CN101933996B - Chinese medicinal composition having effects of clearing heat, relieving fire and eliminating toxins and preparation and detection methods thereof - Google Patents
Chinese medicinal composition having effects of clearing heat, relieving fire and eliminating toxins and preparation and detection methods thereof Download PDFInfo
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Abstract
The invention discloses a medicinal composition having effects of clearing heat, relieving fire and eliminating toxins and preparation and detection methods thereof. The medicinal composition is prepared from the following raw materials: coptsir root, Chinese teasel root and baikal skullcap root. The preparation method comprises the following steps of: adding water into the three raw materials for decoction for 2 to 3 times, wherein the amount of the added water is 6 to 9 times that of the raw materials and the decoction time is 1 to 2 hours for each time; combining decoction solution and filtering the mixed solution; concentrating filtrate to ensure that the relative density is about 1.25 (detected at the temperature of 65 to 75 DEG C); performing spray drying on the obtained product to obtain dry powdered extract; adding a proper amount of cane sugar and dextrine into the dry powdered extract; uniformly mixing the mixture; preparing the mixture into particles; and drying the particles to obtain 1,000g of particles so as to obtain the finished product. In the detection method, the content of baicalin is measured by high performance liquid chromatography. The medicinal composition has good effects of clearing the heat, relieving the fire and eliminating the toxins.
Description
The present invention is for dividing an application, and the original bill application number is 200710064797.1, and the original bill applying date is on March 27th, 2007, and the original bill name is called a kind of Chinese medicine composition with clearing heat-fire detoxication and preparation method thereof and method of quality control.
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof and method of quality control, particularly relate to a kind of Chinese medicine composition and preparation method thereof and method of quality control with clearing heat-fire detoxication.
Background technology
In recent years; Along with people's growth in the living standard and working pressure increase; Reasons such as, rhythm of life confusion rich owing to overfeeding; The get angry disease incidence of symptom such as chronic pharyngitis, tonsillitis constantly rises, and Chinese medicine of the prior art all can not solve whole situations of above-mentioned existence, is the task of top priority so seek a medicine that can solve the symptomatology of above-mentioned existence.
Use this type of disease of treatment by Chinese herbs then can avoid the shortcoming of above-mentioned Western medicine, traditional Chinese medicine thinks that flu is because ailment said due to cold or exposure when taking advantage of human body to drive evil scarce capacity, and the invasion and attack lung is defended due to the fur.The many medicines with dispersing superficial exopathogens, releasing table disease of Chinese medicine are main treatment, make outer evilly separate from sweat, be equipped with purging intense heat and detonicating, removing heat from the lung and relieving sorethroat etc. clearing heat and detoxicating and induce sweat in medicine, make above-mentioned symptom be able to alleviate and cure.Therefore the patient uses saferly during this symptom of treatment by Chinese herbs, is difficult for producing drug resistance, can also enhances human body the prevention ability of disease and evil to external world.
Medicine of the present invention as go heat-clearing, reduce internal heat, the representative medicine of antidote, have clinical application effect preferably.The body heat that is used for due to the fiery malicious blood-head is irritated, the hot eyes aphtha, and throat, swelling and aching of gum, constipation, and pharyngitis, tonsillitis, gingivitis see the above-mentioned symptom, and the person has good effect.
Summary of the invention
The object of the invention is to provide a kind of Chinese medicine composition with clearing heat-fire detoxication;
The object of the invention also is to provide a kind of Chinese medicine composition preparation method with clearing heat-fire detoxication;
The object of the invention also is to provide a kind of method of quality control with Chinese medicine composition of clearing heat-fire detoxication.
The present invention seeks to realize through following technical scheme:
Chinese medicine composition with clearing heat-fire detoxication of the present invention is to be processed by the bulk drug of following weight ratio:
Coptis 100-300 weight portion rheum officinale 400-700 weight portion root of large-flowered skullcap 150-380 weight portion
The above-mentioned raw materials optimum ratio is:
Coptis 100-150 weight portion rheum officinale 600-700 weight portion root of large-flowered skullcap 150-250 weight portion
Chinese medicine composition with clearing heat-fire detoxication of the present invention can be processed by the bulk drug of following weight ratio:
Coptis 100-300 weight portion rheum officinale 400-700 weight portion root of large-flowered skullcap 150-380 weight portion root bark of tree peony 100-200 golden cypress 100-200
The above-mentioned raw materials optimum ratio is:
Coptis 100-150 weight portion rheum officinale 600-700 weight portion root of large-flowered skullcap 150-250 weight portion root bark of tree peony 100-150 weight portion golden cypress 100-150 weight portion
The above-mentioned raw materials optimum ratio is:
The coptis 140 weight portion rheum officinales 650 weight portion roots of large-flowered skullcap 200 weight portions
The root bark of tree peony 130 weight portion golden cypresses 140 weight portions
Composition of the present invention can add auxiliary material by common process and process clinical acceptable forms such as tablet, capsule, oral liquid, dripping pill, spray, granule; Said auxiliary material comprises solvent, disintegrant, flavouring, antiseptic, colorant, bonding agent, lubricant, matrix etc.
The preparation method of Chinese medicine composition granular preparation of the present invention is:
Choose bulk drug: coptis 100-300 weight portion rheum officinale 400-700 weight portion root of large-flowered skullcap 150-380 weight portion
Method for making: above three flavors, boiling is 2-3 time respectively, adds 6-9 times of water gaging at every turn and decocts 1-2 hour, and collecting decoction filters, and filtrating is concentrated into relative density and is about 1.25 (65-75 ℃ of surveys), is spray dried to dry extract; Above-mentioned three kinds of extract powders are added an amount of sucrose and dextrin, and mixing is processed particle, and drying makes particle 1000 weight portions, promptly gets.
