CN101933996A - 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 away 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 away heat-fire Detoxication.
Background technology
In recent years, raising and operating pressure increase along with people's living standard, reasons such as, rhythm of life confusion rich owing to surfeit, 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, 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 dispelling exopathogens from superficies of the body, releasing table disease of Chinese medicine are main treatment, and exopathogen is separated from antiperspirant, are equipped with heat-clearing and toxic substances removing such as eliminating fire and detoxication, removing heat from the lung and relieving sorethroat, and the medicine of reconciling superficies and interior makes above-mentioned symptom be alleviated and cure.Therefore the patient uses saferly during this symptom of treatment by Chinese herbs, is difficult for producing drug resistance, can also strengthen the human body prevention ability of pathogenic factor to external world.
Medicine of the present invention as go heat clearing away, reduce internal heat, the representative medicine of antidote, have clinical application effect preferably.Be used for the fever of the body agitation due to the fire-toxin heat in blood, the conjunctival congestion aphtha, throat, gingival swelling and pain, constipation, and pharyngitis, tonsillitis, gingivitis sees 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 away heat-fire Detoxication;
The object of the invention also is to provide a kind of Chinese medicine composition preparation method with clearing away 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 away heat-fire Detoxication.
The present invention seeks to be achieved through the following technical solutions:
Chinese medicine composition with clearing away heat-fire Detoxication of the present invention is to be made by the crude drug of following weight ratio:
Rhizoma Coptidis 100-300 weight portion Radix Et Rhizoma Rhei 400-700 weight portion Radix Scutellariae 150-380 weight portion
The above-mentioned raw materials optimum ratio is:
Rhizoma Coptidis 100-150 weight portion Radix Et Rhizoma Rhei 600-700 weight portion Radix Scutellariae 150-250 weight portion
Chinese medicine composition with clearing away heat-fire Detoxication of the present invention can be made by the crude drug of following weight ratio:
Rhizoma Coptidis 100-300 weight portion Radix Et Rhizoma Rhei 400-700 weight portion Radix Scutellariae 150-380 weight portion Cortex Moutan 100-200 Cortex Phellodendri 100-200
The above-mentioned raw materials optimum ratio is:
Rhizoma Coptidis 100-150 weight portion Radix Et Rhizoma Rhei 600-700 weight portion Radix Scutellariae 150-250 weight portion Cortex Moutan 100-150 weight portion Cortex Phellodendri 100-150 weight portion
The above-mentioned raw materials optimum ratio is:
Rhizoma Coptidis 140 weight portion Radix Et Rhizoma Rhei 650 weight portion Radix Scutellariaes 200 weight portions
Cortex Moutan 130 weight portion Cortex Phellodendris 140 weight portions
Compositions of the present invention technology adding adjuvant is routinely made clinical acceptable forms such as tablet, capsule, oral liquid, drop pill, spray, granule; Described adjuvant comprises solvent, disintegrating agent, correctives, antiseptic, coloring agent, binding agent, lubricant, substrate etc.
The preparation method of Chinese medicine composition granular preparation of the present invention is:
Choose crude drug: Rhizoma Coptidis 100-300 weight portion Radix Et Rhizoma Rhei 400-700 weight portion Radix Scutellariae 150-380 weight portion
Method for making: above three flavors, decoct with water 2-3 time respectively, add 6-9 times of water gaging at every turn and decocted 1-2 hour, collecting decoction filters, and filtrate 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 made granule, and drying makes granule 1000 weight portions, promptly.
The preparation method of Chinese medicine composition granular preparation of the present invention is:
Choose crude drug:
Rhizoma Coptidis 100-300 weight portion Radix Et Rhizoma Rhei 400-700 weight portion Radix Scutellariae 150-380 weight portion Cortex Moutan 100-200 weight portion Cortex Phellodendri 100-200 weight portion;
Method for making: Radix Et Rhizoma Rhei decocts with water 2-3 time, adds 6-9 times of water gaging at every turn and decocts 1-2 hour; Rhizoma Coptidis, Radix Scutellariae, Cortex Moutan, Cortex Phellodendri decoct with water 2-3 time, add 6-9 times of water gaging at every turn and decoct 1-2 hour; Collecting decoction filters, and filtrate 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 made granule, and drying makes granule 1000 weight portions, promptly.
