CN1857424A

CN1857424A - Compound Chinese medicine preparation and its preparing process and quality control method

Info

Publication number: CN1857424A
Application number: CN 200510068017
Authority: CN
Inventors: 张友生; 张思宁
Original assignee: Individual
Current assignee: Individual
Priority date: 2005-04-30
Filing date: 2005-04-30
Publication date: 2006-11-08
Anticipated expiration: 2025-04-30
Also published as: CN100464186C

Abstract

The present invention discloses a kind of compound Chinese medicine capsule for treating acute gastroenteritis and its preparation process and quality control method. The compound Chinese medicine capsule is prepared with amplexicaul jasmine leaf, Chinese knotweed, plantain, holly bark and pomegranate rind and through specific technological process. The quality control method has increased thin-layer chromatography analysis of amplexicaul jasmine leaf and holly bark, increased flavonid content measurement and no test reaction.

Description

A kind of compound Chinese medicinal preparation and preparation method thereof, method of quality control

Technical field

The present invention relates to a kind of compound Chinese medicinal preparation, particularly relate to a kind of Chinese medicine compound capsule for the treatment of acute gastroenteritis and preparation method thereof, method of quality control.

Background technology

Acute gastroenteritis belongs to the traditional Chinese medical science " vomiting " category of " having loose bowels ", is common clinical, frequently-occurring disease.Commercially available fukean tablet is pure Chinese herbal and crude drugs preparations at present, with the Cortex Ilicis Rotundae heat-clearing and toxic substances removing, and the dampness removing pain relieving, Herba Oxalidis strictae, Herb Polygoni Chinensis's clearing away heat-damp and promoting diuresis are principal agent altogether; The Herba Plantaginis promoting diuresis to eliminate damp pathogen, tonneau urine is accessory drugs; The Pericarpium Granati convergence is astringent or styptic treatment for spontaneous sweating to be adjuvant drug, all medicines share, play the merit of heat-clearing and toxic substances removing, promoting diuresis to eliminate damp pathogen, convergence pain relieving altogether, be used for acute gastroenteritis, the caused stomachache of dyspepsia, diseases such as diarrhoea, vomiting, belching and acid regurgitation, thick fur are greasy, better curative effect is arranged, but because existing market has only a kind of dosage form of tablet, dosage form is single, can not satisfy different patients' needs, therefore develop a kind of new dosage form and seemed that it is necessary compeling.Differentiate that (1), (2) item are the non-exclusive reaction and record in the fukean tablet quality standard of the 11 in " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation, Pericarpium Granati and Herb Polygoni Chinensis are all contained the gallic acid composition, Cortex Ilicis Rotundae contains the ligustrin composition, but lacks reference substance, fails to carry out quantitative study; Medical materials such as Herba Oxalidis strictae, Herb Polygoni Chinensis, Herba Plantaginis find no the quality control that known reference substance can be used for carrying out this product at present.Therefore, be necessary further to improve and the control criterion that improves the quality.

Summary of the invention

The object of the invention is to provide a kind of Chinese medicine compound capsule of new treatment acute gastroenteritis; The object of the invention also is to provide a kind of preparation method of Chinese medicine compound capsule of acute gastroenteritis; The object of the invention also is to provide a kind of method of quality control for the treatment of the Chinese medicine compound capsule of acute gastroenteritis.

The present invention seeks to be achieved through the following technical solutions.

Chinese medicine compound capsule of the present invention is that the crude drug by following weight ratio is prepared from:

Herba Oxalidis strictae 165-245 weight portion, Herb Polygoni Chinensis 165-245 weight portion, Herba Plantaginis 50-80 weight portion, Cortex Ilicis Rotundae 105-165 weight portion, Pericarpium Granati 50-80 weight portion.

The preferential proportioning of above-mentioned raw materials medicine is:

Herba Oxalidis strictae 200 weight portions, Herb Polygoni Chinensis's 200 weight portions, Herba Plantaginis 66 weight portions, Cortex Ilicis Rotundae 134 weight portions, Pericarpium Granati 66 weight portions.

Chinese medicine compound capsule of the present invention is prepared by following method:

Above five tastes crude drug decocts with water 2-3 time, adds 10-12 times of water gaging at every turn, each 2 hours, collecting decoction filtered, it is 1.08～1.10 that filtrate is concentrated into 85～90 ℃ of relative densities, adds ethanol and makes and contain the alcohol amount and reach 65%, leaves standstill, filter, residue with 65% washing with alcohol once leaves standstill, filter, merge secondary filtrate, reclaim ethanol, be condensed into thick paste, cold drying is pulverized, and adds starch, carboxymethyl starch sodium is an amount of, make granule with 70% ethanol, drying, the adding magnesium stearate is an amount of, mixing, adorn capsule No. 2, promptly get Chinese medicine compound capsule of the present invention.