The preparation method of Chinese medicine composition granular preparation of the present invention is:
Choose bulk drug:
Coptis 100-300 weight portion rheum officinale 400-700 weight portion root of large-flowered skullcap 150-380 weight portion root bark of tree peony 100-200 weight portion golden cypress 100-200 weight portion;
Method for making: rheum officinale boiling 2-3 time adds 6-9 times of water gaging at every turn and decocted 1-2 hour; The coptis, the root of large-flowered skullcap, the root bark of tree peony, golden cypress boiling 2-3 time add 6-9 times of water gaging at every turn and decocted 1-2 hour; Collecting decoction filters, and filtrating is concentrated into relative density and is about 1.25 (65-75 ℃ of surveys), is spray dried to dry extract; Above-mentioned extract powder is added an amount of sucrose and dextrin, and mixing is processed particle, and drying makes particle 1000 weight portions, promptly gets.
Pharmaceutical composition method of quality control of the present invention comprises one or more in following discrimination method and/or the assay:
Differentiate:
(1) get present composition granule 6-10g, add methyl alcohol 40-60ml, flooded 1-3 hour, and jolting constantly; Filter, filtrating is put evaporate to dryness in the water-bath, and residue adds water 8-12ml makes dissolving, adds hydrochloric acid 1ml again; Put in the water-bath and heated 25-35 minute, cooling divides 2-3 extraction with chloroform 18-22ml immediately; Combined chloroform liquid is concentrated into about 1ml, as need testing solution; Other gets the archen reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to thin-layered chromatography; Draw above-mentioned two kinds of solution, 10 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, (13-18: 4-6: upper solution 1-2) is a developping agent with sherwood oil (60～90 ℃)-ethyl formate-formic acid; Launch; Take out, dry, it is stifling clear to the spot colour developing to put in the ammonia steam; In the test sample chromatogram, with control medicinal material chromatogram relevant position on, show identical punctation;
(2) get present composition granule 4-7g, add 28-34ml methyl alcohol dipping 1-2 hour, jolting constantly filters evaporate to dryness; Residue is dissolved in water, and transferring pH with watery hydrochloric acid again is 1-2, extracts 2-3 time with the ethyl acetate jolting, and each 14-16ml merges ethyl acetate liquid, evaporate to dryness; With the 1ml dissolve with methanol as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and processes the solution that every 1ml contains 2mg, as reference substance solution; According to the thin-layered chromatography test, get each 2 μ l of above-mentioned two kinds of solution and put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (8-12: 6-9: 1-2: 1-2) be developping agent, launch, take out that dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, with reference substance chromatogram relevant position on show the spot of same color;
(3) get present composition granule 7-9g, add methyl alcohol 45-55ml, flooded 1-3 hour, and jolting constantly, filtering, filtrating is put and is concentrated into about 1ml in the water-bath, as need testing solution; Other gets the Berberine hydrochloride reference substance and adds methyl alcohol and process the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to thin-layered chromatography; Draw each 1 μ l of above-mentioned two kinds of solution, put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is a binder, with ethyl acetate-butanone-formic acid-water (9-12: 5-7: 1-2: 1-2) be developping agent; Launch; Take out, dry, under ultraviolet lamp (365nm), inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on show identical yellow fluorescence spot;
Assay:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.2mol/L phosphate sodium dihydrogen buffer solution (regulating pH to 2.7) (40-44: 55-65) be moving phase with phosphoric acid; The detection wavelength is 275nm; Number of theoretical plate calculates by the scutelloside peak should be not less than 5000;
The preparation of reference substance solution: precision takes by weighing the scutelloside reference substance 12.5mg that is dried to constant weight at 105 ℃, puts in the 250ml measuring bottle, with the small amount of methanol dissolving, is diluted to scale with double distilled water, shakes up, and promptly gets (containing scutelloside 50 μ g among every 1ml);
The preparation of need testing solution: get the content under the present composition granule content uniformity item, mixing, porphyrize; Get about 0.75g, the accurate title, decide, and puts in the 100ml measuring bottle; Add methyl alcohol 10ml, sonicated 8-12 minute, be diluted to scale with double distilled water; Get the centrifugal 8-12 of this liquid minute (the per minute rotating speed is that 13000-18000 changes), obtain supernatant, promptly get;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get.