Pharmaceutical composition method of quality control of the present invention comprises one or more in following discrimination method and/or the assay:
Differentiate:
(1) gets present composition granule 6-10g, add methanol 40-60ml, flooded 1-3 hour, and jolting constantly, filtering, filtrate is put evaporate to dryness in the water-bath, residue adds water 8-12ml makes dissolving, add hydrochloric acid 1ml again, put in the water-bath and heated 25-35 minute, immediately cooling, divide 2-3 extraction with chloroform 18-22ml, combined chloroform liquid is concentrated into about 1ml, as need testing solution; Other gets the emodin reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer 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 adhesive with the sodium carboxymethyl cellulose, (13-18: 4-6: upper solution 1-2) is developing solvent with petroleum ether (60～90 ℃)-Ethyl formate-formic acid, launch, take out, dry, it is stifling clear to the speckle colour developing to put in the ammonia steam; In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show identical punctation;
(2) get present composition granule 4-7g, add 28-34ml methanol dipping 1-2 hour, jolting constantly filters evaporate to dryness; Residue is dissolved in water, and transferring pH with dilute 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 baicalin reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to the thin layer 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 developing solvent, launch, take out that dry, spray is with 2% ferric chloride alcoholic solution; In the test sample chromatograph, with reference substance chromatograph relevant position on show the speckle of same color;
(3) get present composition granule 7-9g, add methanol 45-55ml, flooded 1-3 hour, and jolting constantly, filtering, filtrate 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 methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer 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 an adhesive, with ethyl acetate-butanone-formic acid-water (9-12: 5-7: 1-2: 1-2) be developing solvent, launch, take out, dry, under ultra-violet lamp (365nm), inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on show identical yellow fluorescence speckle;
Assay:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-0.2mol/L phosphate sodium dihydrogen buffer solution (regulating pH to 2.7) (40-44: 55-65) be mobile phase with phosphoric acid; The detection wavelength is 275nm; Number of theoretical plate calculates by the baicalin peak should be not less than 5000;
The preparation of reference substance solution: precision takes by weighing the baicalin 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 baicalin 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 is got about 0.75g, the accurate title, decide, put in the 100ml measuring bottle, add methanol 10ml, supersound process 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), divide and get supernatant, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Pharmaceutical composition method of quality control of the present invention is preferably as follows one or more in discrimination method and/or the assay:
Differentiate:
(1) gets this product 8g, add methanol 50ml, flooded 2 hours, and jolting constantly, filtering, filtrate is put evaporate to dryness in the water-bath, residue adds water 10ml makes dissolving, add hydrochloric acid 1ml again, put in the water-bath and heated 30 minutes, immediately cooling, divide 2 extractions with chloroform 20ml, combined chloroform liquid is concentrated into about 1ml, as need testing solution; Other gets the emodin reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer 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 adhesive with the sodium carboxymethyl cellulose, upper solution with petroleum ether (60～90 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, it is stifling clear to the speckle colour developing to put in the ammonia steam; In the test sample chromatograph, with reference substance chromatograph relevant position on, show identical punctation;
(2) get this product 5g, add 30ml methanol dipping 1 hour, jolting constantly filters evaporate to dryness; Residue is dissolved in water, and transferring pH with dilute 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 baicalin reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to the thin layer 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 developing solvent, launch that taking-up is dried, spray was with 2% ferric chloride alcoholic solution with ethyl acetate-butanone-formic acid-water; In the test sample chromatograph, with reference substance chromatograph relevant position on show the speckle of same color;
(3) get this product 8g, add methanol 50ml, flooded 2 hours, and jolting constantly, filtering, filtrate 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 methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer 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 an adhesive, (10: 6: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, under ultra-violet lamp (365nm), inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on show identical yellow fluorescence speckle;
Assay:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-0.2mol/L phosphate sodium dihydrogen buffer solution (regulating pH to 2.7 with phosphoric acid) (42: 58) is mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the baicalin peak should be not less than 5000; The preparation of reference substance solution: precision takes by weighing the baicalin 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 baicalin 50 μ g among every 1ml);
The preparation of need testing solution: get the content under this product content uniformity item, mixing, porphyrize is got about 0.75g, the accurate title, decide, put in the 100ml measuring bottle, add methanol 10ml, supersound process 10 minutes, be diluted to scale with double distilled water, got this liquid centrifugal 10 minutes (the per minute rotating speed is 15000 commentaries on classics), divide and get supernatant, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly; This product contains Radix Scutellariae with baicalin (C for every bag
21H
18O
11) meter, must not be less than 21mg.
