CN103977097A - Yiqing granule preparing method - Google Patents
Yiqing granule preparing method Download PDFInfo
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- CN103977097A CN103977097A CN201410254977.6A CN201410254977A CN103977097A CN 103977097 A CN103977097 A CN 103977097A CN 201410254977 A CN201410254977 A CN 201410254977A CN 103977097 A CN103977097 A CN 103977097A
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Abstract
The invention discloses a Yiqing granule preparing method. The method comprises the following steps: respectively extracting dry extract powder from rhizoma coptidis, rheum officinale and radix scutellaria; adding a pharmaceutically-acceptable auxiliary material in the dry extract powder of rhizoma coptidis, evenly mixing, and adding an ethanol-water solution or water so as to prepare rhizoma coptidis granules; adding a pharmaceutically-acceptable auxiliary material in the dry extract powder of rheum officinale, evenly mixing, and adding a sodium hydroxide water solution or an ethanol-water solution containing sodium hydroxide so as to prepare rheum officinale granules; adding a pharmaceutically-acceptable auxiliary material in the dry extract powder of radix scutellariae, evenly mixing, and adding a sodium hydroxide water solution or an ethanol-water solution containing sodium hydroxide so as to prepare radix scutellaria granules; finally mixing rhizoma coptidis granules, rheum officinale granules and radix scutellaria granules to obtain mixed granules, and sub-packaging the mixed granules in bags, thereby obtaining Yiqing granules. The Yiqing granules prepared by virtue of the method have qualified dissolubility and a strong curative effect and are safe and effective to take; besides, the technology is simple; the application prospect is broad.
Description
Technical field
The present invention relates to a kind of preparation method of medicine, particularly a kind of preparation method of YIQING KELI.
Background technology
YIQING KELI is a kind of Chinese medicine granules medicine that < < Chinese Pharmacopoeia > > version in 2010 is recorded, and has clearing away heat-fire removing toxic substances, the function of blood stasis dispelling cooling blood for hemostasis.Be widely used in clinically fever of the body agitation, conjunctival congestion aphtha, throat gingival swelling and pain, constipation, haematemesis, spitting of blood, hemorrhoidal bleeding and pharyngitis due to fire-toxin heat in blood, tonsillitis, gingivitis is shown in above-mentioned symptom person.Along with the raising of people's living standard, being afraid of to get angry, will reduce internal heat is the problem that a lot of people often run into, so the routine use amount of YIQING KELI is very large.
But, YIQING KELI is national essential drugs, according to the principle of essential drugs sampling observation all standing, national drug supervisory and management department puts more effort to making a random inspection of YIQING KELI in recent years, also just exposed the problem of YIQING KELI: repeatedly selective examination is defective to YIQING KELI melting, allow the general common people dare not relieved use YIQING KELI, Ye Rang pharmaceutical production producer be very puzzled.The defective decline that also can cause its curative effect of medication of YIQING KELI melting.
The underproof reason of YIQING KELI melting is mainly following two aspects: (1) YIQING KELI adds adjuvant to make by Rhizoma Coptidis, Radix Et Rhizoma Rhei, Radix Scutellariae three taste Chinese medicines after getting indescribably, and the effective constituent berberine hydrochloride that mainly contains of Rhizoma Coptidis is water-fast, the effective constituent emodin that mainly contains of Radix Et Rhizoma Rhei is that almost water-fast, chrysophanic acid is water-fast, the effective constituent baicalin that mainly contains of Radix Scutellariae is also almost water-fast, and the granule melting of being made by them self can have problems.(2) the effective constituent berberine hydrochloride that mainly contains of Rhizoma Coptidis is strong basicity, Radix Et Rhizoma Rhei mainly contain effective constituent emodin, chrysophanic acid is faintly acid composition.If allowed in drug production process between them, simply mix, brew taking Shi Jiashui, between them, will react and generate the macromolecular salt that is insoluble in water, thereby further affect the melting of granule.
The preparation method of < < Chinese Pharmacopoeia > > version YIQING KELI in 2010 is (Rhizoma Coptidis, Radix Et Rhizoma Rhei, Radix Scutellariae) " above three tastes; decoct with water respectively secondary; 1.5 hours for the first time; 1 hour for the second time; collecting decoction; filter, filtrate decompression is concentrated into the clear paste that relative density is about 1.25 (70 ℃), is spray dried to dry extract; Above-mentioned three kinds of extract powders are merged, add dextrin 729.6g and sodium cyclamate 15.04g, mix, granulation, dry, make 1000g, obtain." although this preparation method considers that in the extraction stage several medical material mixed extraction can generate precipitation and active ingredient is lost; when preparing granule, but ignore the macromolecular salt that is insoluble in water of generation that can react after it mixes, and then affected the problem of granule melting.
Summary of the invention
The object of the invention is to overcome existing above-mentioned deficiency in prior art, a kind of preparation method of YIQING KELI is provided.Preparation method of the present invention is that the dry extract that Rhizoma Coptidis, Radix Et Rhizoma Rhei, three kinds of medicinal material extract of Radix Scutellariae are obtained is granulated respectively, adds respectively sodium hydroxide in the process of preparing Radix Et Rhizoma Rhei granule and Radix Scutellariae granule simultaneously, finally again three kinds of granules is mixed, is distributed into bag.The YIQING KELI melting being made by this preparation method is qualified, safe and effective for medication, and curative effect effect is strong.