The method of quality control of Chinese medicine compound capsule of the present invention comprises one or more in following discriminating and/or the content assaying method.

Differentiate:

A. get the content of 10 of Chinese medicine compound capsules of the present invention, add methanol 30ml, reflux 30 minutes, put cold, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with the ethyl acetate jolting, each 20ml merges ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Herba Oxalidis strictae control medicinal material 1g, adds water 50ml, decocts 30 minutes, filters, and filtrate is concentrated into 20ml, shines medical material solution in pairs with legal system; According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 8-10: 3-5: toluene-ethyl acetate-formic acid of 1 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

B. get the content of 15 of Chinese medicine compound capsules of the present invention, add ethanol 50ml, reflux 30 minutes, put coldly, filter, filtrate is put and is concentrated into about 2ml in the water-bath, adding neutral alumina 1g mixes thoroughly in water-bath, drying adds the neutral alumina post (100～200 orders, the 4g that have filled, on the internal diameter 10～15mm), use earlier ethyl acetate-dehydrated alcohol 80ml eluting of 5-6: 5-4, discard eluent, the ethyl acetate of reuse 1-3: 7-9-dehydrated alcohol 50ml eluting, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Ilicis Rotundae control medicinal material 1.5g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 8-10: 2-4: 2-4: toluene-butanone of 1-methanol-formic acid is 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 at 90 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle or the fluorescence speckle of same color respectively.

Assay:

Take by weighing at 120 ℃ of drying under reduced pressure in right amount, add 60% ethanol and make the reference substance solution that every 1ml contains 0.2mg to the control substance of Rutin of constant weight;

Measure reference substance solution 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml 6.0ml puts respectively in the 25ml measuring bottle, respectively add 10% sodium nitrite solution 1ml, mixing is placed, 6 minutes, add 10% aluminum nitrate solution 1ml, mixing, placed 6 minutes, and added 4% caustic lye of soda 4ml, shake up, add 30% ethanol to scale, shake up, placed 15 minutes; With corresponding solution is blank; According to spectrophotography, measure trap at the wavelength place of 510nm, be vertical coordinate with the trap, concentration is abscissa, the drawing standard curve;

Get the content under the Chinese medicine compound capsule content uniformity item of the present invention, mixing is got 0.2g, and it is fixed to claim, put in the round-bottomed flask, add methanol 25ml, shake up, reflux 1 hour, take out, be cooled to room temperature, filter, filter paper adds methanol 25ml again together with residue, reflux 1 hour is taken out, and cooling filters, merging filtrate, residue washs with methanol 15ml gradation, and washing liquid and filtrate merge, evaporate to dryness, residue adds 60% ethanol makes dissolving, is transferred in the 50ml measuring bottle and is diluted to scale, shakes up, and promptly gets need testing solution; Measure need testing solution 2ml, the method under the preparation of sighting target directrix curve from " putting respectively in the 25ml measuring bottle ", is measured trap in accordance with the law, and gets need testing solution 2ml and add 30% ethanol dilution and do blank to 25ml; Read the weight of rutin the need testing solution from standard curve, calculate, promptly;

Every of Chinese medicine compound capsule of the present invention contains total flavones with rutin (C ₂₇H ₃₀O ₁₆) meter, must not be less than 10.0mg.

The extraction solvent of need testing solution can also be 70% ethanol or 50% ethanol in the invention described above assay.

Chinese medicine compound capsule of the present invention has clearing away heat-damp and promoting diuresis, and convergence analgesic effect is used for stomachache, diarrhoea, vomiting that acute gastroenteritis, dyspepsia cause; Oral, one time 2,3 times on the one.

The quality control standard of Chinese medicine compound capsule of the present invention has been revised and enlarged the thin layer chromatography of Herba Oxalidis strictae, Cortex Ilicis Rotundae and has been differentiated on the basis of former " fukean tablet " quality standard, has removed test-tube reaction; Revised and enlarged content of total flavone mensuration, the detection wavelength is 510nm, and average recovery rate is 96.83%, and relative standard deviation is 1.49%, has set up content of total flavone in accurate, the reliable colorimetric method for determining capsule of the present invention.After increasing thin layer chromatography discriminating and content of total flavone mensuration, carried out 18 months stability test.

Following experimental example and embodiment are used to further specify but are not limited to the present invention.