The present composition has good clearing away heat-fire Detoxication, compares SHUANGHUANGLIAN KOUFUYE and shows good drug effect.To the fever of the body agitation due to the fire-toxin heat in blood, the conjunctival congestion aphtha, throat, gingival swelling and pain, constipation, and pharyngitis, tonsillitis, gingivitis has good effect.
The method of quality control of Chinese medicine composition provided by the present invention, be by obtaining behind the creative experiment sieving of big measuring, pass through screening in the discrimination method to sample treatment, the selection of developing solvent, make and differentiate that specificity is fine, and method is economic and practical, the result is quick, and can both use different lamellaes.Pass through screening in the content assaying method to sample, test sample processing method, the selection of developing solvent, 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 away 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.The same day, measure the preceding basal body temperature of modeling, oneself rabbit ear vein bacterial injection endotoxin normal saline solution, dosage is 1ml.kg-1 (10ml), observation body temperature changes, per 0.5 hour record once, choose injection 1h after body temperature rise surpass 0.5 ℃ rabbit, be divided into 5 groups at random, 8 every group: the large, medium and small dosage group 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 record 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, and the results are shown in following table:
The influence of the fever in rabbit body temperature that bacterial endotoxin is caused
Annotate: compare * P＜0.05, * * P＜0.01 with matched group
The result shows: 1 group, 2 groups high, medium and low dosage of medicine of the present invention all have obvious inhibitory action to fever in rabbits due to the bacterial endotoxin, relatively have significant difference with the blank group, and 2 groups of same doses of medicine of the present invention are better than 1 group of medicine of the present invention.
2, Detoxication:
Experiment was surveyed body temperature 3 in advance with rat, experiment measured value on the same day is the rat basal body temperature, 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% carrageenin 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 inhibitory action of on Carrageenan solution mice 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 antibacterial antidotal effect.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 better than 1 group of medicine of the present invention.
Experimental example 2 is differentiated screening experiment
1, thin layer to Radix Et Rhizoma Rhei is differentiated in the pharmaceutical preparation of the present invention
(1) thin layer of Radix Et Rhizoma Rhei is differentiated the preferred of developing solvent 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 adhesive with the sodium carboxymethyl cellulose, petroleum ether 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 developing solvent, launch, take out, dry, it is stifling clear to the speckle colour developing to put in the ammonia steam.Observe the unfolded effect of test sample principal spot on the lamellae, the results are shown in following table:
Developing solvent proportion optimization experimental result table in the discrimination method of Radix Et Rhizoma Rhei
Developing solvent proportioning as can be seen from the above table is 15: 5: 1 o'clock, launches effectively on lamellae, and principal spot is clear, does not have hangover, and is identical with the speckle displacement and the color of reference substance, is fit to test requirements document.
(2) sample solution point sample amount preferred in the above-mentioned Radix Et Rhizoma Rhei 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 developing solvent, launch, take out, dry, it is stifling clear to the speckle colour developing to put in the ammonia steam, and the effect of observing test sample principal spot colour developing on the lamellae the results are shown in following table:
Sample solution point sample amount optimization experiment table as a result in the discrimination method of Radix Et Rhizoma Rhei
Test sample point sample amount is when 10 μ l as can be seen from the above table, and color developing effect is good on lamellae, is fit to test requirements document.
(3) negative control test
Get the negative sample that lacks Radix Et Rhizoma Rhei, prepare negative control solution, launch the back and corresponding speckle on the reference substance solution correspondence position, do not occur, illustrate that selected identification experiment specificity is strong according to need testing solution preparation method in the discrimination method of above-mentioned Radix Et Rhizoma Rhei.
2, thin layer to Radix Scutellariae is differentiated in the pharmaceutical preparation of the present invention
(1) developing solvent preferred in the above-mentioned Radix Scutellariae discrimination method:
1. draw need testing solution, each 2 μ l of 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: acetic acid: water is developing solvent, launch, take out, dry, spray is with 2% ferric chloride alcoholic solution, observe the effect of test sample principal spot colour developing on the lamellae, the results are shown in following table:
Developing solvent optimization experiment table as a result in the Radix Scutellariae 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 developing solvent launches, and observes the unfolded effect of test sample principal spot on the lamellae, the results are shown in following table:
The optimization experiment of developing solvent proportioning is table as a result
From 1. above and 2. result of the test as can be seen, select ethyl acetate: butanone: formic acid: water is 10: 7: 1: 1 developing solvent, 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 above-mentioned Radix Scutellariae:
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 developing solvent, launch, take out, dry, spray is with 2% ferric chloride alcoholic solution, in the test sample chromatograph, with reference substance chromatograph relevant position on show the speckle of same color, the effect of observing test sample principal spot colour developing on the lamellae the results are shown in following table:
Sample solution point sample amount optimization experiment table as a result in the discrimination method of Radix Scutellariae
Test sample point sample amount is when 2 μ l as can be seen from the above table, and color developing effect is good on lamellae, is fit to test requirements document.
