gas is fragrant, sweet in the mouth, little hardship.
Wherein content is differentiated, step is:
These article 10g is got in [discriminating] (1), grinds or chopping, adds methanol 30ml, and merceration spends the night, supersound process 15 minutes; Filter, residue adds methanol 10ml, and washing filters merging filtrate; Evaporate to dryness, residue add water 15ml while hot makes dissolving, puts coldly, extracts 2 times each 15ml with the ether jolting; Merge ether solution, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material 1g, shines medical material solution in pairs with legal system.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With normal hexane-ethyl acetate (9: 1) is developing solvent, launches, and takes out; Dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.(2) get these article 20g, grind or chopping, add methanol 50ml, merceration spends the night; Put in the water-bath and refluxed 30 minutes, filter, the filtrating evaporate to dryness, residue adds water 20ml while hot makes dissolving; Put coldly, extract 2 times each 25ml, combined ether liquid with the ether jolting; Volatilize, residue adds methanol 0.5ml makes dissolving, as need testing solution.Other gets Radix Aucklandiae control medicinal material 0.2g, adds methanol 10ml, shines medical material solution in pairs with legal system.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw need testing solution 10 μ l, control medicinal material solution 2 μ l put respectively on same silica gel g thin-layer plate; With cyclohexane extraction-acetone (10: 3) is developing solvent, launches, and takes out; Dry, spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.(3) in the chromatogram that under the assay item, writes down, the test sample main peak is consistent with the retention time of monoammonium glycyrrhizinate reference substance main peak.
Wherein official method checks that to content step is:
[inspection] should meet each item regulation (an appendix I of Chinese Pharmacopoeia version in 2005 A) relevant under the pill item.
Wherein the effective ingredient monoammonium glycyrrhizinate that contains is carried out assay, step is:
[assay] measured according to HPLC (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filler, and methanol-water-acetic acid (69: 31: 0.5) is mobile phase; The detection wavelength is 254nm.Number of theoretical plate is pressed the monoammonium glycyrrhizinate peak and is calculated, and should be not less than 3500.
The preparation precision of reference substance solution takes by weighing through the monoammonium glycyrrhizinate reference substance of 80 ℃ of drying under reduced pressure to constant weights an amount of, adds 50% ethanol again and makes dissolving and process the solution that every 1ml contains monoammonium glycyrrhizinate 10 μ g, promptly gets.
These article porphyrize is got in the preparation of need testing solution, gets about 0.5g, and accurate the title decides, and puts in the 100ml round-bottomed flask, the accurate 50% ethanol 50ml that adds; Claim to decide weight, put in the water-bath reflux, extract, 2 hours, put coldly, weigh, supply the weight of loss with 50% ethanol; Shake up, filter, get subsequent filtrate, promptly get.
Algoscopy precision is respectively measured above-mentioned reference substance solution and is supplied each 20 μ l of examination solution, injects chromatograph of liquid, and the record chromatogram calculates, and promptly gets.
The every 1g of these article contains Radix Glycyrrhizae with monoammonium glycyrrhizinate (C
42H
63O
16N) meter must not be less than 1.17mg.
Following experimental data can prove excellent results of the present invention.
Granular preparation with embodiments of the invention 1 experimentizes; The pharmacodynamics result of study shows before clinical: return spleen granule big (7.78g/Kg), in (3.86g/Kg) dose groups can make the hemoglobin of model of blood dificiency mice reach 84.2,81.5 (g/l) respectively; Compare with 76.1 (g/l) of model of blood dificiency group; The difference that highly significant is arranged makes RBC number rise to 8.86 ± 0.86,8.44 ± 0.47 (10 from 6.43 ± 0.89,6.88 ± 0.59 respectively
12/ L), with the blood deficiency matched group relatively, P＜0.01 returns the big or middle dosage of spleen granule can reduce effectively all that mice is spontaneous walks about the time in the research of returning the spleen granule to the spontaneous activity in mice influence, the time of walking about in 2 minutes descends 50.1,44.4% respectively; Make the number of times lifted on the mice forelimb before the administration 18.56 ± 4.3,18.66 ± 2.8 reduce to 6.77 ± 3.11,11.0 ± 6.6 (inferior/2min), 17.55 ± 3.9 (inferior/as min) relatively, the difference of highly significant to be arranged with matched group; In the experiment of returning the spleen granule to the immune function of mice effect; Can obviously increase the content of specific antibody one hemolysin that is produced through the chicken red blood cell immune mouse; Compare with the inductive immunosuppressant group of cyclophosphamide, the content of hemolysin increases by 81.8,109.1% respectively.Return in the spleen granule, heavy dose can make the mice swimming time extend to 65.5 ± 26.6 and 85.4 ± 27.1 (branches), relatively there were significant differences with matched group; Can also obviously prolong the mice hypoxia endurance time.