In preferred following discrimination method of pharmaceutical composition method of quality control of the present invention and/or the assay one or more:
Differentiate:
(1) get these article 8g, add methyl alcohol 50ml, flooded 2 hours, and jolting constantly; Filter, filtrating is put evaporate to dryness in the water-bath, and residue adds water 10ml makes dissolving, adds hydrochloric acid 1ml again; Put in the water-bath and heated 30 minutes, cooling divides 2 extractions with chloroform 20ml immediately; Combined chloroform liquid is concentrated into about 1ml, as need testing solution; Other gets the archen reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to thin-layered chromatography; Draw above-mentioned two kinds of solution, 10 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with the upper solution of sherwood oil (60～90 ℃)-ethyl formate-formic acid (15: 5: 1); Launch; Take out, dry, it is stifling clear to the spot colour developing to put in the ammonia steam; In the test sample chromatogram, with reference substance chromatogram relevant position on, show identical punctation;
(2) get these article 5g, add 30ml methyl alcohol dipping 1 hour, jolting constantly filters evaporate to dryness; Residue is dissolved in water, and transferring pH with watery hydrochloric acid again is 1-2, extracts 2 times with the ethyl acetate jolting, and each 15ml merges ethyl acetate liquid, evaporate to dryness; With the 1ml dissolve with methanol as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and processes the solution that every 1ml contains 2mg, as reference substance solution; According to the thin-layered chromatography test, get each 2 μ l of above-mentioned two kinds of solution and put respectively on same silica gel g thin-layer plate, (10: 7: 1: 1) be developping agent, launch that taking-up is dried, spray was with 2% ferric trichloride ethanolic solution with ethyl acetate-butanone-formic acid-water; In the test sample chromatogram, with reference substance chromatogram relevant position on show the spot of same color;
(3) get these article 8g, add methyl alcohol 50ml, flooded 2 hours, and jolting constantly, filtering, filtrating is put and is concentrated into about 1ml in the water-bath, as need testing solution; Other gets the Berberine hydrochloride reference substance and adds methyl alcohol and process the solution that every 1ml contains 0.5mg, as reference substance solution; According to thin-layered chromatography test, draw each 1 μ l of above-mentioned two kinds of solution, put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is a binder; (10: 6: 1: 1) be developping agent, expansion was taken out with ethyl acetate-butanone-formic acid-water; Dry, under ultraviolet lamp (365nm), inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on show identical yellow fluorescence spot;
Assay:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.2mol/L phosphate sodium dihydrogen buffer solution (regulating pH to 2.7 with phosphoric acid) (42: 58) is moving phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the scutelloside peak should be not less than 5000; The preparation of reference substance solution: precision takes by weighing the scutelloside reference substance 12.5mg that is dried to constant weight at 105 ℃, puts in the 250ml measuring bottle, with the small amount of methanol dissolving, is diluted to scale with double distilled water, shakes up, and promptly gets (containing scutelloside 50 μ g among every 1ml);
The preparation of need testing solution: get the content under these article content uniformity item, mixing, porphyrize; Get about 0.75g, the accurate title, decide, and puts in the 100ml measuring bottle; Add methyl alcohol 10ml, sonicated 10 minutes is diluted to scale with double distilled water; Got this liquid centrifugal 10 minutes (the per minute rotating speed is 15000 commentaries on classics), obtain supernatant, promptly get;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get; These article contain the root of large-flowered skullcap with scutelloside (C for every bag
21H
18O
11) meter, must not be less than 21mg.
The present composition has good clearing heat-fire detoxication, compares shuanghuanglian mixture, shuanghuanglian koufuye and shows good drug effect.Body heat to due to the malicious blood-head of fire is irritated, the hot eyes aphtha, and throat, swelling and aching of gum, constipation, and pharyngitis, tonsillitis, gingivitis have good effect.
The method of quality control of Chinese medicine composition provided by the present invention; Be through obtaining behind the creative experiment sieving of big measuring; Through the screening to sample treatment, the selection of developping agent makes and differentiates that specificity is fine in the discrimination method; And method is economic and practical, the result is quick, and can both use different thin layer plates.Pass through screening in the content assaying method to sample, test sample disposal route; The selection of developping agent; Make content assaying method effectivelyly to carry out quality control, and will compare more stable that product that additive method measures shows on pharmacological effect with the product that this method is measured to product.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Experimental example 1 pharmacological testing
Medicine 1 adopts embodiment 7
Medicine 2 adopts embodiment 1
1, clearing heat-fire effect:
Get the white big ear rabbit of body weight at 2.0～3.0kg, male and female have concurrently, experiment the previous day choose body temperature at 38.0～39.4 ℃, and body temperature changed the rabbit be no more than 0.4 ℃ and used rabbit as experiment the same day.On the same day, measure basal body temperature before the modeling, oneself rabbit ear vein bacterial injection endotoxin normal saline solution; Dosage is 1ml.kg-1 (10ml); Observation body temperature changes, and per 0.5 hour record is once chosen behind the injection 1h body temperature and risen and surpass 0.5 ℃ rabbit; Be divided into 5 groups at random, 8 every group: the large, medium and small dose groups of medicine of the present invention, blank group.Irritate stomach to rabbit, after the administration, continue to observe rabbit body temperature and change, per 0.5 hour record once, continuous recording 5h is an observation index with the animal heat of every 0.5h and the difference of basal body temperature, data are carried out t and are checked, the result sees the following form:
The influence of the fever in rabbit body temperature that bacterial endotoxin is caused
Annotate: compare * P＜0.05, * * P＜0.01 with control group
The result shows: 1 group, 2 groups high, medium and low dosage of medicine of the present invention all have obvious inhibiting effect to fever in rabbits due to the bacterial endotoxin, relatively have significant difference with blank control group, and 2 groups of same doses of medicine of the present invention are superior to 1 group of medicine of the present invention.
2, detoxication:
Experiment was surveyed body temperature 3 in advance with rat, and experiment measured value on the same day is the rat basal body temperature, and the variation of screening body temperature is no more than 0.3 ℃ animal; Be divided into 5 groups at random; Every group 13: blank group, the large, medium and small dosage of medicine of the present invention, behind the gastric infusion, inject 1% carrageenan solution 0.1ml under the rat right hind leg sole immediately; Record causes before the inflammation and causes scorching back 1～6h rat foot volume, and calculating swelling rate.
The inhibiting effect of on Carrageenan solution mouse sole swelling
The result shows: 1 group, 2 groups high, medium and low dosage of medicine of the present invention all can significantly suppress the volume of rat swelling sole, have the effect of antibacterial detoxifcation.Medicine of the present invention and blank group relatively have significant difference, and 2 groups of same doses of medicine of the present invention are superior to 1 group of medicine of the present invention.