(3) negative control test
Get the negative sample that lacks Radix Scutellariae, prepare negative control solution, launch the back and corresponding speckle on the reference substance solution correspondence position, do not occur, illustrate that selected identification experiment specificity is strong according to need testing solution preparation method in the above-mentioned Radix Scutellariae discrimination method.
3, thin layer to Rhizoma Coptidis is differentiated in the pharmaceutical preparation of the present invention
(1) developing solvent proportioning preferred in the above-mentioned Rhizoma Coptidis 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 developing solvent, observe the unfolded effect of test sample principal spot on the lamellae, the results are shown in following table:
Developing solvent proportion optimization experimental result in the Rhizoma Coptidis discrimination method
As can be seen from the above table, be 10: 6: 1 with ethyl acetate-butanone-formic acid-water proportioning: 1 o'clock, launch effect, separating effect is all better.
(2) sample solution point sample amount preferred in the above-mentioned Rhizoma Coptidis discrimination method:
Get need testing solution 0.5 μ l, 1.0 μ l, 1.5 μ l, 2 μ l, point sample is on the silica gel G plate respectively, with ethyl acetate-butanone-formic acid-water proportioning is 10: 6: 1: 1 developing solvent, launch, taking out, dry, is to inspect under the 365nm in the ultra-violet lamp wavelength, observe the effect of test sample principal spot colour developing on the lamellae, the results are shown in following table:
Sample solution point sample amount optimization experiment result in the discrimination method of Rhizoma Coptidis
Test sample point sample amount is when 1.0 μ l as can be seen from the above table, and color developing effect is good on lamellae, is fit to test requirements document.
(3) negative control test
Get the negative sample that lacks Rhizoma Coptidis, prepare negative control solution, launch the back and corresponding speckle on the reference substance solution correspondence position, do not occur, illustrate that selected identification experiment specificity is strong according to need testing solution preparation method in the above-mentioned Rhizoma Coptidis discrimination method.
The experiment of experimental example 3 assays
Adopt the content of baicalin in the high-efficient liquid phase color popularize law mensuration medicine of the present invention, to improve quality determining method of the present invention:
(1) mobile phase reagent is preferred:
Be that 15: 85 solution, 0.05mol/L methanol and potassium dihydrogen phosphate ratio is 40: 65 solution, 0.2mol/L methanol with acetonitrile and water ratio respectively: phosphate sodium dihydrogen buffer solution is that 42: 58 solution is mobile phase, carry out the test sample assay at molten night, by comparing among the general figure of high-efficient liquid phase color, the separating effect at each peak, determine preferred mobile phase, the results are shown in Table following table:
The optimization experiment result of mobile phase reagent
As can be seen from the above table, mobile phase is selected 0.2mol/L methanol: 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 methanol: the phosphate sodium dihydrogen buffer solution proportioning is that (30: 80), (40: 70), (42: 60), (42: 58) are mobile phase, carry out the test sample assay at molten night, by comparing among the general figure of high-efficient liquid phase color, the separating effect at each peak, determine preferred mobile phase, the results are shown in following table:
The optimization experiment result of proportion of mobile phase
As can be seen from the above 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)
Mobile phase: methanol-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: baicalin is purchased lot number: the 0715-9909 in Nat'l Pharmaceutical ﹠ Biological Products Control Institute
Assay method: the preparation method of getting by need testing solution under [assay] item prepares sample liquid; And by preparing the blank sample that lacks Radix Scutellariae under [method for making] item, the preparation negative controls.With microporous filter membrane (0.45 μ m).The accurate respectively negative controls of drawing, each 10 μ l of reference substance liquid and need testing solution inject chromatograph of liquid, measure, promptly.