More than research all compares there was no significant difference between group with the effect of GUIPI WAN.Prompting is adopted new technology such as spray drying to process at present and is returned the spleen granule, and five pharmacodynamic study results that carry out according to its main effect show, returns the spleen granule not only to keep the effect of GUIPI WAN but also to have a dose few; Advantages such as taking convenience.
Toxicologic study prompting before returning the spleen granule clinical: returning the spleen granule to give mouse stomach administration maximum tolerated dose on the one is 75 gram/kilograms, is equivalent to 416 times of clinical consumption, and experiment shows that the maximum tolerated dose of returning the spleen granule greater than GUIPI WAN, is safe drugs.
Return the spleen granule that rat long term toxicity test result is shown: to return the spleen granule to equal no difference of science of statistics of organ weights coefficient such as growth body weight, routine blood test, hepatic and renal function and the heart of each treated animal, liver, spleen, lung, kidney, thymus, adrenal gland; The pathology inspection of the above-mentioned organ of surviving animals does not also have specificity and changes.It is a safe drugs that the spleen granule is returned in prompting.
Results of stability
Stability test, three batches of these article are pressed existing packing at ambient temperature through 2 years reserved sample observings, and regularly pick test is investigated by each item index that quality standard is formulated, and each item index all ability is up to specification, and no significant difference is explained these article stability better.
Clinical verification:
Clinical observation through 100 routine syndrome of deficiency of both heart and spleen patients; Its obvious effective rate is 68%; Total effective rate is 98%; Show that these article can significantly improve syndrome of deficiency of both heart and spleen and cause various symptoms, especially to doing well,improvings more remarkable (P＜0.01) such as cardiopalmus, uncomfortable in chest, insomnia, forgetful, spiritlessness and sparing of words, fatigue and weakness, diarrhea with loose stool, abdominal distention after meal and loss of appetite.
The contrast in twos that treatment group, treatment group add single symptom treatment front and back integration differential between open bank and matched group shows: except that diarrhea with loose stool, abdominal distention after meal, all there were significant differences (P＜0.01, P＜0.05).Prompting returns the spleen granule that syndrome of deficiency of both heart and spleen is had obvious improvement effect, is superior to GUIPI WAN.
The safety observed result shows: all observe case and do not see that all obvious adverse reaction is arranged, the treatment group has no adverse effects to routine blood test, liver, kidney function test after returning the treatment of spleen granule, and can obvious haematochrome increasing and hematoblastic value.
Clinical results is thought: the spleen granule of returning of the present invention, and oral liquid and concentrated pill preparation for treating syndrome of deficiency of both heart and spleen determined curative effect have QI invigorating and blood producing, the effect of invigorating spleen and nourishing heart, safely, have no side effect, and taking convenience, the patient is easy to accept.
The spleen granule of returning of the present invention, oral liquid and concentrated pill preparation are to come through changing dosage form on the basis of existing technology, and granule of the present invention is guaranteeing under the constant condition of clinical usage and consumption; Adopted new preparation and detection method, overcome the defective of original preparation, be easy to carry and take; And disperse soon, good absorbing, bioavailability is high; Make preparation stabilization simultaneously, side effect reduces.
The specific embodiment
Below further specify the present invention through embodiment, but not as to claim of the present invention restriction.
Embodiment 1
The Radix Codonopsis 140g Rhizoma Atractylodis Macrocephalae (stir-fry) the 280g Radix Astragali (processed with honey) 140g Radix Glycyrrhizae (processed with honey) 70g
Poria 280g Radix Polygalae (system) 280g Semen Ziziphi Spinosae (stir-fry) 140g Arillus Longan 280g
Radix Angelicae Sinensis 280g Radix Aucklandiae 70g Fructus Jujubae (enucleation) 70g
Suitable granule is pulverized or be chopped into to [technology] above ten simply, and the little dynamic reflux, extract, secondary that boils of water adds 10 times of water gagings for the first time and extracted 1 hour; Add for the second time 5 times of water gagings and extracted 0.5 hour, merge medicinal liquid, filter; Filtrate decompression is concentrated into the extractum of relative density 1.05-1.15 (50 ℃), filters, and it is an amount of that filtrating adds dextrin; Mixing is processed granule 1000g, promptly gets.