Experimental example 2 is differentiated screening experiment
1, thin layer to rheum officinale is differentiated in the pharmaceutical preparation of the present invention
(1) thin layer of rheum officinale is differentiated the preferred of developping agent proportioning in the above-mentioned discrimination method:
Draw need testing solution, each 10 μ l of reference substance solution respectively; Put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Sherwood oil with 60～90 ℃: ethyl formate: the upper solution that formic acid was respectively 15: 5: 1,10: 5: 1,5: 5: 1,20: 10: 1 is a developping agent, launches, and takes out; Dry, it is stifling clear to the spot colour developing to put in the ammonia steam.Observe the effect that the test sample principal spot launches on the thin layer plate, the result sees the following form:
Developping agent proportion optimization experimental result table in the discrimination method of rheum officinale
Can find out that from last table the developping agent proportioning is at 15: 5: 1 o'clock, on thin layer plate, launch effectively that principal spot is clear, does not have hangover, and is identical with the speckle displacement and the color of reference substance, is fit to testing requirements.
(2) sample solution point sample amount preferred in the above-mentioned rheum officinale discrimination method:
Draw need testing solution 1 μ l, 5 μ l, 10 μ l, 15 μ l points on same silica gel g thin-layer plate; With benzene-ethyl acetate-formic acid solution proportioning is that (8: 5: 0.8) are developping agent, launches, and takes out; Dry; It is stifling clear to the spot colour developing to put in the ammonia steam, the effect of observing test sample principal spot colour developing on the thin layer plate, and the result sees the following form:
Sample solution point sample amount optimization experiment table as a result in the discrimination method of rheum officinale
Can find out test sample point sample amount when the 10 μ l from last table, color developing effect is good on thin layer plate, is fit to testing requirements.
(3) negative control test
Get the negative sample that lacks rheum officinale, prepare negative control solution, launch the back and corresponding spot on the reference substance solution correspondence position, do not occur, explain that selected identification experiment specificity is strong according to need testing solution preparation method in the discrimination method of above-mentioned rheum officinale.
2, thin layer to the root of large-flowered skullcap is differentiated in the pharmaceutical preparation of the present invention
(1) developping agent preferred in the above-mentioned root of large-flowered skullcap discrimination method:
1. draw each 2 μ l of need testing solution, reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: butanone: formic acid: water, ethyl formate: butanone: formic acid: water, ethyl acetate: ketone: acetate: water is developping agent; Launch; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; Observe the effect of test sample principal spot colour developing on the thin layer plate, the result sees the following form:
Developping agent optimization experiment table as a result in the root of large-flowered skullcap discrimination method
2. with ethyl acetate: butanone: formic acid: the water proportioning was respectively 10: 7: 1: 1,10: 10: 1: 1,10: 8: 2: 1,10: 7: 2: 1 developping agent launches, and observes the effect that the test sample principal spot launches on the thin layer plate, and the result sees the following form:
The optimization experiment of developping agent proportioning is table as a result
From 1. above and 2. test findings can find out that select ethyl acetate: butanone: formic acid: water is 10: 7: 1: 1 developping agent, principal spot launch effect and color developing effect identical with the reference substance principal spot, the Pass Test requirement.
(2) sample solution point sample amount preferred in the discrimination method of the above-mentioned root of large-flowered skullcap:
Draw need testing solution 0.5 μ l, 1.0 μ l, 1.5 μ l, 2 μ l points on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (10: 7: 1: 1) be developping agent, expansion; Take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram; With reference substance chromatogram relevant position on show the spot of same color, the effect of observing test sample principal spot colour developing on the thin layer plate, the result sees the following form:
Sample solution point sample amount optimization experiment table as a result in the discrimination method of the root of large-flowered skullcap
Can find out test sample point sample amount when the 2 μ l from last table, color developing effect is good on thin layer plate, is fit to testing requirements.
(3) negative control test
Get the negative sample that lacks the root of large-flowered skullcap, prepare negative control solution, launch the back and corresponding spot on the reference substance solution correspondence position, do not occur, explain that selected identification experiment specificity is strong according to need testing solution preparation method in the above-mentioned root of large-flowered skullcap discrimination method.
3, thin layer to coptis root is differentiated in the pharmaceutical preparation of the present invention
(1) developping agent proportioning preferred in the above-mentioned coptis root discrimination method:
Be 10: 10: 1 with ethyl acetate-butanone-formic acid-water respectively: 1,10: 8: 1: 1,10: 6: 1: 1,10: 6: 2: 1 developping agent, observe the effect that the test sample principal spot launches on the thin layer plate, the result sees the following form:
Developping agent proportion optimization experimental result in the coptis root discrimination method
Can find out from last table, be 10: 6: 1 with ethyl acetate-butanone-formic acid-water proportioning: 1 o'clock, launch effect, and separating effect is all better.
(2) sample solution point sample amount preferred in the above-mentioned coptis root discrimination method:
Get need testing solution 0.5 μ l, 1.0 μ l, 1.5 μ l, 2 μ l, point sample is 10: 6: 1 with ethyl acetate-butanone-formic acid-water proportioning: 1 developping agent on the silica G plate respectively; Launch; Taking out, dry, is to inspect under the 365nm in the ultraviolet lamp wavelength; Observe the effect of test sample principal spot colour developing on the thin layer plate, the result sees the following form:
Sample solution point sample amount optimization experiment result in the discrimination method of coptis root
Can find out test sample point sample amount when the 1.0 μ l from last table, color developing effect is good on thin layer plate, is fit to testing requirements.
(3) negative control test
Get the negative sample that lacks coptis root, prepare negative control solution, launch the back and corresponding spot on the reference substance solution correspondence position, do not occur, explain that selected identification experiment specificity is strong according to need testing solution preparation method in the above-mentioned coptis root discrimination method.