In order to realize foregoing invention object, the invention provides following technical scheme:
A preparation method for YIQING KELI, comprises the steps:
(1) get Rhizoma Coptidis, Radix Et Rhizoma Rhei, Radix Scutellariae, decocts with water respectively, and collecting decoction filters, and filtrate decompression is concentrated into clear paste, and spraying is dry, obtains respectively Rhizoma Coptidis dry extract, Radix Et Rhizoma Rhei dry extract and Radix Scutellariae dry extract;
(2) get the Rhizoma Coptidis dry extract that step (1) makes, add pharmaceutically acceptable adjuvant, mix, add ethanol water or water, granulation, dry, obtain Rhizoma Coptidis granule;
(3) get the Radix Et Rhizoma Rhei dry extract that step (1) makes, add pharmaceutically acceptable adjuvant, mix, add sodium hydrate aqueous solution or containing the ethanol water of sodium hydroxide, granulation, dry, obtain Radix Et Rhizoma Rhei granule;
(4) get the Radix Scutellariae dry extract that step (1) makes, add pharmaceutically acceptable adjuvant, mix, add sodium hydrate aqueous solution or containing the ethanol water of sodium hydroxide, granulation, dry, obtain Radix Scutellariae granule;
(5) Rhizoma Coptidis granule step (2)～(4) being made respectively, Radix Et Rhizoma Rhei granule are mixed homogeneously with Radix Scutellariae granule, are distributed into bag, obtain YIQING KELI.
The dry extract that above-mentioned preparation method obtains Rhizoma Coptidis, Radix Et Rhizoma Rhei, three kinds of medicinal material extract of Radix Scutellariae is granulated respectively, and according to the character that mainly contains effective constituent in three kinds of dry extracts, take measure targetedly when granulating, effectively solve the underproof problem of YIQING KELI melting, thereby guarantee the performance of its curative effect, safe and effective for medication.First, the dry extract that Rhizoma Coptidis, Radix Et Rhizoma Rhei, three kinds of medicinal material extract of Radix Scutellariae are obtained is granulated respectively, has avoided three kinds of dry extracts just to react in pelletization and has generated the macromolecular salt that is insoluble in water, thereby affected the melting of YIQING KELI.Secondly, according to Radix Et Rhizoma Rhei to mainly contain effective constituent emodin water-soluble hardly, chrysophanic acid is water insoluble, Radix Scutellariae to mainly contain effective constituent baicalin water-soluble hardly, but be but all dissolved in sodium hydrate aqueous solution, when preparing Radix Et Rhizoma Rhei granule and Radix Scutellariae granule, all added respectively sodium hydroxide, this several meltages that mainly contain effective constituent itself have been increased on the one hand, on the other hand in clothes for patients YIQING KELI, when water brews, if also have free berberine hydrochloride, emodin, chrysophanic acid, baicalin, first they are to contact with micromolecular sodium hydroxide, thereby avoided several macromolecular active ingredients directly to contact and generated the macromolecular problem that is insoluble in the salt of water.
Preferably, in described step (1), the weight portion proportioning of Rhizoma Coptidis, Radix Et Rhizoma Rhei and Radix Scutellariae is Rhizoma Coptidis 150-400 part, Radix Et Rhizoma Rhei 600-900 part, Radix Scutellariae 200-600 part.
Preferably, on described step (2)～(4) Chinese materia medica, acceptable adjuvant is selected from any one or a few in dextrin, cane sugar powder, soluble starch, lactose and sodium cyclamate.Further preferably, on described step (2)～(4) Chinese materia medica, acceptable adjuvant is dextrin and sodium cyclamate, because dextrin is macromolecular substances with respect to sucrose, lactose, digests slowlyer, and diabetes patient also can take; In addition, several compositions in YIQING KELI are all the materials that taste is extremely bitter, and sodium cyclamate has good sugariness, is good sweeting agent, can greatly improve the mouthfeel of the YIQING KELI medicine of making.
Preferably, in described step (2), in adjuvant and step (1), the weight ratio of Rhizoma Coptidis is 1-3:3-8.
In above-mentioned preparation method, described step adds appropriate water or ethanol water in (2), can make relative medicine have certain cohesive, is convenient to granulation.Preferably, in described step (2), ethanol water or the volume of water and the weight ratio of adjuvant are 1～3ml:5-15g.In the preferred described step of the present invention (2), add ethanol water; Ethanol more easily volatilizees, thereby makes the more open porous of granule that makes, and in the use procedure of medicine, melting is better.Further preferably, in described step (2) ethanol water, the percentage by volume of ethanol is 5～70%.When ethanol content can cause the granule of making to harden lower than 5%; When ethanol content is higher than 70% time, can cause the excessively loose and not molding of the granule made, granularity is too poor, does not meet drug standard requirement.In described step (2) ethanol water, percentage by volume the best of ethanol is preferably 40%.
Preferably, in described step (3), in adjuvant and step (1), the weight ratio of Radix Et Rhizoma Rhei is 2-5:6-9.