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, the results are shown in following table:
(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 results are shown in following table, and drawing standard curve, show that baicalin 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 results are shown in following table:
(4) the text method is pressed in the repeatability test, gets same lot number sample and measures, and tries to achieve relative standard deviation＜2%, the results are shown in following table:
(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 baicalin reference substance solution (0.133mg/ml), press the preparation method operation of text need testing solution, measure its content, and calculate its response rate, measurement result sees the following form:
By above methodology examination result as can be seen, its linear relationship of the content assaying method that medicine of the present invention adopted, stability, precision, repeatability etc. are all good, can effectively control drug quality of the present invention.
From the result of study of above quality determining method as can be seen, the quality determining method science that pharmaceutical preparation of the present invention is 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
The specific embodiment
Embodiment 1: granule
Rhizoma Coptidis 140g Radix Et Rhizoma Rhei 650g Radix Scutellariae 200g Cortex Moutan 130g Cortex Phellodendri 140g
Radix Et Rhizoma Rhei decocts with water 2 times, adds 8 times of water gagings at every turn and decocts 1 hour; Rhizoma Coptidis, Radix Scutellariae, Cortex Moutan, Cortex Phellodendri decoct with water 2 times, add 7 times of water gagings at every turn and decoct 1 hour; Collecting decoction filters, and filtrate 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 made granule, and drying makes granule 1000g, promptly.
Embodiment 2: drop pill
Rhizoma Coptidis 176g Radix Et Rhizoma Rhei 533.3g Radix Scutellariae 266.7g
Method for making: above three flavors, decoct with water secondary respectively, 1.5 hours for the first time, the 21 hour, collecting decoction, filter, filtrate is concentrated into 70 ℃ of relative densities and is about 1.25, adds in Macrogol 4000 and the blended substrate of polyethylene glycol 6000, splashes in the liquid paraffin with certain speed, the drop ball, promptly.
Embodiment 3: effervescent
Rhizoma Coptidis 150g Radix Et Rhizoma Rhei 550g Radix Scutellariae 300g Cortex Moutan 140g Cortex Phellodendri 150g
Method for making: the above five tastes, decoct with water secondary respectively, 1.5 hours for the first time, the 21 hour, collecting decoction filtered, and filtrate is concentrated into 70 ℃ of relative densities and is about 1.25 thick paste; After the Polyethylene Glycol dissolving, behind the adding sodium bicarbonate, be sprayed in the thick paste, with sweetener and acidic flavoring agent tabletting, promptly.
Embodiment 4:
Rhizoma Coptidis 136g Radix Et Rhizoma Rhei 673.3g Radix Scutellariae 246.7g
This pharmaceutical composition adds conventional adjuvant, makes capsule by common process.
Embodiment 5:
Rhizoma Coptidis 146g Radix Et Rhizoma Rhei 653.3g Radix Scutellariae 236.7g
This pharmaceutical composition adds conventional adjuvant, makes tablet by common process.
Embodiment 6:
Rhizoma Coptidis 150g Radix Et Rhizoma Rhei 550g Radix Scutellariae 300g Cortex Phellodendri 150g
This pharmaceutical composition adds conventional adjuvant, makes capsule by common process.
Embodiment 7:
Rhizoma Coptidis 176g Radix Et Rhizoma Rhei 533.3g Radix Scutellariae 266.7g
Method for making: above three flavors, decoct with water secondary respectively, add 8 times of water gagings for the first time and decocted 1.5 hours, second adds 6 times of water gagings decocted 1 hour, and collecting decoction filters, and filtrate 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 made granule, and drying makes granule 1000g, promptly;
Differentiate:
(1) gets this product 8g, add methanol 50ml, flooded 2 hours, and jolting constantly, filtering, filtrate is put evaporate to dryness in the water-bath, residue adds water 10ml makes dissolving, add hydrochloric acid 1ml again, put in the water-bath and heated 30 minutes, immediately cooling, divide 2 extractions with chloroform 20ml, combined chloroform liquid is concentrated into about 1ml, as need testing solution; Other gets the emodin reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer 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 adhesive with the sodium carboxymethyl cellulose, upper solution with petroleum ether (60～90 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, it is stifling clear to the speckle colour developing to put in the ammonia steam.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show identical punctation;
(2) get this product 5g, add 30ml methanol dipping 1 hour, jolting constantly filters evaporate to dryness; Residue is dissolved in water, and transferring pH with dilute 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 baicalin reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to the thin layer 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 developing solvent, launch that taking-up is dried, spray was with 2% ferric chloride alcoholic solution with ethyl acetate-butanone-formic acid-water.In the test sample chromatograph, with reference substance chromatograph relevant position on show the speckle of same color;
(3) get this product 8g, add methanol 50ml, flooded 2 hours, and jolting constantly, filtering, filtrate 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 methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer 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 an adhesive, (10: 6: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, under ultra-violet lamp (365nm), inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on show identical yellow fluorescence speckle;
Assay: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-0.2mol/L phosphate sodium dihydrogen buffer solution (regulating pH to 2.7 with phosphoric acid) (42: 58) is mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the baicalin peak should be not less than 5000;
The preparation of reference substance solution: precision takes by weighing the baicalin 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 baicalin 50 μ g among every 1ml);
The content under this product content uniformity item is got in the preparation of need testing solution, mixing, porphyrize is got about 0.75g, the accurate title, decide, put in the 100ml measuring bottle, add methanol 10ml, supersound process 10 minutes, be diluted to scale with double distilled water, got this liquid centrifugal 10 minutes (the per minute rotating speed is 15000 commentaries on classics), divide and get supernatant, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly; This product contains Radix Scutellariae with baicalin (C for every bag
21H
18O
11) meter, must not be less than 21mg.
