CN102151322A - Chinese medicine composition for treating cold in children, preparation method and detection method thereof - Google Patents

Abstract

The invention discloses a Chinese medicine composition for treating cold in children, a preparation method and a detection method thereof, belonging to the technical field of traditional Chinese medicines. The Chinese medicine composition is prepared from Chinese medicinal herbs such as musk, bezoar, pearl and the like, and is respectively prepared into pharmaceutically allowable dosage forms. The Chinese medicine composition has good stability and high bioavailability, is convenient for taking, is attractive and clean in appearance, and is easy to accept by patients. The preparation method provided by the invention can be used for effectively preparing the required Chinese medicine composition and ensuring that the obtained Chinese medicine composition is scientific and reasonable in the production process. The detection method provided by the invention effectively ensures Chinese medicine composition quality.

Description

A kind of Chinese medicine composition and method for making and detection method for the treatment of infantile common cold

Technical field

The present invention is a kind of Chinese medicine composition for the treatment of infantile common cold and preparation method thereof and detection method, belongs to technical field of Chinese medicine.

Technical background

Infantile common cold is all generable throughout the year commonly encountered diseases.The medicine for the treatment of flu is numerous, can buy or eat to child by adult's coldrex that family stores to pharmacy if a lot of head of a family's discovery child has caught a cold.

Children's dress drug overdose phenomenon is very general, is one of reason that causes child's drug intoxication.Because it is little at child's coldrex choice, the head of a family very worried PD again after child caught a cold, and took the coldrex of several plates simultaneously for sometimes child, yet did not know to contain identical component in these coldrexs, cause the children's dress pharmaceutical quantities too high easily, cause drug intoxication.

Even the heads of a family reduce taking dose, but there is potential danger in such behavior.Because the coldrex of most adult's usefulness all contains compositions such as acetaminophen, phenacetin, aminophenazone, caffeine, these compositions may produce inhibitory action to the also not physically well developed medulla hematopoietic system of children's, thereby influence the generation and the growth of its hemocyte, cause leukopenia and agranulocytosis, reduce child's immunity, serious sometimes caused toxic liver damages.

The main cause that causes the problems referred to above is exactly to lack effective medicine at the child, and child catches a cold and uses Chinese medicine safer, so in view of such circumstances, providing a kind of determined curative effect, toxic and side effects tcm product little, taking convenience is the thing of being badly in need of solution.

Summary of the invention

Technical problem to be solved by this invention provides a kind of Chinese medicine composition and method for making and detection method for the treatment of infantile common cold; The present invention is directed to prior art, little, the taking convenience of product determined curative effect, toxic and side effects that provides.

Technical scheme of the present invention is to constitute like this: it is made up of following active drug raw material: Moschus 12-20 part; Calculus Bovis 20-40 part; natural Broneolum Syntheticum 80-120 part; Margarita 50-80 part; Lapis Micae Aureus 50-80 part; calcined Alumen 50-80 part; succinum 120-150 part; processed with salt Herba Ephedrae 80-120 part; Concretio Silicea Bambusae 120-150 part; Radix Saposhnikoviae 140-180 part; Bulbus Fritillariae Cirrhosae 140-180 part; wine Bombyx Batryticatus(processed) 80-120 part; Rhizoma Pinelliae Preparatum 120-150 part; Rhizoma Gastrodiae 50-80 part; Rhizoma Coptidis 50-80 part; Ramulus Uncariae Cum Uncis 140-180 part; Herba Menthae 80-120 part; Periostracum Cicadae 80-120 part; Arisaema Cum Bile 80-120 part; Radix Curcumae 120-150 part; processed with salt Scorpio 80-120 part; Rhizoma Paridis 120-150 part.Be preferably: 15.3 parts in Moschus; 30.5 parts of Calculus Boviss; 105.8 parts of natural Broneolum Syntheticums; 64.5 parts of Margaritas; 64.5 parts of Lapis Micae Aureuses; 64.5 parts of calcined Alumen; 136.4 parts of succinums; 100.1 parts in processed with salt Herba Ephedrae; 133.5 parts of Concretio Silicea Bambusaes; 166.9 parts of Radix Saposhnikoviaes; 166.9 parts of Bulbus Fritillariae Cirrhosaes; 100.1 parts of wine Bombyx Batryticatus(processed); 133.5 parts of Rhizoma Pinelliae Preparatum; 66.75 parts in Rhizoma Gastrodiae; 66.75 parts of Rhizoma Coptidis; 166.9 parts of Ramulus Uncariae Cum Uncis; 100.1 parts of Herba Menthaes; 100.1 parts of Periostracum Cicadaes; 100.1 parts of Arisaema Cum Bile; 133.5 parts of Radix Curcumaes; 100.1 parts of processed with salt Scorpios; 133.5 parts of Rhizoma Paridis.

In the described raw material, calcined Alumen can also be a Borax(calcined).

The preparation method of the Chinese medicine composition of described treatment infantile common cold: the raw material of getting it filled, make multiple peroral dosage form respectively, comprising: tablet, dispersible tablet, capsule, soft capsule, granule, pill, powder, drop pill, gel, oral liquid.Be preferably: remove Moschus, Calculus Bovis, natural Broneolum Syntheticum, Margarita, Lapis Micae Aureus, Alumen, succinum seven flavor pulverize separately and become fine powder, all the other ten ground spices are broken into fine powder, and with fine powder bedding-in such as above-mentioned Moschus, mixing promptly, promptly gets powder.

The detection method of the Chinese medicine composition of described treatment infantile common cold comprises following all or part of content:

(1) all or part of microscopical identification method of testing in Bulbus Fritillariae Cirrhosae medical material, Herba Ephedrae medical material, Radix Saposhnikoviae medical material, Rhizoma Coptidis medical material, Scorpio medical material, Bombyx Batryticatus medical material, Moschus medical material, succinum medical material, Margarita medical material, the Calculus Bovis medical material;

(2) all or part of thin layer, gas chromatogram differential test method in Calculus Bovis medical material, natural Broneolum Syntheticum, Radix Saposhnikoviae medical material, Bulbus Fritillariae Cirrhosae medical material, Rhizoma Coptidis medical material, Herba Menthae medical material, Rhizoma Paridis medical material, berberine hydrochloride, ephedrine hydrochloride, Rhizoma Paridis saponin VI, Rhizoma Paridis saponin VII, cholic acid, the deoxycholic acid;

(3) content assaying method of all or part of composition in berberine hydrochloride, gastrodine, cimicifugoside and the 5-O-methyl-visamminol.

Furtherly: described discrimination method comprises following all or part of content:

A, microscopical identification method:

Get this product, put microscopically and observe, the wide avette or shell-like of starch grain, diameter 40～60um, the short seam of omphalion shape, herringbone shape or horse-hof shape, laminated striation can be examined and see; Has fine crystals on the fiber; Oil pipe contains golden yellow secretions; The stone cell foresythia is that similar round, rectangle, class are square, class triangle or class ellipse; The body wall fragment is faint yellow to have reticular texture and circular trichopore to yellow, visible sometimes sepia bristle; The body wall fragment is colourless, and there is superfine mycelium on the surface; Amorphous agglomerate is fallow, is embedded with tiny square crystallization; Irregular fragment pistac or pale brown color, transparent or semitransparent; Colourless or the light green of irregular fragment, translucent, glossy, visible sometimes fine and closely woven wavy grain; Irregular fragment is golden yellow or orange-yellow, glossy, for a long time the postpone virescence;

The thin layer chromatography discrimination method of b, Rhizoma Coptidis, berberine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol are an amount of, extracts, and is adjusted to debita spissitudo, as need testing solution; Other gets the Rhizoma Coptidis control medicinal material, shines medical material solution in pairs with legal system; Get the berberine hydrochloride reference substance again, make reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with toluene or benzene-Ethyl formate or ethyl acetate-methanol or ethanol-isopropyl alcohol-water=2～10: 1～5: 1～4: 0.5～3: 0.1～0.5 solution is developing solvent, put in the chromatography cylinder of ammonia saturated with vapor, launch after the presaturation, take out, dry, put under the ultra-violet lamp 365nm and inspect, in the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;

The gas chromatogram discrimination method of c, natural Broneolum Syntheticum, Herba Menthae:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol extractions, filters, and filtrate is as need testing solution; Other gets natural Broneolum Syntheticum, Mentholum reference substance, makes reference substance solution, according to the gas chromatography test among an appendix VI of Chinese Pharmacopoeia version in 2010 E, adopts capillary column, and heating schedule is: rise to 250 ℃ from 40 ℃; Precision is measured need testing solution and reference substance solution is an amount of respectively, inject gas chromatograph, and the test sample chromatograph should detect and natural Broneolum Syntheticum, chromatographic peak that Mentholum reference substance chromatographic retention is identical;

The thin layer chromatography discrimination method of d, ephedrine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds alkaline solution and chloroform or dichloromethane or ethyl acetate extraction, as need testing solution; Other gets the ephedrine hydrochloride reference substance and makes reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned contrast solution and test solution respectively, puts in same silica gel thin-layer plate, and with n-butyl alcohol-formic acid or glacial acetic acid-water=2～15: be developing solvent at 0.2～5: 0.1～2, launch, take out, dry, spray is with ninhydrin solution, it is clear to be heated to the speckle colour developing, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

The thin layer chromatography discrimination method of e, Radix Saposhnikoviae:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds chloroform or dichloromethane or acetic acid ethyl ester and alkaline solution and extracts, and be adjusted to debita spissitudo, as need testing solution; Other gets the Radix Saposhnikoviae control medicinal material and makes control medicinal material solution; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned contrast solution and test solution respectively, puts in same silica gel thin-layer plate, and with benzene or toluene-acetone-ethyl acetate or Ethyl formate-liquor ammoniae fortis=0.5～5: be developing solvent at 1～5: 2～6: 0.05～0.5, launch, take out, dry, spray is with vitriolated solution, heat after several minutes, put and inspect under the ultra-violet lamp 365nm in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

The thin layer chromatography discrimination method of f, Bulbus Fritillariae Cirrhosae:

It is an amount of to get compound Chinese medicinal preparation to be measured, add alkaline test solution and chloroform or dichloromethane or ethyl acetate extraction, filter, filtrate is extracted with hydrochloric acid solution, merges hydrochloric acid solution, regulate pH value to alkalescence, use chloroform extraction, complete and chloroform liquid, evaporate to dryness, residue adds ethanol or dissolve with methanol, as need testing solution; Other gets the Bulbus Fritillariae Cirrhosae control medicinal material and makes control medicinal material solution; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned test solution and contrast solution respectively, puts on same silica gel thin-layer plate, and with chloroform or dichloromethane-ethyl acetate or Ethyl formate-methanol or alcohol-water=4～12: 5～12: 1～5: 0.5～4 solution or lower floor's solution are developing solvent, launch, take out, dry, spray is to contain the solution of rare bismuth potassium iodide and sodium nitrite, inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the same color speckle;

The thin layer chromatography discrimination method of one or both of g, Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII, Rhizoma Paridis:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol extractions, filters, and the filtrate evaporate to dryness is used water dissolution, and the reuse n-butanol extraction is got n-butyl alcohol liquid, washes the back evaporate to dryness with water, and residue adds methanol or dissolve with ethanol, as need testing solution; Other gets the Rhizoma Paridis control medicinal material, makes control medicinal material solution with reference to the method for making of need testing solution; One or both that get Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII reference substance are again made mixed solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with chloroform or dichloromethane-ethyl acetate or Ethyl formate-methanol or alcohol-water=2～10: be developing solvent at 1～8: 1～6: 0.1～1, launch, take out, dry, spray is with vitriolated developer, be heated to clear spot, put respectively under daylight and the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle and the fluorescence speckle of same color;

The thin layer chromatography discrimination method of one or both of h, cholic acid and deoxycholic acid, Calculus Bovis:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol extractions, and is adjusted to debita spissitudo, as need testing solution; Get the Calculus Bovis control medicinal material, make control medicinal material solution with reference to the need testing solution method for making; Get one or both of cholic acid, deoxycholic acid, make reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with toluene or benzene-formic acid or glacial acetic acid-water=5～15: be developing solvent at 5～15: 0.3～2, launches, and takes out, dry, spray is heated to clear spot with vitriolated developer, puts under the ultra-violet lamp 365nm and inspects; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the same color speckle.