The experiment of experimental example 3 assays
Adopt the high-efficient liquid phase color popularize law to measure the content of baicalin in the medicine of the present invention, to improve quality determining method of the present invention:
(1) moving phase reagent is preferred:
Be that 15: 85 solution, 0.05mol/L methyl alcohol and potassium dihydrogen phosphate ratio is 40: 65 solution, 0.2mol/L methyl alcohol with acetonitrile and water ratio respectively: phosphate sodium dihydrogen buffer solution is that 42: 58 solution is moving phase; Carry out test sample and dissolve the assay at night; Through comparing among the general figure of high-efficient liquid phase color; The separating effect at each peak is confirmed preferred moving phase, and the result sees the table following table:
The optimization experiment result of moving phase reagent
Can find out that from last table moving phase is selected 0.2mol/L methyl alcohol: phosphate sodium dihydrogen buffer solution is that 42: 58 solution more can effectively separate each peak, and assay is more accurate.
(2) proportion of mobile phase is preferred:
Respectively with 0.2mol/L methyl alcohol: the phosphate sodium dihydrogen buffer solution proportioning is that (30: 80), (40: 70), (42: 60), (42: 58) are moving phase; Carry out test sample and dissolve the assay at night; Through comparing among the general figure of high-efficient liquid phase color; The separating effect at each peak is confirmed preferred moving phase, and the result sees the following form:
The optimization experiment result of proportion of mobile phase
Can find out that from last table proportion of mobile phase is selected 42: 58 for well.
Detecting instrument (room temperature detection): Agilent 1100 type high performance liquid chromatographs: chromatographic column: (Zorbax C184.6 * 150mm, 5 μ m) producer: Agilent Techologies Anjelen Sci. & Tech. Inc (China)
Moving phase: methyl alcohol-0.2mol/L phosphate sodium dihydrogen buffer solution (regulating PH to 2.7) (42: 58) with phosphoric acid
Detect wavelength: 275nm flow velocity: 1.000ml/min column temperature: room temperature
The reference substance source: scutelloside is purchased lot number: the 0715-9909 in Nat'l Pharmaceutical & Biological Products Control Institute
Assay method: the preparation method who gets by need testing solution under [assay] item prepares sample liquid; And by preparing the blank sample that lacks the root of large-flowered skullcap under [method for making] item, the preparation negative controls.With miillpore filter (0.45 μ m).The accurate respectively negative controls of drawing, each 10 μ l of reference substance liquid and need testing solution inject liquid chromatograph, measure, and promptly get.
1. content assaying method is investigated:
(1) stability test reference substance solution respectively at preparing the back 0,2,4,6,12,24 hour, is measured in accordance with the law, and the result shows that it is basicly stable in 24 hours, and the result sees the following form:
(2) linear relationship is investigated and to be got reference substance solution (95.6 μ g/ml) and shake up; Accurate respectively 1,3,5,7,9, the 11 μ l of absorption inject high performance liquid chromatograph; Measure peak area, the result sees the following form, and the drawing standard curve; Show that scutelloside is linear between 0.0956 μ g-1.0516 μ g, its regression equation is:
Area＝3314.362273*Amt-5.59596(r＝0.999998)
(3) the accurate need testing solution of drawing of precision test, (lot number: 04010701) 10 μ l, repeat sample introduction 5 times, try to achieve relative standard deviation＜2%, the result sees the following form:
(4) the text method is pressed in the reappearance test, gets same lot number sample and measures, and tries to achieve relative standard deviation＜2%, and the result sees the following form:
(5) the recovery test precision takes by weighing the same lot number (lot number: sample 0.375g 04010802) of known content; Put in the 100ml measuring bottle; Add 10ml scutelloside reference substance solution (0.133mg/ml), press preparation method's operation of text need testing solution, measure its content; And calculate its recovery, measure the result and see the following form:
Can find out that by above methodology examination result its linear relationship of the content assaying method that medicine of the present invention adopted, stability, precision, reappearance etc. are all good, can effectively control drug quality of the present invention.
Can find out from the result of study of above quality determining method, the quality determining method science that pharmaceutical preparation of the present invention adopted, rationally, have originality, can effectively control pharmaceutical preparation quality of the present invention.
Following embodiment all can realize the described effect of above-mentioned experimental example
Embodiment
Embodiment 1: granule
Coptis 140g rheum officinale 650g root of large-flowered skullcap 200g root bark of tree peony 130g golden cypress 140g
Rheum officinale boiling 2 times adds 8 times of water gagings at every turn and decocted 1 hour; The coptis, the root of large-flowered skullcap, the root bark of tree peony, golden cypress boiling 2 times add 7 times of water gagings at every turn and decocted 1 hour; Collecting decoction filters, and filtrating is concentrated into relative density and is about 1.25 (65-75 ℃ of surveys), is spray dried to dry extract; Above-mentioned extract powder is added an amount of sucrose and dextrin, and mixing is processed particle, and drying makes particle 1000g, promptly gets.
Embodiment 2: dripping pill
Coptis 176g rheum officinale 533.3g root of large-flowered skullcap 266.7g
Method for making: above three flavors, difference boiling secondary, 1.5 hours for the first time; The 21 hour, collecting decoction filtered; Filtrating is concentrated into 70 ℃ of relative densities and is about 1.25, adds in Macrogol 4000 and the matrix that Macrogol 6000 mixes, splashes in the whiteruss with certain speed; The drop ball promptly gets.
Embodiment 3: effervescent agent
Coptis 150g rheum officinale 550g root of large-flowered skullcap 300g root bark of tree peony 140g golden cypress 150g
Method for making: the above five tastes, difference boiling secondary, 1.5 hours for the first time, the 21 hour, collecting decoction filtered, and filtrating is concentrated into 70 ℃ of relative densities and is about 1.25 thick paste; After the polyglycol dissolving, behind the adding soda mint, be sprayed in the thick paste, with sweetener and acid compressing tablet, promptly get.
Embodiment 4:
Coptis 136g rheum officinale 673.3g root of large-flowered skullcap 246.7g
This pharmaceutical composition adds conventional auxiliary material, processes capsule through common process.
Embodiment 5:
Coptis 146g rheum officinale 653.3g root of large-flowered skullcap 236.7g
This pharmaceutical composition adds conventional auxiliary material, processes tablet through common process.