Preferably, in described step (4), in adjuvant and step (1), the weight ratio of Radix Scutellariae is 2-5:2-6.
In above-mentioned preparation method, in described step (3) and (4), add appropriate sodium hydrate aqueous solution or containing the ethanol water of sodium hydroxide, make relative medicine have certain cohesive on the one hand, be convenient to granulation, on the other hand Radix Et Rhizoma Rhei to mainly contain effective constituent emodin water-soluble hardly, chrysophanic acid is water insoluble, Radix Scutellariae to mainly contain effective constituent baicalin water-soluble hardly, but be but all dissolved in sodium hydrate aqueous solution, when preparing Radix Et Rhizoma Rhei granule and Radix Scutellariae granule, all add respectively sodium hydroxide, this several meltages that mainly contain effective constituent itself have not only been increased, simultaneously when clothes for patients brews with YIQING KELI water, if also have free berberine hydrochloride, emodin, chrysophanic acid, baicalin, first they are to contact with micromolecular sodium hydroxide, thereby avoided several macromolecular active ingredients directly to contact and generated the macromolecular problem that is insoluble in the salt of water.The present invention preferably adds the ethanol water containing sodium hydroxide; Ethanol more easily volatilizees, thereby makes the more open porous of granule that makes, and in the use procedure of medicine, melting can be better.
Preferably, sodium hydrate aqueous solution or be 2-6ml:10-25g containing the volume of ethanol water and the weight ratio of adjuvant of sodium hydroxide in described step (3), sodium hydrate aqueous solution or be 0.5～3% containing the mass percent of sodium hydroxide in the ethanol water of sodium hydroxide wherein, the best is 1.5%; Percentage by volume containing ethanol in the ethanol water of sodium hydroxide is 5～70%, and the best is 40%.
Preferably, sodium hydrate aqueous solution or be 4-15ml:20-50g containing the volume of ethanol water and the weight ratio of adjuvant of sodium hydroxide in described step (4), sodium hydrate aqueous solution or be 0.5～3% containing the mass percent of sodium hydroxide in the ethanol water of sodium hydroxide wherein, the best is 1.5%; Percentage by volume containing ethanol in the ethanol water of sodium hydroxide is 5～70%, and the best is 40%.
Applicant finds through test of many times, when in step (3) and step (4), the mass percent of sodium hydroxide is less than 0.5%, do not have and increase deliquescent effect, and can cause alkalescence excessively strong while being greater than 3%, affect the acid-base balance of mouthfeel and user's gastric juice, and then affect the curative effect of medicine.
By preferably above, not only make YIQING KELI melting better, curative effect effect is stronger, and grain graininess is good simultaneously, does not harden, and mouthfeel is suitable.
Compared with prior art, the invention has the beneficial effects as follows:
(1) the present invention extracts three kinds of Chinese crude drugs of preparation YIQING KELI respectively and obtains dry extract, add again suitable adjuvant granulation respectively, finally mix, bag distribution packaging, avoid three kinds of dry extracts just to react in pelletization and generated the macromolecular salt that is insoluble in water, thereby affected the problem of YIQING KELI melting.
(2) the present invention is directed to the character of three kinds of Chinese crude drugs, in the preparation process of Radix Et Rhizoma Rhei granule and Radix Scutellariae granule, add sodium hydroxide respectively, solved Radix Et Rhizoma Rhei to mainly contain effective constituent emodin water-soluble hardly, chrysophanic acid is water insoluble, the almost water-fast problem of effective constituent baicalin that mainly contains of Radix Scutellariae, also people have been solved when taking YIQING KELI water and brewing, several active ingredients react mutually and generate the macromolecular problem that is insoluble in the salt of water, make the YIQING KELI melting of preparation qualified, the YIQING KELI that drug effect adopts traditional method to prepare increases significantly, safe and effective for medication.
(3) preparation method of the present invention is simple, easily grasps, and production equipment is also identical with the production equipment of conventional YIQING KELI, is convenient to promote, and is applicable to industrialized great production.
The specific embodiment
Below in conjunction with test example and the specific embodiment, the present invention is described in further detail.But this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment, all technology realizing based on content of the present invention all belong to scope of the present invention.
Embodiment 1
(1) get Rhizoma Coptidis 264g, Radix Et Rhizoma Rhei 800g, Radix Scutellariae 400g, decocts with water respectively 3 times, for the first time 1.5h, each 1h of second and third time, collecting decoction, filters, the clear paste that when filtrate decompression is concentrated into 70 ℃ of surveys, relative density is 1.15, spraying is dry, obtains respectively Rhizoma Coptidis dry extract, Radix Et Rhizoma Rhei dry extract and Radix Scutellariae dry extract;
(2) get the Rhizoma Coptidis dry extract that step (1) makes, add dextrin 100g, sodium cyclamate 3g, mix, add 40% ethanol water 20ml, granulation, dry, obtain Rhizoma Coptidis granule;
(3) get the Radix Et Rhizoma Rhei dry extract that step (1) makes, add dextrin 300g, sodium cyclamate 6g, mix, (mass percent containing sodium hydroxide in the ethanol water of sodium hydroxide is 1.5% to add 50ml to contain the ethanol water of sodium hydroxide, the percentage by volume of ethanol is 40%), granulation, dry, obtain Radix Et Rhizoma Rhei granule;
(4) get the Radix Scutellariae dry extract that step (1) makes, add dextrin 330g, sodium cyclamate 6g, mix, (mass percent containing sodium hydroxide in the ethanol water of sodium hydroxide is 1.5% to add 55ml to contain the ethanol water of sodium hydroxide, the percentage by volume of ethanol is 40%), granulation, dry, obtain Radix Scutellariae granule;
(5) Rhizoma Coptidis granule step (2)～(4) being made respectively, Radix Et Rhizoma Rhei granule are mixed homogeneously with Radix Scutellariae granule, are distributed into every bag of 5g, obtain YIQING KELI.