Be preferably: described discrimination method comprises following all or part of content:

A, microscopical identification method:

Get this product, put microscopically and observe, the wide avette or shell-like of starch grain, diameter 40～60um, the short seam of omphalion shape, herringbone shape or horse-hof shape, laminated striation can be examined and see; Has fine crystals on the fiber; Oil pipe contains golden yellow secretions; The stone cell foresythia is that similar round, rectangle, class are square, class triangle or class ellipse; The body wall fragment is faint yellow to have reticular texture and circular trichopore to yellow, visible sometimes sepia bristle; The body wall fragment is colourless, and there is superfine mycelium on the surface; Amorphous agglomerate is fallow, is embedded with tiny square crystallization; Irregular fragment pistac or pale brown color, transparent or semitransparent; Colourless or the light green of irregular fragment, translucent, glossy, visible sometimes fine and closely woven wavy grain; Irregular fragment is golden yellow or orange-yellow, glossy, for a long time the postpone virescence;

The thin layer chromatography discrimination method of b, Rhizoma Coptidis, berberine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filters, and filtrate is as need testing solution; Other gets the Rhizoma Coptidis control medicinal material, shines medical material solution in pairs with legal system; Getting berberine hydrochloride again adds methanol and makes reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, puts on same silica gel thin-layer plate, and with toluene-ethyl acetate-methanol-isopropyl alcohol-water=6: 3: 2: be developing solvent at 1.5: 0.3, put in the chromatography cylinder of ammonia saturated with vapor, launch after the presaturation, take out, dry, put under the ultra-violet lamp 365nm and inspect, in the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;

The gas chromatogram discrimination method of c, natural Broneolum Syntheticum, Herba Menthae:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filters, and filtrate is as need testing solution; Other gets natural Broneolum Syntheticum, Mentholum reference substance, add ethanol and make reference substance solution respectively, test according to the gas chromatography among an appendix VI of Chinese Pharmacopoeia version in 2010 E, with the Polyethylene Glycol is the capillary column of filler, heating schedule is: the heating rate with 10 ℃/min rises to 130 ℃ from 80 ℃, heating rate with 20 ℃/min rises to 180 ℃, precision is measured need testing solution and reference substance solution is an amount of respectively, inject gas chromatograph, test sample chromatograph should detect and natural Broneolum Syntheticum, chromatographic peak that Mentholum reference substance chromatographic retention is identical;

The thin layer chromatography discrimination method of d, ephedrine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds liquor ammoniae fortis and dichloromethane extraction, filters, and filtrate evaporate to dryness, the residue 1ml that adds methylene chloride makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methylene chloride to make reference substance solution; Employing thin layer chromatography test, it is an amount of to draw above-mentioned contrast solution and test solution respectively, put in same silica gel thin-layer plate, be developing solvent with n-butyl alcohol-glacial acetic acid-water=8: 2: 1, launch, take out, dry, spray is with ninhydrin solution, be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

The thin layer chromatography discrimination method of e, Radix Saposhnikoviae:

It is an amount of to get compound Chinese medicinal preparation to be measured, and add chloroform and liquor ammoniae fortis and extract, the filtrate evaporate to dryness, residue adds dissolve with methanol, as need testing solution; Other gets the Radix Saposhnikoviae control medicinal material and shines medical material solution in pairs with legal system; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned contrast solution and test solution respectively, point is in same silica gel thin-layer plate, with benzene-acetone-ethyl acetate-liquor ammoniae fortis=2: 3: 4: 0.2 was developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing, puts under the ultra-violet lamp 365nm and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

The thin layer chromatography discrimination method of f, Bulbus Fritillariae Cirrhosae:

It is an amount of to get compound Chinese medicinal preparation to be measured, add ammonia solution and chloroform extraction, filter, filtrate is extracted with the jolting of 0.1mol/L hydrochloric acid solution, merges hydrochloric acid solution, add strong ammonia solution and regulate pH value to 10, extract with the chloroform jolting, merge chloroform liquid, evaporate to dryness, residue adds dissolve with ethanol, as need testing solution; Other gets the Bulbus Fritillariae Cirrhosae control medicinal material and shines medical material solution in pairs with legal system; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned test solution and contrast solution respectively, point is on same silica gel thin-layer plate, with chloroform-ethyl acetate-methanol-water=8: 8: 3: lower floor's solution of 2 was developing solvent, launch, take out, dry, spray successively with rare bismuth potassium iodide test solution and sodium nitrite ethanol test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;

The thin layer chromatography discrimination method of one or both of g, Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII, Rhizoma Paridis:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filters, and the filtrate evaporate to dryness is used water dissolution, puts in the separatory funnel, extracts with n-butyl alcohol liquid, gets n-butyl alcohol liquid, washes with water, and n-butyl alcohol liquid is put evaporate to dryness in the water-bath, and residue adds dissolve with methanol, as need testing solution; Other gets the Rhizoma Paridis control medicinal material, makes control medicinal material solution with reference to the method for making of need testing solution; One or both that get Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII reference substance again add methanol and make mixed solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with chloroform-ethyl acetate-methanol-water=5: 4: 3: 0.6 was developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing, puts respectively under daylight and the ultra-violet lamp 365nm and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle and the fluorescence speckle of same color;

The thin layer chromatography discrimination method of one or both of h, cholic acid and deoxycholic acid, Calculus Bovis:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filter, and the filtrate evaporate to dryness, residue adds dissolve with methanol, as need testing solution; Get the Calculus Bovis control medicinal material, make control medicinal material solution with reference to the need testing solution method for making; Get one or both of cholic acid, deoxycholic acid, add methanol and make reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with toluene-glacial acetic acid-water=10: 10: 0.8 was developing solvent, launched, and took out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing, puts under the ultra-violet lamp 365nm and inspects; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the same color speckle.

Specifically, described content assaying method should comprise following all or part of content:

The content assaying method of a, berberine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides, and adds acidic methanol solution and extracts, and extracting solution is as need testing solution; With the berberine hydrochloride reference substance, make reference substance solution, adopt liquid chromatography, chromatographic column is a filler with the alkyl silane bonded silica gel, with methanol or acetonitrile-0.1%～1% glacial acetic acid aqueous solution or 0.1%～1% aqueous formic acid or 0.1%～1% phosphate aqueous solution or 0.02mol/L～0.2mol/L sodium dihydrogen phosphate or 0.02mol/L～0.2mol/L potassium dihydrogen phosphate or 0.02mol/L～0.2mol/L biphosphate amine aqueous solution=20～35: 80～65 is mobile phase, detects wavelength and be among 330～370nm; Accurate respectively above-mentioned test solution of absorption and contrast solution are an amount of, inject chromatograph of liquid, calculate with one point external standard method or standard curve method, and the hydrochloric berberine of the every gram of preparation must not be less than 0.5mg;

The content assaying method of b, cimicifugoside and 5-O-methyl-visamminol:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides, and adds 80～100% methanol or 80～100% ethanol extractions, and is adjusted to debita spissitudo, as need testing solution; Get cimicifugoside reference substance and 5-O-methyl-visamminol reference substance, make reference substance solution; Adopt liquid chromatography, chromatographic column is a filler with the alkyl silane bonded silica gel, with methanol or acetonitrile-water or 0.05%～0.1% glacial acetic acid aqueous solution or 0.05%～0.1% aqueous formic acid or 0.005%～0.01% phosphate aqueous solution=25～45: 75～55 is mobile phase, detects wavelength and be among 280～320nm; It is an amount of to draw above-mentioned test solution and contrast solution respectively, injects chromatograph of liquid, calculates with one point external standard method or standard curve method, and the total amount that the every gram of preparation contains cimicifugoside and 5-O-methyl-visamminol must not be less than 0.05mg;

The content assaying method of c, gastrodine:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides, and adds 80～100% methanol or 80～100% ethanol extractions, and extracting solution is concentrated near doing, and residue dissolves with mobile phase, as need testing solution; Make reference substance solution with the gastrodine reference substance, adopt liquid chromatography, chromatographic column is a filler with the alkyl silane bonded silica gel, acetonitrile or methanol-0.05%～0.2% phosphate aqueous solution or 0.05%～0.2% glacial acetic acid aqueous solution or 0.05%～0.2% aqueous formic acid=1～3: 99～97 is mobile phase, and the detection wavelength is among 200～250nm; It is an amount of to draw above-mentioned test solution and contrast solution respectively, injects chromatograph of liquid, calculates with one point external standard method or standard curve method, and the every gram of preparation contains gastrodine must not be less than 0.015mg.

Be preferably: described content assaying method comprises following all or part of content:

The content assaying method of a, berberine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, and the 2% hydrochloric acid-methanol mixed solution that adds by preparation in 1: 1 extracts, the extracting solution evaporate to dryness, and extracting solution is as need testing solution; Methanol solution with berberine hydrochloride is made reference substance solution, adopts liquid chromatography, and the chromatographic column octadecylsilane chemically bonded silica is a filler, is mobile phase with acetonitrile-0.05mol/L potassium dihydrogen phosphate=28: 72, and the detection wavelength is 350nm; Accurate respectively above-mentioned test solution of absorption and contrast solution are an amount of, inject chromatograph of liquid, calculate with one point external standard method, and the hydrochloric berberine of the every gram of preparation must not be less than 1mg;

The liquid chromatograph content assaying method of b, cimicifugoside and 5-O-methyl-visamminol:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides, methanol extraction, and be adjusted to debita spissitudo, as need testing solution; Get the cimicifugoside reference substance and the 5-O-methyl-visamminol reference substance is made reference substance solution with methanol; Adopt liquid chromatography, the chromatographic column octadecylsilane chemically bonded silica is a filler, is mobile phase with methanol-water=35: 65, and the detection wavelength is 292nm; It is an amount of to draw above-mentioned test solution and contrast solution respectively, injects chromatograph of liquid, calculates with one point external standard method, and the total amount that the every gram of preparation contains cimicifugoside and 5-O-methyl-visamminol must not be less than 0.1mg;

The content assaying method of c, gastrodine:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides or measure, and adds methanol extraction, and extracting solution is concentrated near doing, and residue dissolves with mobile phase, as need testing solution; Get the gastrodine reference substance and make reference substance solution with mobile phase; Adopt liquid chromatography, the chromatographic column octadecylsilane chemically bonded silica is a filler, and acetonitrile-0.1% phosphate aqueous solution=2: 98 is a mobile phase, and the detection wavelength is 220nm; It is an amount of to draw above-mentioned test solution and contrast solution respectively, injects chromatograph of liquid, calculates with one point external standard method, and the every gram of preparation contains gastrodine must not be less than 0.03mg.

We are made up of kinds of traditional Chinese medicines such as Moschus, Calculus Boviss, have wind and heat dispersing, the effect of the arresting convulsion of reducing phlegm.Be used for infantile common cold, because of the exterior attacked by wind and cold, fever with chills due to the dyspepsia heat-transformation, the sneeze watery nasal discharge brings up phlegm when one coughs and anorexia, and night cry is easily frightened to wait disease.