Experimental example 1. capsule for treating acute gastroenteritis 30 routine clinical observation brief summaries of the present invention

One, diagnosis and dialectical standard

1, Western medicine diagnose

Publish " disease treatment main points and curative effect determinate standard " formulation according to high Chinese medicine universities and colleges' teaching materials " Chinese Internal Medicine " (the relevant chapters and sections of having loose bowels) and with reference to Hebei province Department of Public Health.The tcm diagnosis acute gastroenteritis is because of taking in by due to the food of antibacterial or its endotoxin contamination mostly.Generally back a few hours morbidity on the feed, clinical symptoms has stomachache, abdominal distention, diarrhoea, feels sick, vomiting, heating, dehydration even shock etc., stool is water sample or mucoid, one day for several times more than.Suspicious food and stool are cultivated and can obtain positive pathogen.

2, Chinese medical discrimination

Damp-heat type: stomach discomfort or feeling of fullness, feel sick, vomiting, borborygmus, stomachache, suffer from diarrhoea yellow watery stool or band mucus, thirsty, yellow urine or heating is arranged, yellow fur or yellow greasy, soft and rapid pulse or sliding number.

The dyspepsia the intestines and stomach: the borborygmus of suffering from abdominal pain, feces is smelly as losing ovum under rushing down, and rushes down the back alleviation of pain, with the thing of indigestion, gastral cavity abdomen feeling of fullness, eructating foul odor acid is smelly, anorexia, the tongue fur dirt is turbid or thick greatly is bored with rolling pulse.

3, state of an illness weight grade scale sees the following form.

Table 1 state of an illness weight grade scale

Symptom		Gently (2 minutes)	In (4 minutes)	Heavy (6 minutes)
Symptom		Gently (2 minutes)	In (4 minutes)	Heavy (6 minutes)	Diarrhoea	Character	Shapeless loose stool	Rare loose stool	Watery stool (Mucous Stool)
Number of times	3-4 time/day	5-6 time/day	More than 6 times/day			Character	Shapeless loose stool	Rare loose stool	Watery stool (Mucous Stool)
Number of times	3-4 time/day	5-6 time/day	More than 6 times/day	The nauseating heating of stomachache vomiting borborygmus gastral cavilty feeling of fullness is thirsty		The random thoughts 1-2 times/day of idol that do not need to take medicine has low-grade fever, body temperature normally sometimes to have random thoughts idols to have and wish drink not	Time is longer, random thoughts are taken medicine and are just alleviated 3-4 time/day 3-4 time/day fever of the body, the body temperature 37-37.5 ℃ morning or borborygmus in afternoon often thoughts yearningly and not desire drink	Be persistence, acutely, need take medicine and could alleviate more than 4 times, frequently vomit half a day above/day fever of the body body temperature＞37.5 ℃ of thirsty desire polydipsia of the hyperfunction full-time thoughts of full-time borborygmus

Above primary symptom diarrhoea, it is slight suffering from abdominal pain, feel sick, vomit the long-pending 6-8 person of branch, and the long-pending 10-14 person of branch is a severe, and amassing 14 fens above persons is severe.

Two, clinical data

1, sex: male 12 examples, women 18 examples.

2, the age: 14～30 years old 11 example, 31～50 years old 12 example, 51～67 years old 7 example.Minimal ages 14 years old, maximum 67 years old age, 33.96 years old mean age.

3, the state of an illness: slight 10 examples, moderate 12 examples, severe 8 examples.

4, the course of disease:＜1 day 7 example ,～2 days 15 examples ,～3 days 8 examples.

5, tcm symptom sees Table 2.

Table 2 tcm symptom distributes

Symptom		The example number	Do not have	Gently	In	Heavy
Symptom		The example number	Do not have	Gently	In	Heavy	Diarrhoea	Character	30	0	11	12	7
Number of times	30	0	10	14	6			Character	30	0	11	12	7
Number of times	30	0	10	14	6	The stomachache nausea and vomiting borborygmus thirsty gastral cavilty feeling of fullness that generates heat		30 30 30 30 30 30 30	0 6 7 20 21 2 10	11 10 11 9 9 18 10	18 11 10 1 0 10 6	1 3 2 0 0 0 4

6, tongue, pulse condition: tongue fur BOHUANG 12 examples, yellow greasy 17 examples, turbid 1 example of dirt.Smooth pulse 18 examples, sliding rapid pulse 7 examples are moistened rapid pulse 5 examples.

7, hemogram and stool routine examination inspection see Table 3.