Embodiment 2
(1) get Rhizoma Coptidis 320g, Radix Et Rhizoma Rhei 700g, Radix Scutellariae 450g, decocts with water respectively 3 times, for the first time 1.5h, each 1h of second and third time, collecting decoction, filters, the clear paste that when filtrate decompression is concentrated into 70 ℃ of surveys, relative density is 1.10, spraying is dry, obtains respectively Rhizoma Coptidis dry extract, Radix Et Rhizoma Rhei dry extract and Radix Scutellariae dry extract;
(2) get the Rhizoma Coptidis dry extract that step (1) makes, add lactose 100g, sodium cyclamate 5g, mix, add 20% ethanol water 15ml, granulation, dry, obtain Rhizoma Coptidis granule;
(3) get the Radix Et Rhizoma Rhei dry extract that step (1) makes, add lactose 300g, sodium cyclamate 5g, mix, (mass percent containing sodium hydroxide in the ethanol water of sodium hydroxide is 1.5% to add 45ml to contain the ethanol water of sodium hydroxide, the percentage by volume of ethanol is 20%), granulation, dry, obtain Radix Et Rhizoma Rhei granule;
(4) get the Radix Scutellariae dry extract that step (1) makes, add lactose 330g, sodium cyclamate 5g, mix, (mass percent containing sodium hydroxide in the ethanol water of sodium hydroxide is 1.5% to add 50ml to contain the ethanol water of sodium hydroxide, the percentage by volume of ethanol is 20%), granulation, dry, obtain Radix Scutellariae granule;
(5) with embodiment 1.
Embodiment 3
(1) get Rhizoma Coptidis 150g, Radix Et Rhizoma Rhei 600g, Radix Scutellariae 200g, decocts with water respectively 3 times, for the first time 1.5h, each 1h of second and third time, collecting decoction, filters, the clear paste that when filtrate decompression is concentrated into 70 ℃ of surveys, relative density is 1.08, spraying is dry, obtains respectively Rhizoma Coptidis dry extract, Radix Et Rhizoma Rhei dry extract and Radix Scutellariae dry extract;
(2) get the Rhizoma Coptidis dry extract that step (1) makes, add soluble starch 47g, sodium cyclamate 3g, mix, add 50% ethanol water 10ml, granulation, dry, obtain Rhizoma Coptidis granule;
(3) get the Radix Et Rhizoma Rhei dry extract that step (1) makes, add soluble starch 196g, sodium cyclamate 4g, mix, (mass percent containing sodium hydroxide in the ethanol water of sodium hydroxide is 0.5% to add 40ml to contain the ethanol water of sodium hydroxide, the percentage by volume of ethanol is 40%), granulation, dry, obtain Radix Et Rhizoma Rhei granule;
(4) get the Radix Scutellariae dry extract that step (1) makes, add soluble starch 197g, sodium cyclamate 3g, mix, (mass percent containing sodium hydroxide in the ethanol water of sodium hydroxide is 0.5% to add 40ml to contain the ethanol water of sodium hydroxide, the percentage by volume of ethanol is 40%), granulation, dry, obtain Radix Scutellariae granule;
(5) with embodiment 1.
Embodiment 4
(1) get Rhizoma Coptidis 400g, Radix Et Rhizoma Rhei 900g, Radix Scutellariae 600g, decocts with water respectively 3 times, for the first time 1.5h, each 1h of second and third time, collecting decoction, filters, the clear paste that when filtrate decompression is concentrated into 70 ℃ of surveys, relative density is 1.05, spraying is dry, obtains respectively Rhizoma Coptidis dry extract, Radix Et Rhizoma Rhei dry extract and Radix Scutellariae dry extract;
(2) get the Rhizoma Coptidis dry extract that step (1) makes, add cane sugar powder 140g, sodium cyclamate 10g, mix, add 25% ethanol water 30ml, granulation, dry, obtain Rhizoma Coptidis granule;
(3) get the Radix Et Rhizoma Rhei dry extract that step (1) makes, add cane sugar powder 484g, sodium cyclamate 16g, mix, (mass percent containing sodium hydroxide in the ethanol water of sodium hydroxide is 2.5% to add 90ml to contain the ethanol water of sodium hydroxide, the percentage by volume of ethanol is 50%), granulation, dry, obtain Radix Et Rhizoma Rhei granule;
(4) get the Radix Scutellariae dry extract that step (1) makes, add cane sugar powder 451g, sodium cyclamate 9g, mix, (mass percent containing sodium hydroxide in the ethanol water of sodium hydroxide is 2.5% to add 90ml to contain the ethanol water of sodium hydroxide, the percentage by volume of ethanol is 50%), granulation, dry, obtain Radix Scutellariae granule;
(5) with embodiment 1.