Function cures mainly: the clearing away heat-fire detoxifcation.Be used for the fever of the body agitation due to the fire-toxin heat in blood, conjunctival congestion aphtha, throat, gingival swelling and pain, constipation, and pharyngitis, tonsillitis, gingivitis sees above-mentioned symptom person.
Usage and dosage: boiled 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 (6)
1. pharmaceutical composition with clearing away heat-fire Detoxication is characterized in that the crude drug of this pharmaceutical composition consists of:
Rhizoma Coptidis 100-300 weight portion Radix Et Rhizoma Rhei 400-700 weight portion Radix Scutellariae 150-380 weight portion Cortex Moutan 100-200 Cortex Phellodendri 100-200.
2. pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug of this pharmaceutical composition consists of:
Rhizoma Coptidis 100-150 weight portion Radix Et Rhizoma Rhei 600-700 weight portion Radix Scutellariae 150-250 weight portion Cortex Moutan 100-150 weight portion Cortex Phellodendri 100-150 weight portion.
3. pharmaceutical composition as claimed in claim 2 is characterized in that the crude drug of this pharmaceutical composition consists of:
Rhizoma Coptidis 140 weight portion Radix Et Rhizoma Rhei 650 weight portion Radix Scutellariaes 200 weight portions
Cortex Moutan 130 weight portion Cortex Phellodendris 140 weight portions.
4. preparation of drug combination method as claimed in claim 1 is characterized in that this method is: choose crude drug:
Rhizoma Coptidis 100-300 weight portion Radix Et Rhizoma Rhei 400-700 weight portion Radix Scutellariae 150-380 weight portion
Cortex Moutan 100-200 weight portion Cortex Phellodendri 100-200 weight portion;
Method for making: Radix Et Rhizoma Rhei decocts with water 2-3 time, adds 6-9 times of water gaging at every turn and decocts 1-2 hour; Rhizoma Coptidis, Radix Scutellariae, Cortex Moutan, Cortex Phellodendri decoct with water 2-3 time, add 6-9 times of water gaging at every turn and decoct 1-2 hour; Collecting decoction filters, and filtrate 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 made granule, and drying makes granule 1000 weight portions, promptly.