Table 3 differential blood count and stool routine examination are checked situation

Project	The example number	Normally	Unusually
Project	The example number	Normally	Unusually	The differential blood count stool routine examination	30 30	23 0	7 30

Three, curative effect determinate standard and treatment observational technique.

1, curative effect determinate standard:

Clinical recovery: traditional Chinese medical science primary symptom, inferior disease disappear, and the stool chemical examination is normal.

Produce effects: primary symptom disappears, inferior disease is most of improves, and the stool chemical examination is normal substantially.

Effectively: primary symptom, inferior disease are improved, and the stool chemical examination takes a turn for the better to some extent.

Invalid: primary symptom, inferior disease do not have improvement, or increase the weight of, and the stool chemical examination does not improve.

2, treatment observational technique: oral capsule of the present invention, each 2.3 times on the one; 5 days was 1 course of treatment, carried out curative effect and summed up.

Four, result

1, total effects: clinical recovery 16 examples (53.33%), produce effects 9 examples (30%), effective 4 examples (13.33%), invalid 1 example (3.34%).

2, tcm symptom and curative effect see Table 4.

Table 4 tcm symptom curative effect

The state of an illness		The example number	Clinical cure	Produce effects	Effectively	Invalid
The state of an illness		The example number	Clinical cure	Produce effects	Effectively	Invalid	Diarrhoea	Character	30	16	10	3	1
Number of times	30	16	11	2	1			Character	30	16	10	3	1
Number of times	30	16	11	2	1	The stomachache nausea and vomiting borborygmus thirsty gastral cavilty feeling of fullness that generates heat		30 24 23 10 9 28 20	18 18 20 3 2 20 16	9 3 1 3 3 6 3	2 2 2 3 4 2 1	1 1 0 1 0 0 0

3, the state of an illness and curative effect see Table 5.

Table 5 state of an illness curative effect

The state of an illness	The example number	Clinical recovery	Produce effects	Effectively	Invalid
The state of an illness	The example number	Clinical recovery	Produce effects	Effectively	Invalid	Slight moderate severe	10 12 8	7 6 3	2 4 3	1 2 1	0 0 1

4, the course of disease and curative effect see Table 6.

Table 6 course of disease curative effect

The course of disease (my god)	The example number	Clinical recovery	Produce effects	Effectively	Invalid
The course of disease (my god)	The example number	Clinical recovery	Produce effects	Effectively	Invalid	＜1 day～2 days～3 days	7 15 8	4 9 3	2 4 3	1 2 1	0 0 1

5, tongue, pulse condition variation see Table 7.

Table 7 tongue, pulse condition change

Tongue, pulse condition	The example number	Take a turn for the better	Improve
Tongue, pulse condition	The example number	Take a turn for the better	Improve	The turbid rolling pulse slippery and rapid pulse of yellow and thin fur yellow and greasy fur dirty fur soft and rapid pulse	12 17 1 18 7 5	7 15 0 8 5 1	5 2 0 9 1 4

6, hemogram and stool routine examination check that situation of change sees Table 8.

Table 8 differential blood count, stool routine examination are checked situation of change

Project	The example number	Normally	Unusually
Project	The example number	Normally	Unusually	The differential blood count stool routine examination	7 30	6 25	0 4

Five, conclusion

Capsule for treating acute gastroenteritis clinical recovery 16 examples of the present invention (53.33%), produce effects 9 examples (30%), effective 4 examples (13.33%), total effective rate 96.67%, determined curative effect, safe in utilization, do not find apparent side effect.

Record in the fukean tablet quality standard of the 11 in " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation and differentiate that (1), (2) item react for non-exclusive, intend leaving out.Thin layer chromatography discrimination method referring now to Herba Oxalidis strictae and Cortex Ilicis Rotundae under " National Drug Administration's standard " (trying) WS-10256 (ZD-0256)-2002 fukean tablet quality standard discriminating item, Chinese medicine compound capsule of the present invention is carried out the thin layer chromatography discrimination test, simultaneously all the other 3 flavor medical materials are carried out the thin layer chromatography discrimination test respectively.Result of the test is seen experimental example 2-4:

Experimental example 2: the thin layer chromatography of Herba Oxalidis strictae is differentiated

1. the preparation of need testing solution: the content of getting 10 of Chinese medicine compound capsules of the present invention, add methanol 30ml, reflux 30 minutes filters, the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, extracts 2 times with the ethyl acetate jolting, each 20ml, merge ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.

2. the preparation of Herba Oxalidis strictae control medicinal material solution: get Herba Oxalidis strictae control medicinal material 1g, add water 50ml, decocted 30 minutes, filter, filtrate is concentrated into 20ml, shines medical material solution in pairs with legal system.