Embodiment 5
(1) with embodiment 1;
(2) get the Rhizoma Coptidis dry extract that step (1) makes, add dextrin 100g, sodium cyclamate 3g, mix, add 20ml water, granulation, dry, obtain Rhizoma Coptidis granule;
(3) get the Radix Et Rhizoma Rhei dry extract that step (1) makes, add dextrin 300g, sodium cyclamate 6g, mix, add 50ml sodium hydrate aqueous solution (in sodium hydrate aqueous solution, the mass percent of sodium hydroxide is 1.5%), granulation, dry, obtain Radix Et Rhizoma Rhei granule;
(4) get the Radix Scutellariae dry extract that step (1) makes, add dextrin 330g, sodium cyclamate 6g, mix, add 55ml sodium hydrate aqueous solution (in sodium hydrate aqueous solution, the mass percent of sodium hydroxide is 1.5%), granulation, dry, obtain Radix Scutellariae granule;
(5) Rhizoma Coptidis granule step (2)～(4) being made respectively, Radix Et Rhizoma Rhei granule are mixed homogeneously with Radix Scutellariae granule, are distributed into every bag of 5g, obtain YIQING KELI.
Test example 1
The YIQING KELI of embodiment 1 preparation is checked according to the quality standard of < < Chinese Pharmacopoeia > > version YIQING KELI in 2010, and result is as follows:
(1) its character is filemot granule; Taste is micro-sweet, bitter.
(2) differentiate
1. get this product 4g, add methanol 25ml, dipping 2h, jolting, filters filtrate evaporate to dryness, residue adds water 10ml to be made to dissolve, then adds hydrochloric acid 1ml, puts and in water-bath, heats 30min, cooling immediately, with chloroform jolting, extract 2 times, each 10ml, merges chloroform extraction liquid, be concentrated into about 1ml, as need testing solution.Separately get Radix Et Rhizoma Rhei control medicinal material 0.1g, be made in the same way of control medicinal material solution.Get again emodin reference substance, add chloroform and make every 1ml containing the solution of 0.5mg, in contrast product solution.According to thin layer chromatography, test, draw each 5 μ l of above-mentioned three kinds of solution, put respectively in same and take on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is adhesive, the upper solution of petroleum ether (60 ℃～90 ℃)-Ethyl formate-formic acid (15: 5: 1) of take is developing solvent, launch, take out, dry, put under ultra-violet lamp (365nm) and inspect.In test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, the fluorescence speckle of aobvious same color; Put in ammonia steam smoked after, under daylight, inspect, speckle becomes redness.
2. get this product 4g, add methanol 25ml, add 1～2 of hydrochloric acid, supersound process 20min, filters, and filtrate is put evaporate to dryness in water-bath, and residue adds methanol 2ml to be made to dissolve, as need testing solution.Separately get Radix Scutellariae control medicinal material 0.5g, be made in the same way of control medicinal material solution.Get again baicalin reference substance, add methanol and make every 1ml containing the solution of 1mg, in contrast product solution.According to thin layer chromatography (appendix VI B of Chinese Pharmacopoeia version in 2005), test, draw each 5 μ l of above-mentioned three kinds of solution, on the silica gel g thin-layer plate that to put respectively in same carboxymethylcellulose sodium solution of take containing 4% sodium acetate be adhesive, take ethyl acetate-butanone-formic acid-water (5: 3: 1: 1) be developing solvent, launch, take out, dry, spray is with 2% ferric chloride alcoholic solution.In test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, the speckle of aobvious same color.
3. get this product 4g, add methanol 25ml, dipping 2h, jolting, filters, and filtrate is put evaporate to dryness in water-bath, and residue adds methanol 2ml to be made to dissolve, as need testing solution.Separately get Rhizoma Coptidis control medicinal material 50mg, add methanol 5ml, reflux 15min, filters, and filtrate adds methanol makes into 5ml, in contrast medical material solution.Get again berberine hydrochloride reference substance, add methanol and make every 1ml containing the solution of 0.5mg, in contrast product solution.According to thin layer chromatography (appendix VI B of Chinese Pharmacopoeia version in 2005), test, draw each 1～2 μ l of above-mentioned three kinds of solution, put respectively in same and take on the silica gel g thin-layer plate that carboxymethylcellulose sodium solution is adhesive, benzene-ethyl acetate-methanol-the isopropanol-water (6: 3: 1.5: 1.5: 0.3) of take is developing solvent, put in the pre-saturated expansion cylinder of ammonia steam, launch, take out, dry, put under ultra-violet lamp (365nm) and inspect.In test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, aobvious identical yellow fluorescence speckle.
(3) assay
According to high performance liquid chromatography (appendix VI D of Chinese Pharmacopoeia version in 2005), measure.
Chromatographic condition and system suitability be take octadecylsilane chemically bonded silica as filler; Methanol-0.2mol/L the sodium dihydrogen phosphate (with phosphorus acid for adjusting pH value to 2.7) (42: 58) of take is mobile phase; Detection wavelength is 275nm; Theoretical cam curve is calculated and should be not less than 5000 by baicalin peak.