The research of experimental example prescription

1 group: 12 parts in Moschus, 20 parts of Calculus Boviss, 80 parts of natural Broneolum Syntheticums, 50 parts of Margaritas, 50 parts of Lapis Micae Aureuses, 50 parts of calcined Alumen, 120 parts of succinums, 80 parts in processed with salt Herba Ephedrae, 120 parts of Concretio Silicea Bambusaes, 140 parts of Radix Saposhnikoviaes, 140 parts of Bulbus Fritillariae Cirrhosaes, 80 parts of wine Bombyx Batryticatus(processed), 120 parts of Rhizoma Pinelliae Preparatum, 50 parts in Rhizoma Gastrodiae, 50 parts of Rhizoma Coptidis, 140 parts of Ramulus Uncariae Cum Uncis, 80 parts of Herba Menthaes, 80 parts of Periostracum Cicadaes, 80 parts of Arisaema Cum Bile, 120 parts of Radix Curcumaes, 80 parts of processed with salt Scorpios, 120 parts of Rhizoma Paridis

2 groups: 20 parts in Moschus, 40 parts of Calculus Boviss, 120 parts of natural Broneolum Syntheticums, 80 parts of Margaritas, 80 parts of Lapis Micae Aureuses, 80 parts of calcined Alumen, 150 parts of succinums, 120 parts in processed with salt Herba Ephedrae, 150 parts of Concretio Silicea Bambusaes, 180 parts of Radix Saposhnikoviaes, 180 parts of Bulbus Fritillariae Cirrhosaes, 120 parts of wine Bombyx Batryticatus(processed), 150 parts of Rhizoma Pinelliae Preparatum, 80 parts in Rhizoma Gastrodiae, 80 parts of Rhizoma Coptidis, 180 parts of Ramulus Uncariae Cum Uncis, 120 parts of Herba Menthaes, 120 parts of Periostracum Cicadaes, 120 parts of Arisaema Cum Bile, 150 parts of Radix Curcumaes, 120 parts of processed with salt Scorpios, 150 parts of Rhizoma Paridis

3 groups: 15.3 parts in Moschus; 30.5 parts of Calculus Boviss; 105.8 parts of natural Broneolum Syntheticums; 64.5 parts of Margaritas; 64.5 parts of Lapis Micae Aureuses; 64.5 parts of calcined Alumen; 136.4 parts of succinums; 100.1 parts in processed with salt Herba Ephedrae; 133.5 parts of Concretio Silicea Bambusaes; 166.9 parts of Radix Saposhnikoviaes; 166.9 parts of Bulbus Fritillariae Cirrhosaes; 100.1 parts of wine Bombyx Batryticatus(processed); 133.5 parts of Rhizoma Pinelliae Preparatum; 66.75 parts in Rhizoma Gastrodiae; 66.75 parts of Rhizoma Coptidis; 166.9 parts of Ramulus Uncariae Cum Uncis; 100.1 parts of Herba Menthaes; 100.1 parts of Periostracum Cicadaes; 100.1 parts of Arisaema Cum Bile; 133.5 parts of Radix Curcumaes; 100.1 parts of processed with salt Scorpios; 133.5 parts of Rhizoma Paridis

4 groups: 12 parts in Moschus, 20 parts of Calculus Boviss, 80 parts of natural Broneolum Syntheticums, 50 parts of Margaritas, 50 parts of Lapis Micae Aureuses, 50 parts of Borax(calcined), 120 parts of succinums, 80 parts in processed with salt Herba Ephedrae, 120 parts of Concretio Silicea Bambusaes, 140 parts of Radix Saposhnikoviaes, 140 parts of Bulbus Fritillariae Cirrhosaes, 80 parts of wine Bombyx Batryticatus(processed), 120 parts of Rhizoma Pinelliae Preparatum, 50 parts in Rhizoma Gastrodiae, 50 parts of Rhizoma Coptidis, 140 parts of Ramulus Uncariae Cum Uncis, 80 parts of Herba Menthaes, 80 parts of Periostracum Cicadaes, 80 parts of Arisaema Cum Bile, 120 parts of Radix Curcumaes, 80 parts of processed with salt Scorpios, 120 parts of Rhizoma Paridis

5 groups: 20 parts in Moschus, 40 parts of Calculus Boviss, 120 parts of natural Broneolum Syntheticums, 80 parts of Margaritas, 80 parts of Lapis Micae Aureuses, 80 parts of Borax(calcined), 150 parts of succinums, 120 parts in processed with salt Herba Ephedrae, 150 parts of Concretio Silicea Bambusaes, 180 parts of Radix Saposhnikoviaes, 180 parts of Bulbus Fritillariae Cirrhosaes, 120 parts of wine Bombyx Batryticatus(processed), 150 parts of Rhizoma Pinelliae Preparatum, 80 parts in Rhizoma Gastrodiae, 80 parts of Rhizoma Coptidis, 180 parts of Ramulus Uncariae Cum Uncis, 120 parts of Herba Menthaes, 120 parts of Periostracum Cicadaes, 120 parts of Arisaema Cum Bile, 150 parts of Radix Curcumaes, 120 parts of processed with salt Scorpios, 150 parts of Rhizoma Paridis

6 groups: 15.3 parts in Moschus; 30.5 parts of Calculus Boviss; 105.8 parts of natural Broneolum Syntheticums; 64.5 parts of Margaritas; 64.5 parts of Lapis Micae Aureuses; 64.5 parts of Borax(calcined); 136.4 parts of succinums; 100.1 parts in processed with salt Herba Ephedrae; 133.5 parts of Concretio Silicea Bambusaes; 166.9 parts of Radix Saposhnikoviaes; 166.9 parts of Bulbus Fritillariae Cirrhosaes; 100.1 parts of wine Bombyx Batryticatus(processed); 133.5 parts of Rhizoma Pinelliae Preparatum; 66.75 parts in Rhizoma Gastrodiae; 66.75 parts of Rhizoma Coptidis; 166.9 parts of Ramulus Uncariae Cum Uncis; 100.1 parts of Herba Menthaes; 100.1 parts of Periostracum Cicadaes; 100.1 parts of Arisaema Cum Bile; 133.5 parts of Radix Curcumaes; 100.1 parts of processed with salt Scorpios; 133.5 parts of Rhizoma Paridis

(1) to the influence of rat fever due to the dry yeast

Choose healthy white rat, male and female half and half are allowed to condition at laboratory environment and adapt to 3 days, measure the anus temperature every day 2 times, get the body temperature variation during experiment in the 4th day and be no more than 0.3 ℃ rat, after measuring normal body temperature (anus temperature) 2 times,, select after the 6th hour 70 of the rat of body temperature rise more than 0.8 ℃ in the dry yeast suspension 10ml/kg of rat back subcutaneous injection 20% body weight, be divided into 7 groups at random, 10 of every treated animals are pressed 2.66g/kg gastric infusion respectively then, and matched group gives the equivalent distilled water.Behind medicine, respectively surveyed body temperature 1 time in 1,2,3 hour, relatively the difference of each animal heat drop-out value.The results are shown in Table 1.

The refrigeration function of table 1 pair yeast mixture pyrogenicity rat

Table 1 result as seen, behind the administration group medicine after 1,2,3 hour, of the present invention group all has tangible refrigeration function to yeast mixture pyrogenicity rat, with matched group relatively, effect is all obvious.

(2) influence that white mice due to the strychnine is fainted from fear

Choosing body weight is 140 of 18-20g healthy mices, and male and female half and half are divided into 7 groups at random, press the 2.66g/kg gastric infusion, every day 1 time, continuous 7 days, the convulsions incubation period of white mice and the number that causes death were respectively organized in observation in mice by intraperitoneal injection strychnine nitrate 1.5mg/kg in 1 hour after the last administration.The results are shown in Table 2.

The influence that white mice is fainted from fear due to the table 2 pair strychnine

Table 2 result as seen, of the present invention group white mice due to the strychnine being fainted from fear all can prolong its incubation period and reduce the number that causes death, and obviously reduces mortality rate.

Above-mentioned experiment shows that each set product of the present invention all has certain heat-clearing and toxic substances removing, and the relieving convulsion effect of reducing phlegm is wherein, remarkable with the effect of prescription 3 and prescription 6 especially.

The correlational study of experimental example detection method

This prescription element complexity, so the applicant has formulated the quality that perfect discriminating and content assaying method are controlled this compound preparation comprehensively by a large amount of experimentatioies.But because contained complex chemical composition between each medical material in this compound preparation, discriminating and assay are caused interference, cause differentiating, the feature instability of assay, so must just can obtain good thin layer chromatography and contain the survey condition by control mobile phase, developing solvent isochromatic spectrum condition.That is to say,, just can obtain ideal thin layer chromatography and content assaying method because each composition interference effect each other in the prescription has only the condition of the present invention of employing.

(1) the microscopical identification method research of part medical material in the preparation:

Get this product, put microscopically and observe, the wide avette or shell-like of starch grain, diameter 40～60um, the short seam of omphalion shape, herringbone shape or horse-hof shape, laminated striation can be examined and see (Bulbus Fritillariae Cirrhosae).Has fine crystals (Herba Ephedrae) on the fiber.Oil pipe contains golden yellow secretions (Radix Saposhnikoviae).The stone cell foresythia is that similar round, rectangle, class are square, class triangle or class ellipse (Rhizoma Coptidis).The body wall fragment is faint yellow to have reticular texture and circular trichopore to yellow, visible sometimes sepia bristle (Scorpio).The body wall fragment is colourless, and there is superfine mycelium (Bombyx Batryticatus) on the surface.Amorphous agglomerate is fallow, is embedded with tiny square crystallization (Moschus).Irregular fragment pistac or pale brown color, transparent or semitransparent (succinum).Colourless or the light green of irregular fragment, translucent, glossy, visible sometimes fine and closely woven wavy grain (Margarita).Irregular fragment is golden yellow or orange-yellow, glossy, for a long time postpone virescence (Calculus Bovis).

(2) the thin layer chromatography discrimination method of Rhizoma Coptidis, berberine hydrochloride research in the preparation:

For the feature of outstanding Rhizoma Coptidis, selected Rhizoma Coptidis control medicinal material and berberine hydrochloride reference substance in contrast, but, can differentiate the feature speckle and cause interference owing to become split pole many in this compound preparation.Have only the interference of getting rid of other compositions, could obtain ideal chromatograph effect.The key factor of thin layer chromatography effect quality is the composition of unfolding condition, particularly developing solvent.Therefore, experiment sieving the different expansion effect of sample preparation methods under multiple unfolding condition, seeking available method simultaneously, determine optimum discrimination method.Part unfolding condition and result are as follows:

The thin layer chromatography discrimination method of Rhizoma Coptidis, berberine hydrochloride research in the preparation

Through screening, we are informed under the following condition can obtain basic identification result:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol are an amount of, extracts, and is adjusted to debita spissitudo, as need testing solution; Other gets the Rhizoma Coptidis control medicinal material, shines medical material solution in pairs with legal system; Get the berberine hydrochloride reference substance again, make reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with toluene or benzene-Ethyl formate or ethyl acetate-methanol or ethanol-isopropyl alcohol-water=2～10: 1～5: 1～4: 0.5～3: 0.1～0.5 solution is developing solvent, put in the chromatography cylinder of ammonia saturated with vapor, launch after the presaturation, take out, dry, put under the ultra-violet lamp 365nm and inspect.

Determine that optimum condition is:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filters, and filtrate is as need testing solution; Other gets the Rhizoma Coptidis control medicinal material, shines medical material solution in pairs with legal system; Getting berberine hydrochloride again adds methanol and makes reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with toluene-ethyl acetate-methanol-isopropyl alcohol-water=6: 3: 2: be developing solvent at 1.5: 0.3, put in the chromatography cylinder of ammonia saturated with vapor, launch after the presaturation, take out, dry, put under the ultra-violet lamp 365nm and inspect.

With this understanding, the Rf value of the speckle of Rhizoma Coptidis control medicinal material feature speckle and berberine hydrochloride reference substance is moderate, and it is clear to separate with other speckle, and is negative noiseless.

(3) the gas chromatogram discrimination method of natural Broneolum Syntheticum, Herba Menthae research in the preparation:

Feature for outstanding natural Broneolum Syntheticum, Herba Menthae, natural Broneolum Syntheticum, Mentholum product have in contrast been selected, adopt gas chromatography to differentiate, because these two kinds of compositions all have volatility, it is easier to adopt gas chromatogram to differentiate, and specificity is differentiated stronger than thin layer, and the key factor of thin layer chromatography effect quality is the selection of chromatographic column, particularly the intensification condition of chromatographic column.Therefore, experiment sieving the different separating effect of sample preparation methods under multiple heating schedule, seeking available method simultaneously, determine optimum discrimination method.Part heating schedule and result are as follows:

The gas chromatogram discrimination method of natural Broneolum Syntheticum, Herba Menthae research in the preparation

Through screening, we are informed under the following condition can obtain basic identification result:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol extractions, filters, and filtrate is as need testing solution; Other gets natural Broneolum Syntheticum, Mentholum reference substance, makes reference substance solution, according to the gas chromatography test among an appendix VI of Chinese Pharmacopoeia version in 2010 E, adopts capillary column, and heating schedule is: rise to 250 ℃ from 40 ℃; Precision is measured need testing solution and reference substance solution is an amount of respectively, and inject gas chromatograph can be observed.

Determined optimum condition:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filters, and filtrate is as need testing solution; Other gets natural Broneolum Syntheticum, Mentholum reference substance, add ethanol and make reference substance solution respectively, test according to the gas chromatography among an appendix VI of Chinese Pharmacopoeia version in 2010 E, with the Polyethylene Glycol is the capillary column of filler, heating schedule is: rise to 130 ℃ with the heating rate of 10 ℃/min from 80 ℃, rise to 180 ℃ with the heating rate of 20 ℃/min, precision is measured need testing solution and reference substance solution is an amount of respectively, inject gas chromatograph can be observed.