Embodiment 2
Radix Codonopsis 70g Rhizoma Atractylodis Macrocephalae 140g Radix Astragali 70g Radix Glycyrrhizae 35g
Poria 140g Radix Polygalae 140g Semen Ziziphi Spinosae 70g Arillus Longan 140g
Radix Angelicae Sinensis 140g Radix Aucklandiae 35g Fructus Jujubae 35g
Its preparation method is following:
More than ten simply, pulverize or be chopped into suitable granule, the little dynamic reflux, extract, secondary that boils of water adds 10 times of water gagings for the first time and extracted 1 hour; Add for the second time 5 times of water gagings and extracted 0.5 hour, merge medicinal liquid, filter; Filtrate decompression is concentrated into the extractum of relative density 1.05-1.15 (50 ℃), filters, and it is an amount of that filtrating adds dextrin; Mixing is processed granule 1000g, promptly gets.
Embodiment 3
Radix Codonopsis 280g Rhizoma Atractylodis Macrocephalae 560g Radix Astragali 280g Radix Glycyrrhizae 140g
Poria 560g Radix Polygalae 560g Semen Ziziphi Spinosae 280g Arillus Longan 560g
Radix Angelicae Sinensis 560g Radix Aucklandiae 140g Fructus Jujubae 140g
Its preparation method is following:
More than ten simply, pulverize or be chopped into suitable granule, the little dynamic reflux, extract, secondary that boils of water adds 10 times of water gagings for the first time and extracted 1 hour; Add for the second time 5 times of water gagings and extracted 0.5 hour, merge medicinal liquid, filter; Filtrate decompression is concentrated into the extractum of relative density 1.05-1.15 (50 ℃), filters, and it is an amount of that filtrating adds dextrin; Mixing is processed granule 1000g, promptly gets.
Embodiment 4
The Radix Codonopsis 140g Rhizoma Atractylodis Macrocephalae (stir-fry) the 280g Radix Astragali (processed with honey) 140g Radix Glycyrrhizae (processed with honey) 70g
Poria 280g Radix Polygalae (system) 280g Semen Ziziphi Spinosae (stir-fry) 140g Arillus Longan 280g
Radix Angelicae Sinensis 280g Radix Aucklandiae 70g Fructus Jujubae (enucleation) 70g
Its preparation method is following:
More than ten simply, pulverize or be chopped into suitable granule, the little dynamic reflux, extract, secondary that boils of water adds 10 times of water gagings for the first time and extracted 1 hour; Add for the second time 5 times of water gagings and extracted 0.5 hour, merge medicinal liquid, filter, filtrate decompression is concentrated into the extractum of relative density 1.05-1.15 (50 ℃); Filter, adding sucrose is an amount of in the filtrating, and benzoic acid is an amount of, dissolving; Adding distil water filters to 1015ml or 2030ml, embedding, and sterilization promptly gets oral liquid.
Embodiment 5
The Radix Codonopsis 140g Rhizoma Atractylodis Macrocephalae (stir-fry) the 280g Radix Astragali (processed with honey) 140g Radix Glycyrrhizae (processed with honey) 70g
Poria 280g Radix Polygalae (system) 280g Semen Ziziphi Spinosae (stir-fry) 140g Arillus Longan 280g
Radix Angelicae Sinensis 280g Radix Aucklandiae 70g Fructus Jujubae (enucleation) 70g
Its preparation method is following:
More than ten simply, pulverize or be chopped into suitable granule, the little dynamic reflux, extract, secondary that boils of water adds 10 times of water gagings for the first time and extracted 1 hour; Add for the second time 5 times of water gagings and extracted 0.5 hour, merge medicinal liquid, filter; Filtrate decompression is concentrated into the extractum of relative density 1.05-1.15 (50 ℃), filters, and filtrating adds an amount of water, Mel, dextrin; Mixing, the general 1000g ball of processing is drying to obtain.