Baicalin reference substance 12.5mg is got in the preparation of reference substance solution, accurately weighed, puts in 250ml measuring bottle, adds methanol 10ml and makes to dissolve, and is diluted with water to scale, shakes up, and obtains (in every 1ml, containing baicalin 50 μ g).
This product under content uniformity item is got in the preparation of need testing solution, and porphyrize is got about 0.75g, accurately weighed, put in 100ml measuring bottle, add methanol 10ml, supersound process (power 250W, frequency 50kHz) 10min, lets cool, be diluted with water to scale, shake up, centrifugal, get supernatant, with 0.45 μ m microporous filter membrane, filter, get subsequent filtrate, obtain.
Algoscopy is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
Every bag of this product containing Radix Scutellariae with baicalin (C
12h
18o
11) meter, must not be less than 21mg.
The present invention has equality altogether and has measured 3 times, and measurement result is 30.79mg, 30.61mg, 30.87mg.
The equal conformance with standard regulation of above testing result.
Test example 2
The melting of YIQING KELI prepared by the present invention and drug effect advantage thereof are by experimental results show that below:
Experiment one: melting
According to the method for < < Chinese Pharmacopoeia > > version melting inspection in 2010, the melting of the YIQING KELI of embodiment 1～5 preparation is detected.
Particular exam method is:
(1) get filter paper, doubling is placed in weighing botle, and lid is not placed in weighing botle drying baker together with lid, in 105 ℃, be dried 30 minutes, from drying baker, take out weighing botle and the lid of weighing botle is covered tightly, being placed in the exsiccator that discolour silica gel is housed, being cooled to room temperature, open the lid of weighing botle, take out filter paper, the weight of the weighed dry filter paper of analytical balance that is 0.0001g with minimum calibration, its weight is designated as M
1;
(2) get for examination granule 10g, put in 250ml beaker, add temperature and be the distilled water 200ml of 70 ℃～80 ℃, stir 5 minutes, then dried filter paper is converted into funnel-form, be placed in funnel, liquid after stirring is above passed through to Glass rod drain, pour on the filter paper in funnel, allow liquid filter from filter paper, with the distilled water 20ml that temperature is 70 ℃～80 ℃, wash beaker 2 times again, make the whole wash cleans of material in beaker, washing liquid is passed through to Glass rod drain, pour on the filter paper in funnel, allow washing liquid filter from filter paper, with the distilled water 50ml that temperature is 70 ℃～80 ℃, divide and from the nearly upper edge of filter paper, along surrounding, wash filter paper 3 times comprehensively again, allow washing liquid also from filter paper, filter, after the liquid filter to the greatest extent on filter paper, from funnel, take out filter paper, precipitate on filter paper is wrapped in filter paper, then the filter paper wrapping is placed in to the weighing botle of diameter 8cm, do not cover the lid of weighing botle, by being equipped with together with the weighing botle of the filter paper wrapping and the lid of weighing botle, be placed in drying baker, in 105 ℃, be dried 60 minutes, take out weighing botle and the lid of weighing botle is covered tightly, make the filter paper sealing wrapping after being dried, be placed in together the exsiccator that discolour silica gel is housed, be cooled to room temperature, then open the lid of weighing botle, take out the filter paper wrapping after being dried, the analytical balance that is 0.0001g with minimum calibration is weighed, its weight is designated as M
2,
(3) with filter paper and sedimentary gross weight M after filter
2deduct the filter paper weight M before filter
1, drawing the weight M that stays the material on filter paper, the size of M reflects the situation of granule melting.M value is less, shows that granule melting is better.
Following matched group is set simultaneously:
Comparative example 1:
(1)～(2): with embodiment 1;
(3) get the Radix Et Rhizoma Rhei dry extract that step (1) makes, add cane sugar powder 484g, sodium cyclamate 16g, mix, add 40% ethanol water 50ml, granulation, dry, obtain Radix Et Rhizoma Rhei granule;
(4) get the Radix Scutellariae dry extract that step (1) makes, add cane sugar powder 451g, sodium cyclamate 9g, mix, add 40% ethanol water 55ml, granulation, dry, obtain Radix Scutellariae granule;
(5) with embodiment 1.
Comparative example 2:
With reference to the method described in patent of invention CN102145049B, prepare YIQING KELI: Rhizoma Coptidis 264g, Radix Et Rhizoma Rhei 800g, Radix Scutellariae 400g; Rhizoma Coptidis, Radix Scutellariae decoct with water respectively three times, add for the first time 8 times of water gagings and decoct 1.5h, and second adds 6 times of water gagings decocts 1h, adds for the third time 8 times of water gagings and decocts 2h; Radix Et Rhizoma Rhei is with 60% ethanol extraction, 6 times of amounts that consumption is medical material, reflux, extract, 1h; Collecting decoction, filters, and when filtrate is concentrated into 70 ℃ of surveys, relative density is about 1.25, is spray dried to dry extract; Above-mentioned three kinds of extract powders are added to appropriate sucrose and dextrin, mix, granulation, dry, obtain YIQING KELI.