With this understanding, the chromatographic peak appearance time of natural Broneolum Syntheticum and Herba Menthae is moderate, and two chromatographic peaks separate complete, negative noiseless.

(4) the thin layer chromatography discrimination method of ephedrine hydrochloride in the preparation:

For the feature of outstanding Herba Ephedrae, selected ephedrine hydrochloride as its feature speckle, but owing to had composition like more, the polar phase close in the compound Chinese medicinal preparation with the ephedrine hydrochloride structure.Have only the interference of getting rid of these compositions, could obtain ideal chromatograph effect.The key factor of thin layer chromatography effect quality is the composition of unfolding condition, particularly developing solvent.Therefore, experiment sieving the different expansion effect of sample preparation methods under multiple unfolding condition, seeking available method simultaneously, determine optimum discrimination method.Part unfolding condition and result are as follows:

The thin layer chromatography discrimination method of ephedrine hydrochloride in the preparation

Through screening, we are informed under the following condition can obtain basic identification result:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds alkaline solution and chloroform or dichloromethane or ethyl acetate extraction, as need testing solution; Other gets the ephedrine hydrochloride reference substance and makes reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned contrast solution and test solution respectively, puts in same silica gel thin-layer plate, with n-butyl alcohol-formic acid or glacial acetic acid-water=2～15: be developing solvent at 0.2～5: 0.1～2, launches, and takes out, dry, spray is with ninhydrin solution, and it is clear to be heated to speckle colour developing.Can observe.

Determined optimum condition:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds liquor ammoniae fortis and dichloromethane extraction, filters, and filtrate evaporate to dryness, the residue 1ml that adds methylene chloride makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methylene chloride to make reference substance solution; Employing thin layer chromatography test, it is an amount of to draw above-mentioned contrast solution and test solution respectively, put in same silica gel thin-layer plate, be developing solvent with n-butyl alcohol-glacial acetic acid-water=8: 2: 1, launch, take out, dry, spray is with ninhydrin solution, be heated to speckle develop the color clear.Can observe.

With this understanding, the Rf value of ephedrine hydrochloride is moderate, and it is clear to separate with other speckle, and is negative noiseless.

(5) the thin layer chromatography discrimination method of Radix Saposhnikoviae in the preparation:

For the feature of outstanding Radix Saposhnikoviae, selected the Radix Saposhnikoviae control medicinal material in contrast, but because this compound Chinese medicinal preparation medical material amount is more, complicated component.Have only the interference of getting rid of other compositions, could obtain ideal chromatograph effect.The key factor of thin layer chromatography effect quality is the composition of unfolding condition, particularly developing solvent.Therefore, experiment sieving the different expansion effect of sample preparation methods under multiple unfolding condition, seeking available method simultaneously, determine optimum discrimination method.Part unfolding condition and result are as follows:

The thin layer chromatography discrimination method of Radix Saposhnikoviae in the preparation

Conditional outcome

Benzene-ethyl acetate-liquor ammoniae fortis (2: 3: 0.2) silica gel H lamellae Rf value is on the low side, separates unintelligible

(2: 5: 3: 0.5) the silica gel g thin-layer plate Rf value was higher, separated unintelligible for toluene-acetone-ethyl acetate-liquor ammoniae fortis

Benzene-Ethyl formate-liquor ammoniae fortis (3: 6: 0.5) silica gel g thin-layer plate feminine gender has interference

(3: 2: 1: 1) the silica gel H lamellae separated unintelligible toluene-acetone-Ethyl formate-water

Acetone-ethyl acetate-water (8: 3: 7) silica gel g thin-layer plate feminine gender has interference

(3: 4: 5: 0.2) the silica gel g thin-layer plate feminine gender had interference to benzene-ethyl acetate-ethanol-liquor ammoniae fortis

Benzene-acetone-ethyl acetate-liquor ammoniae fortis=(2: 3: 4: 0.2) the silica gel g thin-layer plate separation is clear, and Rf value is moderate, and was negative noiseless

Through screening, we are informed under the following condition can obtain basic identification result:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds chloroform or dichloromethane or acetic acid ethyl ester and alkaline solution and extracts, and be adjusted to debita spissitudo, as need testing solution; Other gets the Radix Saposhnikoviae control medicinal material and makes control medicinal material solution; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned contrast solution and test solution respectively, point is in same silica gel thin-layer plate, with benzene or toluene-acetone-ethyl acetate or Ethyl formate-liquor ammoniae fortis=0.5～5: be developing solvent at 1～5: 2～6: 0.05～0.5, launches, and takes out, dry, spray is heated after several minutes with vitriolated solution, puts under the ultra-violet lamp 365nm and inspects.

Determined optimum condition:

It is an amount of to get compound Chinese medicinal preparation to be measured, and add chloroform and liquor ammoniae fortis and extract, the filtrate evaporate to dryness, residue adds dissolve with methanol, as need testing solution; Other gets the Radix Saposhnikoviae control medicinal material and shines medical material solution in pairs with legal system; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned contrast solution and test solution respectively, point is in same silica gel thin-layer plate, with benzene-acetone-ethyl acetate-liquor ammoniae fortis=2: 3: 4: 0.2 was developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing, puts under the ultra-violet lamp 365nm and inspects.

With this understanding, the feature clear spot of Radix Saposhnikoviae control medicinal material, Rf value is moderate, separates better with other speckle, and is negative noiseless.

(6) the thin layer chromatography discrimination method of Bulbus Fritillariae Cirrhosae in the preparation:

For the feature of outstanding Bulbus Fritillariae Cirrhosae, selected the Bulbus Fritillariae Cirrhosae control medicinal material to be contrast, but, can differentiate the feature speckle and cause interference owing to become split pole many in this compound preparation.Have only the interference of getting rid of other compositions, could obtain ideal chromatograph effect.The key factor of thin layer chromatography effect quality is the composition of unfolding condition, particularly developing solvent.Therefore, experiment sieving the different expansion effect of sample preparation methods under multiple unfolding condition, seeking available method simultaneously, determine optimum discrimination method.Part unfolding condition and result are as follows:

The thin layer chromatography discrimination method of Bulbus Fritillariae Cirrhosae in the preparation

Through screening, we are informed under the following condition can obtain basic identification result:

It is an amount of to get compound Chinese medicinal preparation to be measured, add alkaline test solution and chloroform or dichloromethane or ethyl acetate extraction, filter, filtrate is extracted with hydrochloric acid solution, merges hydrochloric acid solution, regulate pH value to alkalescence, use chloroform extraction, complete and chloroform liquid, evaporate to dryness, residue adds ethanol or dissolve with methanol, as need testing solution; Other gets the Bulbus Fritillariae Cirrhosae control medicinal material and makes control medicinal material solution; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned test solution and contrast solution respectively, point is on same silica gel thin-layer plate, with chloroform or dichloromethane-ethyl acetate or Ethyl formate-methanol or alcohol-water=4～12: 5～12: 1～5: 0.5～4 solution or lower floor's solution are developing solvent, launch, take out, dry, spray is inspected to contain the solution of rare bismuth potassium iodide and sodium nitrite.

Determined optimum condition:

It is an amount of to get compound Chinese medicinal preparation to be measured, add ammonia solution and chloroform extraction, filter, filtrate is extracted with the jolting of 0.1mol/L hydrochloric acid solution, merges hydrochloric acid solution, add strong ammonia solution and regulate pH value to 10, extract with the chloroform jolting, merge chloroform liquid, evaporate to dryness, residue adds dissolve with ethanol, as need testing solution; Other gets the Bulbus Fritillariae Cirrhosae control medicinal material and shines medical material solution in pairs with legal system; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned test solution and contrast solution respectively, point is on same silica gel thin-layer plate, with chloroform-ethyl acetate-methanol-water=8: 8: 3: lower floor's solution of 2 was developing solvent, launch, take out, dry, spray successively with rare bismuth potassium iodide test solution and sodium nitrite ethanol test solution, can inspect.

With this understanding, the Rf value of Bulbus Fritillariae Cirrhosae feature speckle is moderate, and it is clear to separate with other speckle, and is negative noiseless.

(7) the thin layer chromatography discrimination method of Rhizoma Paridis, Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII in the preparation:

For the feature of outstanding Rhizoma Paridis, selected Rhizoma Paridis control medicinal material, Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII reference substance to be contrast, but, can differentiate the feature speckle and cause interference owing to become split pole many in this compound preparation.Have only the interference of getting rid of other compositions, could obtain ideal chromatograph effect.The key factor of thin layer chromatography effect quality is the composition of unfolding condition, particularly developing solvent.Therefore, experiment sieving the different expansion effect of sample preparation methods under multiple unfolding condition, seeking available method simultaneously, determine optimum discrimination method.Part unfolding condition and result are as follows:

The thin layer chromatography discrimination method of Rhizoma Paridis, Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII in the preparation

Through screening, we are informed under the following condition can obtain basic identification result:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol extractions, filters, and the filtrate evaporate to dryness is used water dissolution, and the reuse n-butanol extraction is got n-butyl alcohol liquid, washes the back evaporate to dryness with water, and residue adds methanol or dissolve with ethanol, as need testing solution; Other gets the Rhizoma Paridis control medicinal material, makes control medicinal material solution with reference to the method for making of need testing solution; Get the Rhizoma Paridis saponin VI again and Rhizoma Paridis saponin VII reference substance is made mixed solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with chloroform or dichloromethane-ethyl acetate or Ethyl formate-methanol or alcohol-water=2～10: be developing solvent at 1～8: 1～6: 0.1～1, launches, and takes out, dry, spray is heated to clear spot with vitriolated developer, puts respectively under daylight and the ultra-violet lamp (365nm) and inspects.

Determined optimum condition:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filters, and the filtrate evaporate to dryness is used water dissolution, puts in the separatory funnel, extracts with n-butyl alcohol liquid, gets n-butyl alcohol liquid, washes with water, and n-butyl alcohol liquid is put evaporate to dryness in the water-bath, and residue adds dissolve with methanol, as need testing solution; Other gets the Rhizoma Paridis control medicinal material, makes control medicinal material solution with reference to the method for making of need testing solution; Getting Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII reference substance again adds methanol and makes mixed solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with chloroform-ethyl acetate-methanol-water=5: 4: 3: 0.6 was developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing, puts respectively under daylight and the ultra-violet lamp 365nm and inspects.

With this understanding, the Rf value of the feature clear spot of Rhizoma Paridis control medicinal material, Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII is moderate, and it is clear to separate with other speckle, and is negative noiseless.

(8) the thin layer chromatography discrimination method of Calculus Bovis, cholic acid and deoxycholic acid in the preparation:

Feature for outstanding Calculus Bovis; selected Calculus Bovis control medicinal material, cholic acid and deoxycholic acid reference substance in contrast, but because wherein there is more active component in this compound Chinese medicinal preparation more complicated; have only the interference of getting rid of these compositions, could obtain ideal chromatograph effect.The key factor of thin layer chromatography effect quality is the composition of unfolding condition, particularly developing solvent.Therefore, experiment sieving the different expansion effect of sample preparation methods under multiple unfolding condition, seeking available method simultaneously, determine optimum discrimination method.Part unfolding condition and result are as follows:

The thin layer chromatography discrimination method of Calculus Bovis, cholic acid and deoxycholic acid in the preparation

Conditional outcome

Toluene-acetone-water (6: 5: 0.5) silica gel g thin-layer plate separates unintelligible

The exhibition of ethyl acetate-glacial acetic acid-water (5: 5: 1) silica gel H lamellae reference substance is to the forward position

Benzene-ethyl acetate-glacial acetic acid (5: 5: 4) silica gel g thin-layer plate feminine gender has interference

Toluene-glacial acetic acid (10: 7) silica gel H lamellae feminine gender has interference

Benzene-formic acid-water (7: 5: 0.5) silica gel g thin-layer plate separates unintelligible, and feminine gender has interference

It is clear that toluene-glacial acetic acid-water=(10: 10: 0.8) silica gel g thin-layer plate separates, and Rf value is moderate, negative noiseless

Through screening, we are informed under the following condition can obtain basic identification result:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol extractions, and is adjusted to debita spissitudo, as need testing solution; Get the Calculus Bovis control medicinal material, make control medicinal material solution with reference to the need testing solution method for making; Get cholic acid, deoxycholic acid, make reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with toluene or benzene-formic acid or glacial acetic acid-water=5～15: be developing solvent at 5～15: 0.3～2, launches, and takes out, dry, spray is heated to clear spot with vitriolated developer, puts under the ultra-violet lamp 365nm and inspects.