5. as the detection method of the arbitrary described pharmaceutical composition of claim 1-3, it is characterized in that this method comprises one or more in following discrimination method and/or the assay:
Differentiate:
(1) gets present composition granule 6-10g, add methanol 40-60ml, flooded 1-3 hour, and jolting constantly, filtering, filtrate is put evaporate to dryness in the water-bath, residue adds water 8-12ml makes dissolving, add hydrochloric acid 1ml again, put in the water-bath and heated 25-35 minute, immediately cooling, divide 2-3 extraction with chloroform 18-22ml, combined chloroform liquid is concentrated into about 1ml, as need testing solution; Other gets the emodin reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer 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 adhesive with the sodium carboxymethyl cellulose, (13-18: 4-6: upper solution 1-2) is developing solvent with petroleum ether (60～90 ℃)-Ethyl formate-formic acid, launch, take out, dry, it is stifling clear to the speckle colour developing to put in the ammonia steam; In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show identical punctation;
(2) get present composition granule 4-7g, add 28-34ml methanol dipping 1-2 hour, jolting constantly filters evaporate to dryness; Residue is dissolved in water, and transferring pH with dilute 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 baicalin reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to the thin layer 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 developing solvent, launch, take out that dry, spray is with 2% ferric chloride alcoholic solution; In the test sample chromatograph, with reference substance chromatograph relevant position on show the speckle of same color;
(3) get present composition granule 7-9g, add methanol 45-55ml, flooded 1-3 hour, and jolting constantly, filtering, filtrate 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 methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer 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 an adhesive, with ethyl acetate-butanone-formic acid-water (9-12: 5-7: 1-2: 1-2) be developing solvent, launch, take out, dry, under ultra-violet lamp (365nm), inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on show identical yellow fluorescence speckle;
Assay:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-0.2mol/L phosphate sodium dihydrogen buffer solution (regulating pH to 2.7) (40-44: 55-65) be mobile phase with phosphoric acid; The detection wavelength is 275nm; Number of theoretical plate calculates by the baicalin peak should be not less than 5000;
The preparation of reference substance solution: precision takes by weighing the baicalin 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 baicalin 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 is got about 0.75g, the accurate title, decide, put in the 100ml measuring bottle, add methanol 10ml, supersound process 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), divide and get supernatant, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
6. the detection method of pharmaceutical composition as claimed in claim 5 is characterized in that this method comprises one or more in following discrimination method and/or the assay:
Differentiate:
(1) gets this product 8g, add methanol 50ml, flooded 2 hours, and jolting constantly, filtering, filtrate is put evaporate to dryness in the water-bath, residue adds water 10ml makes dissolving, add hydrochloric acid 1ml again, put in the water-bath and heated 30 minutes, immediately cooling, divide 2 extractions with chloroform 20ml, combined chloroform liquid is concentrated into about 1ml, as need testing solution; Other gets the emodin reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer 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 adhesive with the sodium carboxymethyl cellulose, upper solution with petroleum ether (60～90 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, launch, take out, dry, it is stifling clear to the speckle colour developing to put in the ammonia steam; In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show identical punctation;
(2) get this product 5g, add 30ml methanol dipping 1 hour, jolting constantly filters evaporate to dryness; Residue is dissolved in water, and transferring pH with dilute 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 baicalin reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to the thin layer 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 developing solvent, launch that taking-up is dried, spray was with 2% ferric chloride alcoholic solution with ethyl acetate-butanone-formic acid-water; In the test sample chromatograph, with reference substance chromatograph relevant position on show the speckle of same color;
(3) get this product 8g, add methanol 50ml, flooded 2 hours, and jolting constantly, filtering, filtrate 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 methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer 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 an adhesive, (10: 6: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, under ultra-violet lamp (365nm), inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on show identical yellow fluorescence speckle;
Assay:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-0.2mol/L phosphate sodium dihydrogen buffer solution (regulating pH to 2.7 with phosphoric acid) (42: 58) is mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the baicalin peak should be not less than 5000;
The preparation of reference substance solution: precision takes by weighing the baicalin 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, promptly;
The preparation of need testing solution: get the content under this product content uniformity item, mixing, porphyrize is got about 0.75g, the accurate title, decide, put in the 100ml measuring bottle, add methanol 10ml, supersound process 10 minutes, be diluted to scale with double distilled water, got this liquid centrifugal 10 minutes (the per minute rotating speed is 15000 commentaries on classics), divide and get supernatant, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
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| CN2007100647971A Division CN101274025B (en) | 2007-03-27 | 2007-03-27 | Quality control method of Chinese medicinal composition with functions of reducing fever, purging the intense heat and detoxification |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103127289A (en) * | 2013-03-20 | 2013-06-05 | 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 |
| CN116008461A (en) * | 2022-12-27 | 2023-04-25 | 天津现代创新中药科技有限公司 | Method for detecting traditional Chinese medicine ointment with multiple evaluation on one test |
-
2007
- 2007-03-27 CN CN201010299716A patent/CN101933996B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103127289A (en) * | 2013-03-20 | 2013-06-05 | 呼和浩特市第一医院 | Drug for treatment of eczema skin disease |
| 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 |
| CN116008461A (en) * | 2022-12-27 | 2023-04-25 | 天津现代创新中药科技有限公司 | Method for detecting traditional Chinese medicine ointment with multiple evaluation on one test |
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|---|---|
| CN101933996B (en) | 2012-10-03 |
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