Comparative example 3: commercially available YIQING KELI.
Testing result is as shown in table 1.
The melting of table 1 YIQING KELI
As can be known from Table 1, the M value of the embodiment of the present invention 1～5 is significantly less than comparative example 1, comparative example 2 and commercially available YIQING KELI, and the melting of embodiment 1～5 is obviously more excellent.Show that the dry extract that the inventive method obtains Rhizoma Coptidis, Radix Et Rhizoma Rhei, three kinds of medicinal material extract of Radix Scutellariae granulates respectively, in the process of preparing Radix Et Rhizoma Rhei granule and Radix Scutellariae granule, add respectively sodium hydroxide, can significantly improve the melting of YIQING KELI simultaneously.Comparing embodiment 1～5 is known, because embodiment 5 does not add ethanol in the process of three kinds of granules of preparation, causes the melting of YIQING KELI of embodiment 5 preparation relatively poor; Wherein the melting of embodiment 1 is best.
Experiment two: antiinflammatory experiment
(1) xylol causes the impact of mice ear:
Getting body weight is the male mice random packet of 19～21g, every group 10, gavage gives trial drug (5g/kg), control drug and equivalent distilled water (matched group) respectively, once a day, and continuous three days, after last administration, 60min is only evenly coated with dimethylbenzene 0.05ml/ to the left auricle of mice two sides, causing scorching rear 30min execution mice, the rustless steel punching pin that is 8mm with diameter takes off left and right same area auricle, weighs, be calculated as follows swelling and inhibitory rate of intumesce, result is as shown in table 2.
Swelling=(left auricle weight-auris dextra sheet weight)
Table 2 xylol cause mice ear impact (n=10,
)
| Group | Swelling mg | Suppression ratio % |
| Matched group | 22.3±2.1 | / |
| Embodiment 1 | 5.4±2.5 | 75.78 |
| Embodiment 2 | 7.8±2.7 | 65.02 |
| Embodiment 3 | 8.3±2.2 | 62.78 |
| Embodiment 4 | 7.9±2.6 | 64.57 |
| Embodiment 5 | 10.1±2.2 | 54.71 |
| Comparative example 1 | 13.3±2.7 | 40.36 |
| Comparative example 2 | 16.4±3.2 | 26.46 |
| Commercially available YIQING KELI | 15.9±2.5 | 28.70 |
As can be seen from Table 2, with respect to matched group, the acute inflammation that the equal xylol of each administration group brings out has inhibitory action in various degree; The YIQING KELI successful of embodiment 1～embodiment 5 preparations is better than comparative example 1, comparative example 2 and commercially available YIQING KELI, can make mice auricle swelling degree significantly reduce; Wherein embodiment 1 effect is best.
(2) on Carrageenan causes the impact of rat paw edema
Getting body weight is the male rat random packet of 180～210g, every group 10, gavage gives trial drug (5g/kg), control drug and equivalent distilled water (matched group) respectively, once a day, continuous three days, after last administration, 60min only caused inflammation in Rat Right metapedes subcutaneous injection 1% carrageenin 0.3ml/, before Yu Zhiyan and cause scorching after 4h, with sufficient sole of the foot plethysmometer, measure rat foot volume, and calculate swelling degree of the paw, the results are shown in Table 3.
Swelling (%)=[(cause scorching metapedes volume-cause scorching front foot volume)/cause scorching front foot volume] * 100%
Table 3 on Carrageenan causes the impact of rat paw edema
As can be seen from Table 3, with respect to matched group, the equal on Carrageenan of each administration group causes rat paw edema inhibitory action in various degree; The YIQING KELI successful of embodiment 1～embodiment 5 preparations is better than comparative example 1, comparative example 2 and commercially available YIQING KELI; Wherein the effect of embodiment 1 is best.
Experiment three: hemostasis experiment
Getting body weight is the male mice random packet of 19～21g, every group 10, gavage gives trial drug (5g/kg), control drug and equivalent distilled water (matched group) respectively, once a day, continuous three days, after last administration 60min, mice is placed in to special holder, cuts off Mus tail point 0.3cm, treat that blood overflows voluntarily, every 30s, with filter paper, suck drop of blood, during suction, firmly do not push section, until hemorrhage, naturally stop, calculating the bleeding time.The results are shown in Table 4.
Table 4 is on the mice impact (± s) in docking bleeding time
| Group | Every group of quantity | Bleeding time (min) |
| Matched group | 10 | 6.14±1.51 |
| Embodiment 1 | 10 | 3.30±1.57 |
| Embodiment 2 | 10 | 3.87±1.64 |
| Embodiment 3 | 10 | 3.81±1.82 |
| Embodiment 4 | 10 | 3.96±1.65 |
| Embodiment 5 | 10 | 4.15±1.74 |
| Comparative example 1 | 10 | 4.34±1.66 |
| Comparative example 2 | 10 | 5.39±1.71 |
| Commercially available YIQING KELI | 10 | 5.37±1.98 |
As can be seen from Table 4, with respect to matched group, each administration group all has shortening effect in various degree to the mice docking bleeding time, and the successful of embodiment 1～embodiment 5 is better than comparative example 1, comparative example 2 and commercially available YIQING KELI, and wherein embodiment 1 effect is best.