Determined optimum condition:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filter, and the filtrate evaporate to dryness, residue adds dissolve with methanol, as need testing solution; Get the Calculus Bovis control medicinal material, make control medicinal material solution with reference to the need testing solution method for making; Get cholic acid, deoxycholic acid, add methanol and make reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with toluene-glacial acetic acid-water=10: 10: 0.8 was developing solvent, launched, and took out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing, puts under the ultra-violet lamp 365nm and inspects.

With this understanding, the Rf value of the feature speckle of Calculus Bovis control medicinal material and cholic acid and deoxycholic acid speckle is moderate, and it is clear to separate with other speckle, and is negative noiseless.

(9) assay of berberine hydrochloride in the preparation:

Complicated component in the compound Chinese medicinal preparation must just might be got rid of other compositions and disturb by systematic research, obtains accurate target component content assay method.In concrete research, the preparation of sample, the selection of chromatographic column, the equal multiple factor that flows all have very big influence to experimental result, and we have carried out the screening investigation to each influence factor, in the hope of finding the available survey method that contains.

The part experiment that mobile phase is investigated is as follows:

Sequence number mobile phase

1 methanol-0.05% glacial acetic acid aqueous solution=10: 90

2 methanol-0.1% glacial acetic acid aqueous solution=20: 80

3 methanol-1% glacial acetic acid aqueous solution=35: 65

4 acetonitriles-0.05% aqueous formic acid=10: 90

5 methanol-0.1% aqueous formic acid=20: 80

6 methanol-1% aqueous formic acid=35: 65

7 acetonitriles-0.05% phosphate aqueous solution=10: 90

8 methanol-0.1% phosphate aqueous solution=20: 80

9 methanol-1% METHAPHOSPHORIC ACID aqueous solution=35: 65

10 methanol-0.01% sodium dihydrogen phosphate=10: 90

11 methanol-0.02M sodium dihydrogen phosphate=20: 80

12 methanol-0.2M sodium dihydrogen phosphate=35: 65

13 acetonitriles-0.01% potassium dihydrogen phosphate=10: 90

14 methanol-0.02M potassium dihydrogen phosphate=20: 80

15 methanol-0.2M potassium dihydrogen phosphate=35: 65

16 acetonitriles-0.01% biphosphate amine aqueous solution=10: 90

17 methanol-0.02M biphosphate amine aqueous solution=20: 80

18 methanol-0.2M biphosphate amine aqueous solution=35: 65

19 acetonitriles-0.02M potassium dihydrogen phosphate=20: 80

20 acetonitriles-0.2M potassium dihydrogen phosphate=35: 65

21 acetonitriles-0.05M potassium dihydrogen phosphate=20: 80

22 acetonitriles-0.1M potassium dihydrogen phosphate=35: 65

23 acetonitriles-0.05M potassium dihydrogen phosphate=28: 72

By research, we are informed under the following condition can reach basic separating effect:

Mobile phase is: methanol or acetonitrile-0.1%～1% glacial acetic acid aqueous solution or 0.1%～1% aqueous formic acid or 0.1%～1% phosphate aqueous solution or 0.02mol/L～0.2mol/L sodium dihydrogen phosphate or 0.02mol/L～0.2mol/L potassium dihydrogen phosphate or 0.02mol/L～0.2mol/L biphosphate amine aqueous solution=20～35: 80～65

Through conclusive evidence, obtain best mobile phase condition, that is:

Acetonitrile: 0.05M potassium dihydrogen phosphate=28: 72

Through specificity, stability, repeatability, precision, average recovery research conclusive evidence, the said method availability is strong.

(10) assay of cimicifugoside and 5-O-methyl-visamminol in the preparation

We investigate preparation condition, the chromatographic column of sample, the equal multiple factor that flows, in the hope of finding the available survey method that contains.

By research, we are informed under the following condition can reach basic separating effect:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides, and adds 80～100% methanol or 80～100% ethanol extractions, and is adjusted to debita spissitudo, as need testing solution; Get cimicifugoside reference substance and 5-O-methyl-visamminol reference substance, make reference substance solution; Adopt liquid chromatography, chromatographic column is a filler with the alkyl silane bonded silica gel, with methanol or acetonitrile-water or 0.05%～0.1% glacial acetic acid aqueous solution or 0.05%～0.1% aqueous formic acid or 0.005%～0.01% phosphate aqueous solution=25～45: 75～55 is mobile phase, detects wavelength and be among 280～320nm; It is an amount of to draw above-mentioned test solution and contrast solution respectively, injects chromatograph of liquid, calculates with one point external standard method or standard curve method, promptly.

Through conclusive evidence, obtain best mobile phase condition, that is:

Adopt liquid chromatography, the chromatographic column octadecylsilane chemically bonded silica is a filler, is mobile phase with methanol-water=35: 65, and the detection wavelength is 292nm.

Through specificity, stability, repeatability, precision, average recovery research conclusive evidence, the said method availability is strong.

(11) assay of gastrodine in the preparation

We investigate preparation condition, the chromatographic column of sample, the equal multiple factor that flows, in the hope of finding the available survey method that contains.

By research, we are informed under the following condition can reach basic separating effect:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides, and adds 80～100% methanol or 80～100% ethanol extractions, and extracting solution is concentrated near doing, and residue dissolves with mobile phase, as need testing solution; Make reference substance solution with the gastrodine reference substance, adopt liquid chromatography, chromatographic column is a filler with the alkyl silane bonded silica gel, acetonitrile or methanol-0.05%～0.2% phosphate aqueous solution or 0.05%～0.2% glacial acetic acid aqueous solution or 0.05%～0.2% aqueous formic acid=1～3: 99～97 is mobile phase, and the detection wavelength is among 200～250nm; It is an amount of to draw above-mentioned test solution and contrast solution respectively, injects chromatograph of liquid, calculates with one point external standard method or standard curve method, promptly.

Through conclusive evidence, obtain best mobile phase condition, that is:

Adopt liquid chromatography, the chromatographic column octadecylsilane chemically bonded silica is a filler, and acetonitrile-0.1% phosphate aqueous solution=2: 98 is a mobile phase, and the detection wavelength is 220nm.

Through specificity, stability, repeatability, precision, average recovery research conclusive evidence, the said method availability is strong.

Concrete embodiment

Embodiment 1: 15.3 parts in Moschus; 30.5 parts of Calculus Boviss; 105.8 parts of natural Broneolum Syntheticums; 64.5 parts of Margaritas; 64.5 parts of Lapis Micae Aureuses; 64.5 parts of calcined Alumen; 136.4 parts of succinums; 100.1 parts in processed with salt Herba Ephedrae; 133.5 parts of Concretio Silicea Bambusaes; 166.9 parts of Radix Saposhnikoviaes; 166.9 parts of Bulbus Fritillariae Cirrhosaes; 100.1 parts of wine Bombyx Batryticatus(processed); 133.5 parts of Rhizoma Pinelliae Preparatum; 66.75 parts in Rhizoma Gastrodiae; 66.75 parts of Rhizoma Coptidis; 166.9 parts of Ramulus Uncariae Cum Uncis; 100.1 parts of Herba Menthaes; 100.1 parts of Periostracum Cicadaes; 100.1 parts of Arisaema Cum Bile; 133.5 parts of Radix Curcumaes; 100.1 parts of processed with salt Scorpios; 133.5 parts of Rhizoma Paridis

Remove seven flavor pulverize separately such as Moschus, Calculus Bovis, natural Broneolum Syntheticum, Margarita, Lapis Micae Aureus, Alumen, succinum and become fine powder, ten ground spices such as all the other Herba Ephedraes are broken into fine powder, and with fine powder bedding-in such as above-mentioned Moschus, mixing promptly gets powder.Warm water is taken after mixing with liquid.0 to 6 months children's obey half bottle at every turn, every day 1 time.6 months to 1 years old children's obey 1 bottle at every turn, every day 1 time.To 2 years old children's, obey 1 bottle, every day 2 times more than 1 year old at every turn.More than 2 years old, obey 1 bottle half, every day 2 times at every turn.

Embodiment 2: 12 parts in Moschus, 20 parts of Calculus Boviss, 80 parts of natural Broneolum Syntheticums, 50 parts of Margaritas, 50 parts of Lapis Micae Aureuses, 50 parts of calcined Alumen, 120 parts of succinums, 80 parts in processed with salt Herba Ephedrae, 120 parts of Concretio Silicea Bambusaes, 140 parts of Radix Saposhnikoviaes, 140 parts of Bulbus Fritillariae Cirrhosaes, 80 parts of wine Bombyx Batryticatus(processed), 120 parts of Rhizoma Pinelliae Preparatum, 50 parts in Rhizoma Gastrodiae, 50 parts of Rhizoma Coptidis, 140 parts of Ramulus Uncariae Cum Uncis, 80 parts of Herba Menthaes, 80 parts of Periostracum Cicadaes, 80 parts of Arisaema Cum Bile, 120 parts of Radix Curcumaes, 80 parts of processed with salt Scorpios, 120 parts of Rhizoma Paridis

Above flavour of a drug decoct with water twice, add 3 times of water gagings for the first time and decoct 1 hour, add 3 times of water gagings for the second time, decoct 1 hour, and collecting decoction filters, and concentrate, and drying is granulated, and promptly gets granule.

Embodiment 3: 20 parts in Moschus, 40 parts of Calculus Boviss, 120 parts of natural Broneolum Syntheticums, 80 parts of Margaritas, 80 parts of Lapis Micae Aureuses, 80 parts of calcined Alumen, 150 parts of succinums, 120 parts in processed with salt Herba Ephedrae, 150 parts of Concretio Silicea Bambusaes, 180 parts of Radix Saposhnikoviaes, 180 parts of Bulbus Fritillariae Cirrhosaes, 120 parts of wine Bombyx Batryticatus(processed), 150 parts of Rhizoma Pinelliae Preparatum, 80 parts in Rhizoma Gastrodiae, 80 parts of Rhizoma Coptidis, 180 parts of Ramulus Uncariae Cum Uncis, 120 parts of Herba Menthaes, 120 parts of Periostracum Cicadaes, 120 parts of Arisaema Cum Bile, 150 parts of Radix Curcumaes, 120 parts of processed with salt Scorpios, 150 parts of Rhizoma Paridis

Above flavour of a drug decoct with water twice, add 6 times of water gagings for the first time and decoct 2 hours, add 4 times of water gagings for the second time, decoct 1 hour, and collecting decoction filters, and concentrate, and drying is granulated, and is encapsulated, promptly gets capsule.

Embodiment 4: 18 parts in Moschus, 38 parts of Calculus Boviss, 115 parts of natural Broneolum Syntheticums, 75 parts of Margaritas, 76 parts of Lapis Micae Aureuses, 78 parts of calcined Alumen, 147 parts of succinums, 115 parts in processed with salt Herba Ephedrae, 145 parts of Concretio Silicea Bambusaes, 178 parts of Radix Saposhnikoviaes, 174 parts of Bulbus Fritillariae Cirrhosaes, 119 parts of wine Bombyx Batryticatus(processed), 143 parts of Rhizoma Pinelliae Preparatum, 75 parts in Rhizoma Gastrodiae, 75 parts of Rhizoma Coptidis, 170 parts of Ramulus Uncariae Cum Uncis, 115 parts of Herba Menthaes, 115 parts of Periostracum Cicadaes, 116 parts of Arisaema Cum Bile, 145 parts of Radix Curcumaes, 113 parts of processed with salt Scorpios, 140 parts of Rhizoma Paridis

Above flavour of a drug decoct with water twice, add 6 times of water gagings for the first time and decoct 1 hour, add 4 times of water gagings for the second time, decoct 1 hour, and collecting decoction filters, and concentrate, and vacuum drying is pulverized; Get CMC-Na: PVPP=1: 1 adds an amount of pigment mixing as pharmaceutical adjunct, get 2/5 pharmaceutical adjunct and the medicated powder mix homogeneously that is equivalent to 10 times of amounts of CMC-Na approximately, PVP-K30 anhydrous alcohol solution with 2% is made binding agent, 40 order system material, granulate, remain 3/5 pharmaceutical adjunct, be added on outward in the particle that makes, tabletting promptly gets dispersible tablet.