Embodiment 6:
Coptis 150g rheum officinale 550g root of large-flowered skullcap 300g golden cypress 150g
This pharmaceutical composition adds conventional auxiliary material, processes capsule through common process.
Embodiment 7:
Coptis 176g rheum officinale 533.3g root of large-flowered skullcap 266.7g
Method for making: above three flavors, the boiling secondary adds 8 times of water gagings for the first time and decocted 1.5 hours respectively, and second adds 6 times of water gagings decocted 1 hour, and collecting decoction filters, and filtrating is concentrated into relative density and is about 1.25 (70 ℃ of surveys), is spray dried to dry extract; Above-mentioned three kinds of extract powders are added an amount of sucrose and dextrin, and mixing is processed particle, and drying makes particle 1000g, promptly gets;
Differentiate:
(1) get these article 8g, add methyl alcohol 50ml, flooded 2 hours, and jolting constantly; Filter, filtrating is put evaporate to dryness in the water-bath, and residue adds water 10ml makes dissolving, adds hydrochloric acid 1ml again; Put in the water-bath and heated 30 minutes, cooling divides 2 extractions with chloroform 20ml immediately; Combined chloroform liquid is concentrated into about 1ml, as need testing solution; Other gets the archen reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to thin-layered chromatography; Draw above-mentioned two kinds of solution, 10 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with the upper solution of sherwood oil (60～90 ℃)-ethyl formate-formic acid (15: 5: 1); Launch; Take out, dry, it is stifling clear to the spot colour developing to put in the ammonia steam.In the test sample chromatogram, with control medicinal material chromatogram relevant position on, show identical punctation;
(2) get these article 5g, add 30ml methyl alcohol dipping 1 hour, jolting constantly filters evaporate to dryness; Residue is dissolved in water, and transferring pH with watery hydrochloric acid again is 1-2, extracts 2 times with the ethyl acetate jolting, and each 15ml merges ethyl acetate liquid, evaporate to dryness; With the 1ml dissolve with methanol as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and processes the solution that every 1ml contains 2mg, as reference substance solution; According to the thin-layered chromatography test, get each 2 μ l of above-mentioned two kinds of solution and put respectively on same silica gel g thin-layer plate, (10: 7: 1: 1) be developping agent, launch that taking-up is dried, spray was with 2% ferric trichloride ethanolic solution with ethyl acetate-butanone-formic acid-water.In the test sample chromatogram, with reference substance chromatogram relevant position on show the spot of same color;
(3) get these article 8g, add methyl alcohol 50ml, flooded 2 hours, and jolting constantly, filtering, filtrating is put and is concentrated into about 1ml in the water-bath, as need testing solution; Other gets the Berberine hydrochloride reference substance and adds methyl alcohol and process the solution that every 1ml contains 0.5mg, as reference substance solution; According to thin-layered chromatography test, draw each 1 μ l of above-mentioned two kinds of solution, put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is a binder; (10: 6: 1: 1) be developping agent, expansion was taken out with ethyl acetate-butanone-formic acid-water; Dry, under ultraviolet lamp (365nm), inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on show identical yellow fluorescence spot;
Assay: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.2mol/L phosphate sodium dihydrogen buffer solution (regulating pH to 2.7 with phosphoric acid) (42: 58) is moving phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the scutelloside peak should be not less than 5000;
The preparation of reference substance solution: precision takes by weighing the scutelloside reference substance 12.5mg that is dried to constant weight at 105 ℃, puts in the 250ml measuring bottle, with the small amount of methanol dissolving, is diluted to scale with double distilled water, shakes up, and promptly gets (containing scutelloside 50 μ g among every 1ml);
The content under these article content uniformity item, mixing, porphyrize are got in the preparation of need testing solution; Get about 0.75g, the accurate title, decide, and puts in the 100ml measuring bottle; Add methyl alcohol 10ml, sonicated 10 minutes is diluted to scale with double distilled water; Got this liquid centrifugal 10 minutes (the per minute rotating speed is 15000 commentaries on classics), obtain supernatant, promptly get;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get; These article contain the root of large-flowered skullcap with scutelloside (C for every bag
21H
18O
11) meter, must not be less than 21mg.
Function cures mainly: the clearing heat-fire detoxifcation.The body heat that is used for due to the fiery malicious blood-head is irritated, hot eyes aphtha, throat, swelling and aching of gum, constipation, and pharyngitis, tonsillitis, gingivitis see above-mentioned symptom person.
Usage and dosage: boiling water is taken after mixing it with water, one time 1 bag, 3～4 times on the one.
Specification: every packed 7.5 grams.