Claims (9)
1. a preparation method for YIQING KELI, is characterized in that, comprises the following steps:
(1) by YIQING KELI formula, get Rhizoma Coptidis, Radix Et Rhizoma Rhei, Radix Scutellariae, decocts with water respectively, and collecting decoction filters, and filtrate decompression is concentrated into clear paste, and spraying is dry, obtains respectively Rhizoma Coptidis dry extract, Radix Et Rhizoma Rhei dry extract and Radix Scutellariae dry extract;
(2) get the Rhizoma Coptidis dry extract that step (1) makes, add pharmaceutically acceptable adjuvant, mix, add ethanol water or water, granulation, dry, obtain Rhizoma Coptidis granule;
(3) get the Radix Et Rhizoma Rhei dry extract that step (1) makes, add pharmaceutically acceptable adjuvant, mix, add sodium hydrate aqueous solution or containing the ethanol water of sodium hydroxide, granulation, dry, obtain Radix Et Rhizoma Rhei granule;
(4) get the Radix Scutellariae dry extract that step (1) makes, add pharmaceutically acceptable adjuvant, mix, add sodium hydrate aqueous solution or containing the ethanol water of sodium hydroxide, granulation, dry, obtain Radix Scutellariae granule;
(5) Rhizoma Coptidis granule step (2)～(4) being made respectively, Radix Et Rhizoma Rhei granule are mixed homogeneously with Radix Scutellariae granule, are distributed into bag, obtain YIQING KELI.
2. preparation method according to claim 1, is characterized in that: in described step (1), the weight portion proportioning of Rhizoma Coptidis, Radix Et Rhizoma Rhei and Radix Scutellariae is Rhizoma Coptidis 150-400 part, Radix Et Rhizoma Rhei 600-900 part, Radix Scutellariae 200-600 part.
3. preparation method according to claim 1, is characterized in that: on described step (2)～(4) Chinese materia medica, acceptable adjuvant is selected from a kind of or several arbitrarily in dextrin, cane sugar powder, soluble starch, lactose and sodium cyclamate.
4. preparation method according to claim 1, is characterized in that: in described step (2), in adjuvant and step (1), the weight ratio of Rhizoma Coptidis is 1-3:3-8.
5. preparation method according to claim 1, is characterized in that: in described step (2), ethanol water or the volume of water and the weight ratio of adjuvant are 1～3ml:5-15g; Wherein in ethanol water, the percentage by volume of ethanol is 5～70%.
6. preparation method according to claim 1, is characterized in that: in described step (3), in adjuvant and step (1), the weight ratio of Radix Et Rhizoma Rhei is 2-5:6-9.
7. preparation method according to claim 1, it is characterized in that: sodium hydrate aqueous solution or be 2-6ml:10-25g containing the volume of ethanol water and the weight ratio of adjuvant of sodium hydroxide in described step (3), sodium hydrate aqueous solution or be 0.5～3% containing the mass percent of sodium hydroxide in the ethanol water of sodium hydroxide is wherein 5～70% containing the percentage by volume of ethanol in the ethanol water of sodium hydroxide.
8. preparation method according to claim 1, is characterized in that: in described step (4), in adjuvant and step (1), the weight ratio of Radix Scutellariae is 2-5:2-6.
9. preparation method according to claim 1, it is characterized in that: sodium hydrate aqueous solution or be 4-15ml:20-50g containing the volume of ethanol water and the weight ratio of adjuvant of sodium hydroxide in described step (4), sodium hydrate aqueous solution or be 0.5～3% containing the mass percent of sodium hydroxide in the ethanol water of sodium hydroxide is wherein 5～70% containing the percentage by volume of ethanol in the ethanol water of sodium hydroxide.
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| CN113827571A (en) * | 2021-09-26 | 2021-12-24 | 陕西孙思邈高新制药有限公司 | Yiqing granule prescription and preparation method thereof |
| CN115154427A (en) * | 2022-08-15 | 2022-10-11 | 保定冀中药业有限公司 | Preparation method for improving damp-heat diarrhea effect of Sihuang diarrhea-stopping granules |
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| CN102145049A (en) * | 2010-02-09 | 2011-08-10 | 北京亚东生物制药有限公司 | Preparation method of Yiqing granules |
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| CN102145049A (en) * | 2010-02-09 | 2011-08-10 | 北京亚东生物制药有限公司 | Preparation method of Yiqing granules |
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| 郑姗姗: "一清颗粒喷雾干燥工艺的研究", 《海峡药学》, vol. 21, no. 9, 31 December 2009 (2009-12-31) * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113827571A (en) * | 2021-09-26 | 2021-12-24 | 陕西孙思邈高新制药有限公司 | Yiqing granule prescription and preparation method thereof |
| CN115154427A (en) * | 2022-08-15 | 2022-10-11 | 保定冀中药业有限公司 | Preparation method for improving damp-heat diarrhea effect of Sihuang diarrhea-stopping granules |
| CN115154427B (en) * | 2022-08-15 | 2023-07-11 | 保定冀中药业有限公司 | Preparation method for improving effect of Sihuang dysentery stopping particles in treating damp-heat dysentery |
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