Embodiment 5: 14 parts in Moschus, 22 parts of Calculus Boviss, 85 parts of natural Broneolum Syntheticums, 54 parts of Margaritas, 51 parts of Lapis Micae Aureuses, 52 parts of calcined Alumen, 123 parts of succinums, 83 parts in processed with salt Herba Ephedrae, 124 parts of Concretio Silicea Bambusaes, 144 parts of Radix Saposhnikoviaes, 141 parts of Bulbus Fritillariae Cirrhosaes, 82 parts of wine Bombyx Batryticatus(processed), 123 parts of Rhizoma Pinelliae Preparatum, 51 parts in Rhizoma Gastrodiae, 55 parts of Rhizoma Coptidis, 145 parts of Ramulus Uncariae Cum Uncis, 85 parts of Herba Menthaes, 86 parts of Periostracum Cicadaes, 86 parts of Arisaema Cum Bile, 123 parts of Radix Curcumaes, 81 parts of processed with salt Scorpios, 122 parts of Rhizoma Paridis

Above flavour of a drug decoct with water twice, add 8 times of water gagings for the first time and decoct 1 hour, for the second time add 6 times of water gagings, decocted collecting decoction 2 hours, filter, relative density was 1.36 thick paste when filtrate decompression was concentrated into 60 ℃, vacuum drying, pulverize, cross 80 mesh sieves, press medication amount: substrate amount=1: 1.5 adding soybean oil, mixing, pill promptly gets soft capsule.

Embodiment 6: 12 parts in Moschus, 20 parts of Calculus Boviss, 80 parts of natural Broneolum Syntheticums, 50 parts of Margaritas, 50 parts of Lapis Micae Aureuses, 50 parts of Borax(calcined), 120 parts of succinums, 80 parts in processed with salt Herba Ephedrae, 120 parts of Concretio Silicea Bambusaes, 140 parts of Radix Saposhnikoviaes, 140 parts of Bulbus Fritillariae Cirrhosaes, 80 parts of wine Bombyx Batryticatus(processed), 120 parts of Rhizoma Pinelliae Preparatum, 50 parts in Rhizoma Gastrodiae, 50 parts of Rhizoma Coptidis, 140 parts of Ramulus Uncariae Cum Uncis, 80 parts of Herba Menthaes, 80 parts of Periostracum Cicadaes, 80 parts of Arisaema Cum Bile, 120 parts of Radix Curcumaes, 80 parts of processed with salt Scorpios, 120 parts of Rhizoma Paridis

Remove seven flavor pulverize separately such as Moschus, Calculus Bovis, natural Broneolum Syntheticum, Margarita, Lapis Micae Aureus, Borax, succinum and become fine powder, ten ground spices such as all the other Herba Ephedraes are broken into fine powder, and with fine powder bedding-in such as above-mentioned Moschus, mixing promptly gets powder.

Embodiment 7: 20 parts in Moschus, 40 parts of Calculus Boviss, 120 parts of natural Broneolum Syntheticums, 80 parts of Margaritas, 80 parts of Lapis Micae Aureuses, 80 parts of Borax(calcined), 150 parts of succinums, 120 parts in processed with salt Herba Ephedrae, 150 parts of Concretio Silicea Bambusaes, 180 parts of Radix Saposhnikoviaes, 180 parts of Bulbus Fritillariae Cirrhosaes, 120 parts of wine Bombyx Batryticatus(processed), 150 parts of Rhizoma Pinelliae Preparatum, 80 parts in Rhizoma Gastrodiae, 80 parts of Rhizoma Coptidis, 180 parts of Ramulus Uncariae Cum Uncis, 120 parts of Herba Menthaes, 120 parts of Periostracum Cicadaes, 120 parts of Arisaema Cum Bile, 150 parts of Radix Curcumaes, 120 parts of processed with salt Scorpios, 150 parts of Rhizoma Paridis

Remove seven flavor pulverize separately such as Moschus, Calculus Bovis, natural Broneolum Syntheticum, Margarita, Lapis Micae Aureus, Borax, succinum and become fine powder, ten ground spices such as all the other Herba Ephedraes are broken into fine powder, and with fine powder bedding-in such as above-mentioned Moschus, mixing promptly gets powder.

Embodiment 8: 15.3 parts in Moschus; 30.5 parts of Calculus Boviss; 105.8 parts of natural Broneolum Syntheticums; 64.5 parts of Margaritas; 64.5 parts of Lapis Micae Aureuses; 64.5 parts of Borax(calcined); 136.4 parts of succinums; 100.1 parts in processed with salt Herba Ephedrae; 133.5 parts of Concretio Silicea Bambusaes; 166.9 parts of Radix Saposhnikoviaes; 166.9 parts of Bulbus Fritillariae Cirrhosaes; 100.1 parts of wine Bombyx Batryticatus(processed); 133.5 parts of Rhizoma Pinelliae Preparatum; 66.75 parts in Rhizoma Gastrodiae; 66.75 parts of Rhizoma Coptidis; 166.9 parts of Ramulus Uncariae Cum Uncis; 100.1 parts of Herba Menthaes; 100.1 parts of Periostracum Cicadaes; 100.1 parts of Arisaema Cum Bile; 133.5 parts of Radix Curcumaes; 100.1 parts of processed with salt Scorpios; 133.5 parts of Rhizoma Paridis

Remove seven flavor pulverize separately such as Moschus, Calculus Bovis, natural Broneolum Syntheticum, Margarita, Lapis Micae Aureus, Borax, succinum and become fine powder, ten ground spices such as all the other Herba Ephedraes are broken into fine powder, and with fine powder bedding-in such as above-mentioned Moschus, mixing promptly gets powder.

The microscopical identification method of part medical material in embodiment 9 preparations:

Get this product, put microscopically and observe, the wide avette or shell-like of starch grain, diameter 40～60um, the short seam of omphalion shape, herringbone shape or horse-hof shape, laminated striation can be examined and see (Bulbus Fritillariae Cirrhosae).Has fine crystals (Herba Ephedrae) on the fiber.Oil pipe contains golden yellow secretions (Radix Saposhnikoviae).The stone cell foresythia is that similar round, rectangle, class are square, class triangle or class ellipse (Rhizoma Coptidis).The body wall fragment is faint yellow to have reticular texture and circular trichopore to yellow, visible sometimes sepia bristle (Scorpio).The body wall fragment is colourless, and there is superfine mycelium (Bombyx Batryticatus) on the surface.Amorphous agglomerate is fallow, is embedded with tiny square crystallization (Moschus).Irregular fragment pistac or pale brown color, transparent or semitransparent (succinum).Colourless or the light green of irregular fragment, translucent, glossy, visible sometimes fine and closely woven wavy grain (Margarita).Irregular fragment is golden yellow or orange-yellow, glossy, for a long time postpone virescence (Calculus Bovis).

The thin layer chromatography discrimination method of Rhizoma Coptidis, berberine hydrochloride in embodiment 10 preparations:

Get this product 0.3g, add ethanol 5ml, supersound process 10 minutes filters, and filtrate is as need testing solution.Other gets Rhizoma Coptidis control medicinal material 0.1g, shines medical material solution in pairs with legal system.Get the berberine hydrochloride reference substance again, add methanol and make solution that every ml contains 0.5mg product solution in contrast.Test according to thin layer chromatography, draw need testing solution 2ul, each 1ul of control medicinal material and reference substance solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-methanol-isopropyl alcohol-water (6: 3: 2: 1.5: 0.3), puts in the chromatography cylinder of ammonia saturated with vapor, presaturation launched after 15 minutes, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

The gas chromatogram discrimination method of embodiment 11 preparation natural Broneolum Syntheticums, Herba Menthae:

Get this product 1g, add ethanol 5ml, ultrasonic (ice bath) 10 minutes filters, and filtrate is as need testing solution.Other gets natural Broneolum Syntheticum, Mentholum reference substance, adds ethanol and makes the solution that every 1ml contains 1mg respectively, as natural Broneolum Syntheticum, Mentholum reference substance solution.According to gas chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 E) test, be the capillary column of filler with the Polyethylene Glycol, heating schedule is: rise to 130 ℃ with the heating rate of 10 ℃/min from 80 ℃, rise to 180 ℃ with the heating rate of 20 ℃/min.Precision is measured need testing solution and each 1ul of reference substance solution respectively, inject gas chromatograph, and the test sample chromatograph should detect and natural Broneolum Syntheticum, chromatographic peak that Mentholum reference substance chromatographic retention is identical.

The thin layer chromatography discrimination method of ephedrine hydrochloride in embodiment 12 preparations:

Get this product 2g, add strong ammonia solution 1ml and dichloromethane 20ml, close plug, supersound process 20 minutes is put coldly, filters, and filtrate evaporate to dryness, the residue 1ml that adds methylene chloride makes dissolving, as need testing solution.Other gets the ephedrine hydrochloride reference substance, adds methylene chloride to make the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol-glacial acetic acid-water (8: 2: 1) is developing solvent, launch, take out, dry, spray is with ninhydrin solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

The thin layer chromatography discrimination method of Radix Saposhnikoviae in embodiment 13 preparations:

Get this product 1.5g, add chloroform 20ml, liquor ammoniae fortis 1ml, reflux 1 hour filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Saposhnikoviae control medicinal material 0.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B), draw need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, (2: 3: 4: 0.2) be developing solvent, expansion was taken out with benzene-acetone-ethyl acetate-liquor ammoniae fortis, dry, spray is put about 5 minutes of 105 ℃ of heating with 10% ethanol solution of sulfuric acid, puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

The thin layer chromatography discrimination method of Bulbus Fritillariae Cirrhosae in embodiment 14 preparations:

Get this product 10g, add ammonia solution 10ml and chloroform 30ml, reflux 1 hour, put coldly, filter, filtrate is extracted 2 times with the jolting of 0.1mol/L hydrochloric acid solution, each 20ml merges hydrochloric acid solution, adds strong ammonia solution and regulates pH value to 10, extract 2 times with the chloroform jolting, each 20ml merges chloroform liquid, evaporate to dryness, residue adds ethanol 0.5ml makes dissolving, as need testing solution.Other gets Bulbus Fritillariae Cirrhosae control medicinal material 2g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (8: 8: 3: 2) lower floor's solution of placing below 10 ℃ was developing solvent with chloroform-ethyl acetate-methanol-water, launch, take out, dry, spray successively with rare bismuth potassium iodide test solution and sodium nitrite ethanol test solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

The thin layer chromatography discrimination method of Rhizoma Paridis, Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII in embodiment 14 preparations:

Get this product 4g, add ethanol 50ml, reflux 30 minutes filters the filtrate evaporate to dryness, water 10ml dissolving is put in the separatory funnel, extracts with n-butyl alcohol 10ml jolting, gets n-butyl alcohol liquid, water 5ml washing, n-butyl alcohol liquid is put evaporate to dryness in the water-bath, and residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Rhizoma Paridis control medicinal material 0.5g, shines medical material solution in pairs with legal system.Get Rhizoma Paridis saponin VI reference substance, Rhizoma Paridis saponin VII reference substance again, add methanol and make the mixed solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B), draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform-ethyl acetate-methanol-water (5: 4: 3: 0.6) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃.Put respectively under daylight and the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle and the fluorescence speckle of same color.

The thin layer chromatography discrimination method of Calculus Bovis, cholic acid and deoxycholic acid in embodiment 16 preparations:

Get this product 1.5g, add ethanol 50ml, supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Calculus Bovis control medicinal material 0.02g, shines medical material solution in pairs with legal system; Get the cholic acid reference substance again, the deoxycholic acid reference substance adds methanol and makes the mixed solution that every 1ml contains 0.5mg, product solution in contrast.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2010 B), draw each 5 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-glacial acetic acid-water (10: 10: 0.8) is developing solvent, launch, take out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃.Put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.