Claims (4)
1. detection method with pharmaceutical composition of clearing heat-fire detoxication is characterized in that this method comprises following discrimination method and content assaying method:
Differentiate:
(1) get said composition granule 6-10g, add methyl alcohol 40-60ml, flooded 1-3 hour, and jolting constantly; Filter, filtrating is put evaporate to dryness in the water-bath, and residue adds water 8-12ml makes dissolving, adds hydrochloric acid 1ml again; Put in the water-bath and heated 25-35 minute, cooling divides 2-3 extraction with chloroform 18-22ml immediately; Combined chloroform liquid is concentrated into about 1ml, as need testing solution; Other gets the archen reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to thin-layered chromatography; Draw above-mentioned two kinds of solution, 10 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be that sherwood oil-ethyl formate-formic acid of 60～90 ℃ is that the upper solution of 13-18: 4-6: 1-2 is a developping agent with boiling range; Launch; Take out, dry, it is stifling clear to the spot colour developing to put in the ammonia steam; In the test sample chromatogram, with control medicinal material chromatogram relevant position on, show identical punctation;
(2) get said composition granule 4-7g, add 28-34ml methyl alcohol dipping 1-2 hour, jolting constantly filters evaporate to dryness; Residue is dissolved in water, and transferring pH with watery hydrochloric acid again is 1-2, extracts 2-3 time with the ethyl acetate jolting, and each 14-16ml merges ethyl acetate liquid, evaporate to dryness; With the 1ml dissolve with methanol as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and processes the solution that every 1ml contains 2mg, as reference substance solution; According to thin-layered chromatography test, get each 2 μ l of above-mentioned two kinds of solution and put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water be 8-12: 6-9: 1-2: 1-2 as developping agent, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, with reference substance chromatogram relevant position on show the spot of same color;
(3) get said composition granule 7-9g, add methyl alcohol 45-55ml, flooded 1-3 hour, and jolting constantly, filtering, filtrating is put and is concentrated into about 1ml in the water-bath, as need testing solution; Other gets the Berberine hydrochloride reference substance and adds methyl alcohol and process the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to thin-layered chromatography; Draw each 1 μ l of above-mentioned two kinds of solution, put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is a binder, be 9-12: 5-7: 1-2 with ethyl acetate-butanone-formic acid-water: 1-2 is as developping agent; Launch; Take out, dry, under the 365nm ultraviolet lamp, inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on show identical yellow fluorescence spot;
Assay:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-use the 0.2mol/L phosphate sodium dihydrogen buffer solution of phosphoric acid adjusting pH to 2.7 to be 40-44: 55-65 is as moving phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the scutelloside peak should be not less than 5000;
The preparation of reference substance solution: precision takes by weighing the scutelloside reference substance 12.5mg that is dried to constant weight at 105 ℃, puts in the 250ml measuring bottle, with the small amount of methanol dissolving, is diluted to scale with double distilled water, shakes up, and promptly gets, and contains scutelloside 50 μ g among every 1ml;
The preparation of need testing solution: get the content under the said composition granule content uniformity item, mixing, porphyrize is got about 0.75g; The accurate title, decide, and puts in the 100ml measuring bottle, adds methyl alcohol 10ml; Sonicated 8-12 minute, be diluted to scale with double distilled water, got the centrifugal 8-12 of this liquid minute; The per minute rotating speed is that 13000-18000 changes, and obtains supernatant, promptly gets;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get;
Wherein, the bulk drug of this pharmaceutical composition consists of:
Coptis 100-150 weight portion rheum officinale 600-700 weight portion root of large-flowered skullcap 150-250 weight portion
Root bark of tree peony 100-150 weight portion golden cypress 100-150 weight portion.
2. the detection method of pharmaceutical composition as claimed in claim 1 is characterized in that this method comprises:
Differentiate:
(1) get these article 8g, add methyl alcohol 50ml, flooded 2 hours, and jolting constantly; Filter, filtrating is put evaporate to dryness in the water-bath, and residue adds water 10ml makes dissolving, adds hydrochloric acid 1ml again; Put in the water-bath and heated 30 minutes, cooling divides 2 extractions with chloroform 20ml immediately; Combined chloroform liquid is concentrated into about 1ml, as need testing solution; Other gets the archen reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to thin-layered chromatography; Draw above-mentioned two kinds of solution, 10 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be that 60～90 ℃ of sherwood oil-ethyl formate-formic acid are that 15: 5: 1 upper solution is a developping agent with boiling range; Launch; Take out, dry, it is stifling clear to the spot colour developing to put in the ammonia steam; In the test sample chromatogram, with control medicinal material chromatogram relevant position on, show identical punctation;
(2) get these article 5g, add 30ml methyl alcohol dipping 1 hour, jolting constantly filters evaporate to dryness; Residue is dissolved in water, and transferring pH with watery hydrochloric acid again is 1-2, extracts 2 times with the ethyl acetate jolting, and each 15ml merges ethyl acetate liquid, evaporate to dryness; With the 1ml dissolve with methanol as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and processes the solution that every 1ml contains 2mg, as reference substance solution; According to the thin-layered chromatography test, get each 2 μ l of above-mentioned two kinds of solution and put respectively on same silica gel g thin-layer plate, be 10: 7: 1 with ethyl acetate-butanone-formic acid-water: 1 as developping agent, launches, and takes out, and dries, and spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, with reference substance chromatogram relevant position on show the spot of same color;
(3) get these article 8g, add methyl alcohol 50ml, flooded 2 hours, and jolting constantly, filtering, filtrating is put and is concentrated into about 1ml in the water-bath, as need testing solution; Other gets the Berberine hydrochloride reference substance and adds methyl alcohol and process the solution that every 1ml contains 0.5mg, as reference substance solution; According to thin-layered chromatography test, draw each 1 μ l of above-mentioned two kinds of solution, put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is a binder; With ethyl acetate-butanone-formic acid-water is 10: 6: 1: 1 as developping agent, launches, and takes out; Dry, under the 365nm ultraviolet lamp, inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on show identical yellow fluorescence spot;
Assay:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; The 0.2mol/L phosphate sodium dihydrogen buffer solution that methyl alcohol-use phosphoric acid is regulated pH to 2.7 be 42: 58 as moving phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the scutelloside peak should be not less than 5000;
The preparation of reference substance solution: precision takes by weighing the scutelloside reference substance 12.5mg that is dried to constant weight at 105 ℃, puts in the 250ml measuring bottle, with the small amount of methanol dissolving, is diluted to scale with double distilled water, shakes up, and promptly gets;
The preparation of need testing solution: get the content under these article content uniformity item, mixing, porphyrize is got about 0.75g; The accurate title, decide, and puts in the 100ml measuring bottle, adds methyl alcohol 10ml; Sonicated 10 minutes is diluted to scale with double distilled water, gets this liquid centrifugal 10 minutes; The per minute rotating speed is 15000 commentaries on classics, obtains supernatant, promptly gets;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get.