Claims (1)
1. return the particulate detection method of spleen, step is following:
Character is observed, content is differentiated, official method is checked content, and the effective ingredient monoammonium glycyrrhizinate that contains is carried out assay;
The said spleen granule of returning makes as follows:
Process by following parts by weight of Chinese traditional medicine raw material:
Radix Codonopsis 70-280g, Rhizoma Atractylodis Macrocephalae 140-560g, Radix Astragali 70-280g, Radix Glycyrrhizae 35-140g, Poria 140-560g, Radix Polygalae 140-560g, Semen Ziziphi Spinosae 70-280g, Arillus Longan 140-560g, Radix Angelicae Sinensis 140-560g, Radix Aucklandiae 35-140g, Fructus Jujubae 35-140g;
Its preparation method is following:
More than ten simply, pulverize or be chopped into suitable granule, the little dynamic reflux, extract, secondary that boils of water; Add for the first time 5-12 times of water gaging and extracted 1-2 hour, add 5-12 times of water gaging for the second time and extracted 0.5-1.5 hour, merge medicinal liquid; Filter; Relative density was the extractum of 1.05-1.15 when filtrate decompression was concentrated into 50 ℃, filtered, and filtrating adds adjuvant and is prepared into granule;
Wherein character is observed, and step is:
Character: these article are brown or tan granule; Gas is fragrant, sweet in the mouth, little hardship;
Wherein content is differentiated, step is:
These article 10g is got in discriminating (1), adds methanol 30ml, and merceration spends the night, and supersound process 15 minutes filters, and residue adds methanol 10ml; Washing filters, and merging filtrate, evaporate to dryness, residue add water 15ml while hot makes dissolving; Put coldly, extract 2 times with the ether jolting, each 15ml merges ether solution, volatilizes; Residue adds methanol 1ml makes dissolving, and as need testing solution, other gets Radix Angelicae Sinensis control medicinal material 1g, shines medical material solution in pairs with legal system, according to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography; Drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with normal hexane-ethyl acetate=9: 1, launches taking-up; Dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(2) get these article 20g, add methanol 50ml, merceration spends the night, and puts in the water-bath and refluxes 30 minutes, filters; The filtrating evaporate to dryness, residue adds water 20ml while hot makes dissolving, puts coldly, extracts 2 times with the ether jolting, at every turn 25ml; Combined ether liquid volatilizes, and residue adds methanol 0.5ml makes dissolving, and as need testing solution, other gets Radix Aucklandiae control medicinal material 0.2g; Add methanol 10ml, shine medical material solution in pairs,, draw need testing solution 10 μ l, control medicinal material solution 2 μ l according to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography with legal system; Putting respectively on same silica gel g thin-layer plate, is developing solvent with cyclohexane extraction-acetone=10: 3, launches, and takes out, and dries; Spray is with 5% vanillin sulfuric acid solution, and hot blast blows to clear spot, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(3) in the chromatogram that under the assay item, writes down, the test sample main peak is consistent with the retention time of monoammonium glycyrrhizinate reference substance main peak,
Wherein official method checks that to content step is:
Inspection: according to appendix XIB of Chinese Pharmacopoeia version in 2005, granularity can not and can must not cross 15.0% through the granule and the powder summation of No. five sieves through a sieve,
Moisture is measured according to an appendix IX of Chinese Pharmacopoeia version in 2005 H three therapeutic methods of traditional Chinese medicine aquametry, must not cross 6.0%, and other should meet each item regulation relevant under an appendix I of Chinese Pharmacopoeia version in 2005 the C granule item,
Wherein the effective ingredient monoammonium glycyrrhizinate that contains is carried out assay, step is:
Assay: according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring,
The test of chromatographic condition and system suitability uses octadecylsilane chemically bonded silica to be filler, and methanol-water-acetic acid=69: 31: 0.5 is mobile phase; The detection wavelength is 254nm, and number of theoretical plate is pressed the monoammonium glycyrrhizinate peak and calculated, and should be not less than 3500;
The preparation precision of reference substance solution takes by weighing through the monoammonium glycyrrhizinate reference substance of 80 ℃ of drying under reduced pressure to constant weights an amount of, adds 50% ethanol again and makes dissolving and process the solution that every 1ml contains monoammonium glycyrrhizinate 10 μ g, promptly get,
These article porphyrize is got in the preparation of need testing solution, gets 0.5g, and accurate the title decides, and puts in the 100ml round-bottomed flask, the accurate 50% ethanol 50ml that adds; Claim to decide weight, put in the water-bath reflux, extract, 2 hours, put coldly, weigh, supply the weight of loss with 50% ethanol; Shake up, filter, get subsequent filtrate, promptly get;
Algoscopy precision is respectively measured above-mentioned reference substance solution and each 20 μ l of need testing solution, injects chromatograph of liquid, and the record chromatogram calculates, and promptly gets;
The every 1g of these article contains Radix Glycyrrhizae in monoammonium glycyrrhizinate, must not be less than 1.17mg.
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| CN2010101125222A CN101732466B (en) | 2007-08-13 | 2007-08-13 | Method for controlling quality of Guipi granules |
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| CN2010101125222A CN101732466B (en) | 2007-08-13 | 2007-08-13 | Method for controlling quality of Guipi granules |
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| CN2007101439073A Division CN101095745B (en) | 2007-08-13 | 2007-08-13 | Particles for invigorating the spleen and preparation method |
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| CN102841160B (en) * | 2012-09-27 | 2014-11-05 | 南京中医药大学 | Quality control method of Sijunzi (Chinese name) decoction |
| CN107281305A (en) * | 2017-06-19 | 2017-10-24 | 浙江爱生药业有限公司 | Application of the returns spleen preparation in alcohol dehydrogenase and aldehyde dehydrogenase activity is improved |
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Non-Patent Citations (1)
| Title |
|---|
| 国家药典委员会.归脾丸.《中华人民共和国药典 2005年版 一部》.2005,第41-43、59-60、89、419、附录ⅠC和附录ⅪB. * |
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