The content assaying method of berberine hydrochloride in embodiment 17 preparations:

Precision takes by weighing the about 1g of this product, puts in the tool plug conical flask, and precision adds 2% hydrochloric acid-methanol (1: 1) 50ml, and supersound process is 30 minutes behind the shake well, puts coldly, supplies weightlessness, leaves standstill, and gets supernatant and crosses the 0.45um filter membrane, as need testing solution; Methanol solution with the berberine hydrochloride reference substance is contrast, adopts liquid chromatography, and the chromatographic column octadecylsilane chemically bonded silica is a filler, and acetonitrile-0.05M potassium dihydrogen phosphate (28: 72) is a mobile phase, and the detection wavelength is 350nm; Accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects chromatograph of liquid, measures; Calculate with one point external standard method, the every gram of this product contains Rhizoma Coptidis in berberine hydrochloride, must not be less than 1mg.

The content assaying method of cimicifugoside reference substance and 5-O-methyl-visamminol in embodiment 18 preparations:

Precision takes by weighing the about 3g of this product, accurate claims surely, puts in the tool plug conical flask, and the accurate methanol 50ml that adds claims decide weight, and water-bath refluxed 2 hours, puts coldly, claims to decide weight again, supplies the weight that subtracts mistake with methanol, shakes up, and filtration is got subsequent filtrate, as need testing solution; Methanol solution with cimicifugoside reference substance and 5-O-methyl-visamminol reference substance is contrast, adopts liquid chromatography, and the chromatographic column octadecylsilane chemically bonded silica is a filler, and methanol-water (35: 65) is a mobile phase, and the detection wavelength is 292nm; Accurate respectively reference substance solution and each 10ul of need testing solution of drawing injects chromatograph of liquid, measures; Calculate with one point external standard method, the every gram of this product contains the total amount of Radix Saposhnikoviae in cimicifugoside and 5-O-methyl-visamminol, must not be less than 0.1mg.

The content assaying method of gastrodine in embodiment 19 preparations:

Precision takes by weighing the about 5g of this product, and accurate the title decides, and puts in the tool plug conical flask, the accurate methanol 25ml that adds, close plug claims to decide weight, and supersound process 50 minutes is taken out, put coldly, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter accurate subsequent filtrate 10ml, the evaporate to dryness drawn, residue also quantitatively is transferred in the 10ml measuring bottle with the mobile phase dissolving, is settled to scale with mobile phase, shakes up, filter, get subsequent filtrate, as need testing solution; It is an amount of that precision takes by weighing the gastrodine reference substance, adds mobile phase and make reference substance solution, adopts liquid chromatography, and the chromatographic column octadecylsilane chemically bonded silica is a filler, and acetonitrile-0.1% phosphoric acid solution (2: 98) is a mobile phase, and the detection wavelength is 220nm; Accurate respectively reference substance solution and each 20ul of need testing solution of drawing injects chromatograph of liquid, measures; Calculate with one point external standard method, the every gram of this product contains Rhizoma Gastrodiae in gastrodine, must not be less than 0.03mg.

Claims (10)

1. Chinese medicine composition for the treatment of infantile common cold, it is characterized in that: it is made up of following raw materials according: Moschus 12-20 part; Calculus Bovis 20-40 part; natural Broneolum Syntheticum 80-120 part; Margarita 50-80 part; Lapis Micae Aureus 50-80 part; calcined Alumen 50-80 part; succinum 120-150 part; processed with salt Herba Ephedrae 80-120 part; Concretio Silicea Bambusae 120-150 part; Radix Saposhnikoviae 140-180 part; Bulbus Fritillariae Cirrhosae 140-180 part; wine Bombyx Batryticatus(processed) 80-120 part; Rhizoma Pinelliae Preparatum 120-150 part; Rhizoma Gastrodiae 50-80 part; Rhizoma Coptidis 50-80 part; Ramulus Uncariae Cum Uncis 140-180 part; Herba Menthae 80-120 part; Periostracum Cicadae 80-120 part; Arisaema Cum Bile 80-120 part; Radix Curcumae 120-150 part; processed with salt Scorpio 80-120 part; Rhizoma Paridis 120-150 part.

2. according to the Chinese medicine composition of the described treatment infantile common cold of claim 1, it is characterized in that: it is made up of following raw materials according: 15.3 parts in Moschus; 30.5 parts of Calculus Boviss; 105.8 parts of natural Broneolum Syntheticums; 64.5 parts of Margaritas; 64.5 parts of Lapis Micae Aureuses; 64.5 parts of calcined Alumen; 136.4 parts of succinums; 100.1 parts in processed with salt Herba Ephedrae; 133.5 parts of Concretio Silicea Bambusaes; 166.9 parts of Radix Saposhnikoviaes; 166.9 parts of Bulbus Fritillariae Cirrhosaes; 100.1 parts of wine Bombyx Batryticatus(processed); 133.5 parts of Rhizoma Pinelliae Preparatum; 66.75 parts in Rhizoma Gastrodiae; 66.75 parts of Rhizoma Coptidis; 166.9 parts of Ramulus Uncariae Cum Uncis; 100.1 parts of Herba Menthaes; 100.1 parts of Periostracum Cicadaes; 100.1 parts of Arisaema Cum Bile; 133.5 parts of Radix Curcumaes; 100.1 parts of processed with salt Scorpios; 133.5 parts of Rhizoma Paridis.

3. according to the Chinese medicine composition of claim 1 or 2 described treatment infantile common colds, it is characterized in that: in the described raw material, calcined Alumen can also be a Borax(calcined).

4. according to the preparation method of the Chinese medicine composition of claim 1,2 or 3 described treatment infantile common colds, it is characterized in that: the raw material of getting it filled, make multiple peroral dosage form respectively, comprising: tablet, dispersible tablet, capsule, soft capsule, granule, pill, powder, drop pill, gel, oral liquid.

5. according to the preparation method of the Chinese medicine composition of the described treatment infantile common cold of claim 4; it is characterized in that: except that Moschus, Calculus Bovis, natural Broneolum Syntheticum, Margarita, Lapis Micae Aureus, Alumen, succinum seven flavor pulverize separately become fine powder; all the other ten ground spices are broken into fine powder; with fine powder bedding-ins such as above-mentioned Moschus; mixing; that is, promptly get powder.

6. according to the detection method of the Chinese medicine composition of claim 1,2 or 3 described treatment infantile common colds, it is characterized in that: this method comprises following all or part of content:

(1) all or part of microscopical identification method of testing in Bulbus Fritillariae Cirrhosae medical material, Herba Ephedrae medical material, Radix Saposhnikoviae medical material, Rhizoma Coptidis medical material, Scorpio medical material, Bombyx Batryticatus medical material, Moschus medical material, succinum medical material, Margarita medical material, the Calculus Bovis medical material;

(2) all or part of thin layer, gas chromatogram differential test method in Calculus Bovis medical material, natural Broneolum Syntheticum, Radix Saposhnikoviae medical material, Bulbus Fritillariae Cirrhosae medical material, Rhizoma Coptidis medical material, Herba Menthae medical material, Rhizoma Paridis medical material, berberine hydrochloride, ephedrine hydrochloride, Rhizoma Paridis saponin VI, Rhizoma Paridis saponin VII, cholic acid, the deoxycholic acid;

(3) content assaying method of all or part of composition in berberine hydrochloride, gastrodine, cimicifugoside and the 5-O-methyl-visamminol.

7. according to the detection method of the compound Chinese medicinal preparation of the described treatment infantile common cold of claim 6, it is characterized in that: described discrimination method comprises following all or part of content:

A, microscopical identification method:

Get this product, put microscopically and observe, the wide avette or shell-like of starch grain, diameter 40～60um, the short seam of omphalion shape, herringbone shape or horse-hof shape, laminated striation can be examined and see; Has fine crystals on the fiber; Oil pipe contains golden yellow secretions; The stone cell foresythia is that similar round, rectangle, class are square, class triangle or class ellipse; The body wall fragment is faint yellow to have reticular texture and circular trichopore to yellow, visible sometimes sepia bristle; The body wall fragment is colourless, and there is superfine mycelium on the surface; Amorphous agglomerate is fallow, is embedded with tiny square crystallization; Irregular fragment pistac or pale brown color, transparent or semitransparent; Colourless or the light green of irregular fragment, translucent, glossy, visible sometimes fine and closely woven wavy grain; Irregular fragment is golden yellow or orange-yellow, glossy, for a long time the postpone virescence;

The thin layer chromatography discrimination method of b, Rhizoma Coptidis, berberine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol are an amount of, extracts, and is adjusted to debita spissitudo, as need testing solution; Other gets the Rhizoma Coptidis control medicinal material, shines medical material solution in pairs with legal system; Get the berberine hydrochloride reference substance again, make reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with toluene or benzene-Ethyl formate or ethyl acetate-methanol or ethanol-isopropyl alcohol-water=2～10: 1～5: 1～4: 0.5～3: 0.1～0.5 solution is developing solvent, put in the chromatography cylinder of ammonia saturated with vapor, launch after the presaturation, take out, dry, put under the ultra-violet lamp 365nm and inspect, in the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;

The gas chromatogram discrimination method of c, natural Broneolum Syntheticum, Herba Menthae:

Get living spectrometer to be measured, in the test sample chromatograph, with the reference substance chromatograph consistent chromatographic peak of time of withing a hook at the end; It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol extractions, filters, and filtrate is as need testing solution; Other gets natural Broneolum Syntheticum, Mentholum reference substance, makes reference substance solution, according to the gas chromatography test among an appendix VI of Chinese Pharmacopoeia version in 2010 E, adopts capillary column, and heating schedule is: rise to 250 ℃ from 40 ℃; Precision is measured need testing solution and reference substance solution is an amount of respectively, inject gas chromatograph, and the test sample chromatograph should detect and natural Broneolum Syntheticum, chromatographic peak that Mentholum reference substance chromatographic retention is identical;

The thin layer chromatography discrimination method of d, ephedrine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds alkaline solution and chloroform or dichloromethane or ethyl acetate extraction, as need testing solution; Other gets the ephedrine hydrochloride reference substance and makes reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned contrast solution and test solution respectively, puts in same silica gel thin-layer plate, and with n-butyl alcohol-formic acid or glacial acetic acid-water=2～15: be developing solvent at 0.2～5: 0.1～2, launch, take out, dry, spray is with ninhydrin solution, it is clear to be heated to the speckle colour developing, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

The thin layer chromatography discrimination method of e, Radix Saposhnikoviae:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds chloroform or dichloromethane or acetic acid ethyl ester and alkaline solution and extracts, and be adjusted to debita spissitudo, as need testing solution; Other gets the Radix Saposhnikoviae control medicinal material and makes control medicinal material solution; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned contrast solution and test solution respectively, puts in same silica gel thin-layer plate, with benzene or toluene-acetone-ethyl acetate or Ethyl formate-liquor ammoniae fortis=0.5～5: be developing solvent at 1～5: 2～6: 0.05～0.5, launch, take out, dry, spray is with vitriolated solution, heat after several minutes, put under the ultra-violet lamp 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

The thin layer chromatography discrimination method of f, Bulbus Fritillariae Cirrhosae:

It is an amount of to get compound Chinese medicinal preparation to be measured, add alkaline test solution and chloroform or dichloromethane or ethyl acetate extraction, filter, filtrate is extracted with hydrochloric acid solution, merges hydrochloric acid solution, regulate pH value to alkalescence, use chloroform extraction, complete and chloroform liquid, evaporate to dryness, residue adds ethanol or dissolve with methanol, as need testing solution; Other gets the Bulbus Fritillariae Cirrhosae control medicinal material and makes control medicinal material solution; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned test solution and contrast solution respectively, puts on same silica gel thin-layer plate, and with chloroform or dichloromethane-ethyl acetate or Ethyl formate-methanol or alcohol-water=4～12: 5～12: 1～5: 0.5～4 solution or lower floor's solution are developing solvent, launch, take out, dry, spray is to contain the solution of rare bismuth potassium iodide and sodium nitrite, inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the same color speckle;

The thin layer chromatography discrimination method of one or both of g, Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII, Rhizoma Paridis:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol extractions, filters, and the filtrate evaporate to dryness is used water dissolution, and the reuse n-butanol extraction is got n-butyl alcohol liquid, washes the back evaporate to dryness with water, and residue adds methanol or dissolve with ethanol, as need testing solution; Other gets the Rhizoma Paridis control medicinal material, makes control medicinal material solution with reference to the method for making of need testing solution; One or both that get Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII reference substance are again made mixed solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with chloroform or dichloromethane-ethyl acetate or Ethyl formate-methanol or alcohol-water=2～10: be developing solvent at 1～8: 1～6: 0.1～1, launch, take out, dry, spray is with vitriolated developer, be heated to clear spot, put respectively under daylight and the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle and the fluorescence speckle of same color;

The thin layer chromatography discrimination method of one or both of h, cholic acid and deoxycholic acid, Calculus Bovis:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds 50～100% methanol or 50～100% ethanol extractions, and is adjusted to debita spissitudo, as need testing solution; Get the Calculus Bovis control medicinal material, make control medicinal material solution with reference to the need testing solution method for making; Get in cholic acid, the deoxycholic acid one or both, make reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with toluene or benzene-formic acid or glacial acetic acid-water=5～15: be developing solvent at 5～15: 0.3～2, launches, and takes out, dry, spray is heated to clear spot with vitriolated developer, puts under the ultra-violet lamp 365nm and inspects; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the same color speckle.