3. according to claim 1 or claim 2 method is characterized in that the bulk drug of said pharmaceutical composition consists of:
The coptis 140 weight portion rheum officinales 650 weight portion roots of large-flowered skullcap 200 weight portions
The root bark of tree peony 130 weight portion golden cypresses 140 weight portions.
4. detection method with pharmaceutical composition of clearing heat-fire detoxication is characterized in that this method comprises following discrimination method and content assaying method:
Differentiate:
(1) get said composition granule 6-10g, add methyl alcohol 40-60ml, flooded 1-3 hour, and jolting constantly; Filter, filtrating is put evaporate to dryness in the water-bath, and residue adds water 8-12ml makes dissolving, adds hydrochloric acid 1ml again; Put in the water-bath and heated 25-35 minute, cooling divides 2-3 extraction with chloroform 18-22ml immediately; Combined chloroform liquid is concentrated into about 1ml, as need testing solution; Other gets the archen reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to thin-layered chromatography; Draw above-mentioned two kinds of solution, 10 μ l, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be that sherwood oil-ethyl formate-formic acid of 60～90 ℃ is that the upper solution of 13-18: 4-6: 1-2 is a developping agent with boiling range; Launch; Take out, dry, it is stifling clear to the spot colour developing to put in the ammonia steam; In the test sample chromatogram, with control medicinal material chromatogram relevant position on, show identical punctation;
(2) get said composition granule 4-7g, add 28-34ml methyl alcohol dipping 1-2 hour, jolting constantly filters evaporate to dryness; Residue is dissolved in water, and transferring pH with watery hydrochloric acid again is 1-2, extracts 2-3 time with the ethyl acetate jolting, and each 14-16ml merges ethyl acetate liquid, evaporate to dryness; With the 1ml dissolve with methanol as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and processes the solution that every 1ml contains 2mg, as reference substance solution; According to thin-layered chromatography test, get each 2 μ l of above-mentioned two kinds of solution and put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water be 8-12: 6-9: 1-2: 1-2 as developping agent, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, with reference substance chromatogram relevant position on show the spot of same color;
(3) get said composition granule 7-9g, add methyl alcohol 45-55ml, flooded 1-3 hour, and jolting constantly, filtering, filtrating is put and is concentrated into about 1ml in the water-bath, as need testing solution; Other gets the Berberine hydrochloride reference substance and adds methyl alcohol and process the solution that every 1ml contains 0.5mg, as reference substance solution; Test according to thin-layered chromatography; Draw each 1 μ l of above-mentioned two kinds of solution, put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is a binder, be 9-12: 5-7: 1-2 with ethyl acetate-butanone-formic acid-water: 1-2 is as developping agent; Launch; Take out, dry, under the 365nm ultraviolet lamp, inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on show identical yellow fluorescence spot;
Assay:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-use the 0.2mol/L phosphate sodium dihydrogen buffer solution of phosphoric acid adjusting pH to 2.7 to be 40-44: 55-65 is as moving phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the scutelloside peak should be not less than 5000;
The preparation of reference substance solution: precision takes by weighing the scutelloside reference substance 12.5mg that is dried to constant weight at 105 ℃, puts in the 250ml measuring bottle, with the small amount of methanol dissolving, is diluted to scale with double distilled water, shakes up, and promptly gets, and contains scutelloside 50 μ g among every 1ml;
The preparation of need testing solution: get the content under the said composition granule content uniformity item, mixing, porphyrize is got about 0.75g; The accurate title, decide, and puts in the 100ml measuring bottle, adds methyl alcohol 10ml; Sonicated 8-12 minute, be diluted to scale with double distilled water, got the centrifugal 8-12 of this liquid minute; The per minute rotating speed is that 13000-18000 changes, and obtains supernatant, promptly gets;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get;
Wherein, the bulk drug of this pharmaceutical composition consists of:
Coptis 100-150 weight portion rheum officinale 600-700 weight portion root of large-flowered skullcap 150-250 weight portion
Root bark of tree peony 100-150 weight portion golden cypress 100-150 weight portion;
Method for making: rheum officinale boiling 2-3 time adds 6-9 times of water gaging at every turn and decocted 1-2 hour; The coptis, the root of large-flowered skullcap, the root bark of tree peony, golden cypress boiling 2-3 time add 6-9 times of water gaging at every turn and decocted 1-2 hour; Collecting decoction filters, and filtrating is concentrated into and surveys relative density at 65-75 ℃ is 1.25, is spray dried to dry extract; Above-mentioned extract powder is added an amount of sucrose and dextrin, and mixing is processed particle, and drying makes particle 1000 weight portions, promptly gets.
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| CN201010299716A CN101933996B (en) | 2007-03-27 | 2007-03-27 | Chinese medicinal composition having effects of clearing heat, relieving fire and eliminating toxins and preparation and detection methods thereof |
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| CN102707009A (en) * | 2012-06-18 | 2012-10-03 | 天津中新药业集团股份有限公司达仁堂制药厂 | Method for detecting rhizoma coptidis pills for clearing away heat of upper part of body |
| CN102935136A (en) * | 2012-11-28 | 2013-02-20 | 重庆开洲九鼎牧业科技开发有限公司 | Heat-clearing and toxicity-removing composition and feed for livestock as well as preparation method and application thereof |
| CN103127289B (en) * | 2013-03-20 | 2015-05-27 | 呼和浩特市第一医院 | Drug for treatment of eczema skin disease |
| CN104523529A (en) * | 2015-01-08 | 2015-04-22 | 江苏省中医院 | Traditional Chinese medicine wet tissue for skin decontamination, preparation method thereof and traditional Chinese medicine composition |
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