8. according to the detection method of the compound Chinese medicinal preparation of the described treatment infantile common cold of claim 7, it is characterized in that: described discrimination method comprises following all or part of content:

A, microscopical identification method:

Get this product, put microscopically and observe, the wide avette or shell-like of starch grain, diameter 40～60um, the short seam of omphalion shape, herringbone shape or horse-hof shape, laminated striation can be examined and see; Has fine crystals on the fiber; Oil pipe contains golden yellow secretions; The stone cell foresythia is that similar round, rectangle, class are square, class triangle or class ellipse; The body wall fragment is faint yellow to have reticular texture and circular trichopore to yellow, visible sometimes sepia bristle; The body wall fragment is colourless, and there is superfine mycelium on the surface; Amorphous agglomerate is fallow, is embedded with tiny square crystallization; Irregular fragment pistac or pale brown color, transparent or semitransparent; Colourless or the light green of irregular fragment, translucent, glossy, visible sometimes fine and closely woven wavy grain; Irregular fragment is golden yellow or orange-yellow, glossy, for a long time the postpone virescence;

The thin layer chromatography discrimination method of b, Rhizoma Coptidis, berberine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filters, and filtrate is as need testing solution; Other gets the Rhizoma Coptidis control medicinal material, shines medical material solution in pairs with legal system; Getting berberine hydrochloride again adds methanol and makes reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, puts on same silica gel thin-layer plate, and with toluene-ethyl acetate-methanol-isopropyl alcohol-water=6: 3: 2: be developing solvent at 1.5: 0.3, put in the chromatography cylinder of ammonia saturated with vapor, launch after the presaturation, take out, dry, put under the ultra-violet lamp 365nm and inspect, in the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;

The gas chromatogram discrimination method of c, natural Broneolum Syntheticum, Herba Menthae:

Get living spectrometer to be measured, in the test sample chromatograph, with the reference substance chromatograph consistent chromatographic peak of time of withing a hook at the end; It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filters, and filtrate is as need testing solution; Other gets natural Broneolum Syntheticum, Mentholum reference substance, add ethanol and make reference substance solution respectively, test according to the gas chromatography among an appendix VI of Chinese Pharmacopoeia version in 2010 E, with the Polyethylene Glycol is the capillary column of filler, heating schedule is: the heating rate with 10 ℃/min rises to 130 ℃ from 80 ℃, heating rate with 20 ℃/min rises to 180 ℃, precision is measured need testing solution and reference substance solution is an amount of respectively, inject gas chromatograph, test sample chromatograph should detect and natural Broneolum Syntheticum, chromatographic peak that Mentholum reference substance chromatographic retention is identical;

The thin layer chromatography discrimination method of d, ephedrine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds liquor ammoniae fortis and dichloromethane extraction, filters, and filtrate evaporate to dryness, the residue 1ml that adds methylene chloride makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methylene chloride to make reference substance solution; Employing thin layer chromatography test, it is an amount of to draw above-mentioned contrast solution and test solution respectively, put in same silica gel thin-layer plate, be developing solvent with n-butyl alcohol-glacial acetic acid-water=8: 2: 1, launch, take out, dry, spray is with ninhydrin solution, be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

The thin layer chromatography discrimination method of e, Radix Saposhnikoviae:

It is an amount of to get compound Chinese medicinal preparation to be measured, and add chloroform and liquor ammoniae fortis and extract, the filtrate evaporate to dryness, residue adds dissolve with methanol, as need testing solution; Other gets the Radix Saposhnikoviae control medicinal material and shines medical material solution in pairs with legal system; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned contrast solution and test solution respectively, point is in same silica gel thin-layer plate, with benzene-acetone-ethyl acetate-liquor ammoniae fortis=2: 3: 4: 0.2 was developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing, puts under the ultra-violet lamp 365nm and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

The thin layer chromatography discrimination method of f, Bulbus Fritillariae Cirrhosae:

It is an amount of to get compound Chinese medicinal preparation to be measured, add ammonia solution and chloroform extraction, filter, filtrate is extracted with the jolting of 0.1mol/L hydrochloric acid solution, merges hydrochloric acid solution, add strong ammonia solution and regulate pH value to 10, extract with the chloroform jolting, merge chloroform liquid, evaporate to dryness, residue adds dissolve with ethanol, as need testing solution; Other gets the Bulbus Fritillariae Cirrhosae control medicinal material and shines medical material solution in pairs with legal system; The test of employing thin layer chromatography, it is an amount of to draw above-mentioned test solution and contrast solution respectively, point is on same silica gel thin-layer plate, with chloroform-ethyl acetate-methanol-water=8: 8: 3: lower floor's solution of 2 was developing solvent, launch, take out, dry, spray successively with rare bismuth potassium iodide test solution and sodium nitrite ethanol test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;

The thin layer chromatography discrimination method of one or both of g, Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII, Rhizoma Paridis:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filters, and the filtrate evaporate to dryness is used water dissolution, puts in the separatory funnel, extracts with n-butyl alcohol liquid, gets n-butyl alcohol liquid, washes with water, and n-butyl alcohol liquid is put evaporate to dryness in the water-bath, and residue adds dissolve with methanol, as need testing solution; Other gets the Rhizoma Paridis control medicinal material, makes control medicinal material solution with reference to the method for making of need testing solution; One or both that get Rhizoma Paridis saponin VI and Rhizoma Paridis saponin VII reference substance again add methanol and make mixed solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with chloroform-ethyl acetate-methanol-water=5: 4: 3: 0.6 was developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing, puts respectively under daylight and the ultra-violet lamp 365nm and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle and the fluorescence speckle of same color;

The thin layer chromatography discrimination method of one or both of h, cholic acid and deoxycholic acid, Calculus Bovis:

It is an amount of to get compound Chinese medicinal preparation to be measured, adds ethanol extraction, filter, and the filtrate evaporate to dryness, residue adds dissolve with methanol, as need testing solution; Get the Calculus Bovis control medicinal material, make control medicinal material solution with reference to the need testing solution method for making; Get one or both of cholic acid, deoxycholic acid, add methanol and make reference substance solution; The test of employing thin layer chromatography, it is an amount of to draw in above-mentioned test solution and the contrast solution one or more respectively, point is on same silica gel thin-layer plate, with toluene-glacial acetic acid-water=10: 10: 0.8 was developing solvent, launched, and took out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing, puts under the ultra-violet lamp 365nm and inspects; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the same color speckle.

9. according to the detection method of the compound Chinese medicinal preparation of the described treatment infantile common cold of claim 6, it is characterized in that: described content assaying method should comprise following all or part of content:

The content assaying method of a, berberine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides, and adds acidic methanol solution and extracts, and extracting solution is as need testing solution; With the berberine hydrochloride reference substance, make reference substance solution, adopt liquid chromatography, chromatographic column is a filler with the alkyl silane bonded silica gel, with methanol or acetonitrile-0.1%～1% glacial acetic acid aqueous solution or 0.1%～1% aqueous formic acid or 0.1%～1% phosphate aqueous solution or 0.02mol/L～0.2mol/L sodium dihydrogen phosphate or 0.02mol/L～0.2mol/L potassium dihydrogen phosphate or 0.02mol/L～0.2mol/L biphosphate amine aqueous solution=20～35: 80～65 is mobile phase, detects wavelength and be among 330～370nm; Accurate respectively above-mentioned test solution of absorption and contrast solution are an amount of, inject chromatograph of liquid, calculate with one point external standard method or standard curve method, and the hydrochloric berberine of the every gram of preparation must not be less than 0.5mg;

The content assaying method of b, cimicifugoside and 5-O-methyl-visamminol:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides, and adds 80～100% methanol or 80～100% ethanol extractions, and is adjusted to debita spissitudo, as need testing solution; Get cimicifugoside reference substance and 5-O-methyl-visamminol reference substance, make reference substance solution; Adopt liquid chromatography, chromatographic column is a filler with the alkyl silane bonded silica gel, with methanol or acetonitrile-water or 0.05%～0.1% glacial acetic acid aqueous solution or 0.05%～0.1% aqueous formic acid or 0.005%～0.01% phosphate aqueous solution=25～45: 75～55 is mobile phase, detects wavelength and be among 280～320nm; It is an amount of to draw above-mentioned test solution and contrast solution respectively, injects chromatograph of liquid, calculates with one point external standard method or standard curve method, and the total amount that the every gram of preparation contains cimicifugoside and 5-O-methyl-visamminol must not be less than 0.05mg;

The content assaying method of c, gastrodine:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides, and adds 80～100% methanol or 80～100% ethanol extractions, and extracting solution is concentrated near doing, and residue dissolves with mobile phase, as need testing solution; Make reference substance solution with the gastrodine reference substance, adopt liquid chromatography, chromatographic column is a filler with the alkyl silane bonded silica gel, acetonitrile or methanol-0.05%～0.2% phosphate aqueous solution or 0.05%～0.2% glacial acetic acid aqueous solution or 0.05%～0.2% aqueous formic acid=1～3: 99～97 is mobile phase, and the detection wavelength is among 200～250nm; It is an amount of to draw above-mentioned test solution and contrast solution respectively, injects chromatograph of liquid, calculates with one point external standard method or standard curve method, and the every gram of preparation contains gastrodine must not be less than 0.015mg.

10. according to the detection method of the compound Chinese medicinal preparation of the described treatment infantile common cold of claim 9, it is characterized in that: described content assaying method comprises following all or part of content:

The content assaying method of a, berberine hydrochloride:

It is an amount of to get compound Chinese medicinal preparation to be measured, and the 2% hydrochloric acid-methanol mixed solution that adds by preparation in 1: 1 extracts, the extracting solution evaporate to dryness, and extracting solution is as need testing solution; Methanol solution with berberine hydrochloride is made reference substance solution, adopts liquid chromatography, and the chromatographic column octadecylsilane chemically bonded silica is a filler, is mobile phase with acetonitrile-0.05mol/L potassium dihydrogen phosphate=28: 72, and the detection wavelength is 350nm; Accurate respectively above-mentioned test solution of absorption and contrast solution are an amount of, inject chromatograph of liquid, calculate with one point external standard method, and the hydrochloric berberine of the every gram of preparation must not be less than 1mg;

The liquid chromatograph content assaying method of b, cimicifugoside and 5-O-methyl-visamminol:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides, methanol extraction, and be adjusted to debita spissitudo, as need testing solution; Get the cimicifugoside reference substance and the 5-O-methyl-visamminol reference substance is made reference substance solution with methanol; Adopt liquid chromatography, the chromatographic column octadecylsilane chemically bonded silica is a filler, is mobile phase with methanol-water=35: 65, and the detection wavelength is 292nm; It is an amount of to draw above-mentioned test solution and contrast solution respectively, injects chromatograph of liquid, calculates with one point external standard method, and the total amount that the every gram of preparation contains cimicifugoside and 5-O-methyl-visamminol must not be less than 0.1mg;

The content assaying method of c, gastrodine:

It is an amount of to get compound Chinese medicinal preparation to be measured, and accurate the title decides or measure, and adds methanol extraction, and extracting solution is concentrated near doing, and residue dissolves with mobile phase, as need testing solution; Get the gastrodine reference substance and make reference substance solution with mobile phase; Adopt liquid chromatography, the chromatographic column octadecylsilane chemically bonded silica is a filler, and acetonitrile-0.1% phosphate aqueous solution=2: 98 is a mobile phase, and the detection wavelength is 220nm; It is an amount of to draw above-mentioned test solution and contrast solution respectively, injects chromatograph of liquid, calculates with one point external standard method, and the every gram of preparation contains gastrodine must not be less than 0.03mg.