3. the preparation of Herba Oxalidis strictae blank solution: in described prescription ratio of technical scheme and method for making, replace Herba Oxalidis strictae to make the negative sample that does not contain Herba Oxalidis strictae, get 10 amounts, make Herba Oxalidis strictae blank solution by the preparation method of need testing solution with starch.

4. thin layer chromatography: described according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test by technical scheme, the negative control chromatograph is noiseless with control medicinal material principal spot relevant position.

Conclusion: the discrimination method that can be used as Chinese medicine compound capsule Herba Oxalidis strictae of the present invention.

Experimental example 3: the thin layer chromatography of Cortex Ilicis Rotundae is differentiated

I. [discriminating] (2) following method of recording with reference to FUKEAN Film coated tablets quality standard is tested, and gets the content of 15 of Chinese medicine compound capsules of the present invention, adds methanol 30ml, reflux 30 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with the ethyl acetate jolting, each 20ml merges ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution (same Herba Oxalidis strictae).Other gets Cortex Ilicis Rotundae control medicinal material 1g, adds water 30ml, decocts 30 minutes, filters, and filtrate is concentrated into 20ml, filters, and shines medical material solution in pairs with legal system.(according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel G plate according to thin layer chromatography, with toluene-ethyl acetate-formic acid (9: 4: 1) is developing solvent, launches, and takes out, dry spray ferric chloride test solution.The result: in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color, but feminine gender has interference.

Conclusion: not as the discrimination method of Chinese medicine compound capsule Cortex Ilicis Rotundae of the present invention.

II. adopt the thin layer chromatography discrimination method of the described Cortex Ilicis Rotundae of technical solution of the present invention to test:

1. the preparation of need testing solution: the content of getting 15 of Chinese medicine compound capsules of the present invention, add ethanol 50ml, reflux 30 minutes, put coldly, filter, filtrate is put and is concentrated into about 2ml in the water-bath, adding neutral alumina 1g mixes thoroughly in water-bath, drying adds the neutral alumina post (100～200 orders, the 4g that have filled, on the internal diameter 10～15mm), with ethyl acetate-dehydrated alcohol (6: 4) 80ml eluting, discard eluent, reuse ethyl acetate-dehydrated alcohol (2: 8) 50ml eluting earlier, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.

2. the preparation of Cortex Ilicis Rotundae control medicinal material solution: get Cortex Ilicis Rotundae control medicinal material 1.5g, shine medical material solution in pairs with legal system.

3. the preparation of Cortex Ilicis Rotundae blank solution: in described prescription ratio of technical scheme and method for making, replace Cortex Ilicis Rotundae to make the negative sample that does not contain Cortex Ilicis Rotundae, get 15 amounts, make Cortex Ilicis Rotundae blank solution by the preparation method of need testing solution with starch.

4. thin layer chromatography: described according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test by technical scheme, the negative control chromatograph is noiseless with control medicinal material principal spot relevant position.

Conclusion: the discrimination method that can be used as Chinese medicine compound capsule Cortex Ilicis Rotundae of the present invention.

Experimental example 4: the thin layer chromatography discrimination test of other Chinese crude drug in the crude drug

1. Pericarpium Granati

Method (1): get 10 of Chinese medicine compound capsules of the present invention, porphyrize adds ethanol 25ml, and heating in water bath refluxed 30 minutes, filters, and filtrate is put evaporate to dryness in the water-bath, and residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets Pericarpium Granati control medicinal material 1g, adds water 30ml, decocts 1 hour, filters, and filtrate is concentrated into thick shape, adds ethanol and makes and contain the alcohol amount and reach more than 70%, leaves standstill 24 hours, filters, and evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), drawing each 2 μ l of above-mentioned two kinds of solution, put respectively on same 1% sodium hydroxide-sodium carboxymethyl cellulose silica gel g thin-layer plate, is developing solvent with toluene-ethyl acetate-glacial acetic acid (25: 14: 1), launch, take out, dry, spray is with 1% ferric chloride, one iron potassuim cyanide test liquid, observe under the sight, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.But lack the Pericarpium Granati negative control and be equipped with interference in corresponding positions.Conclusion: the discrimination method that not can be used as Pericarpium Granati.

Method (2): get 10 of Chinese medicine compound capsules of the present invention, porphyrize adds water 30ml heated and stirred and made dissolving in 10 minutes, filters, filtrate adds water-saturated n-butanol extracts 2 times, and each 30ml merges n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Pericarpium Granati control medicinal material 1g, adds water 100ml, decocts 1 hour, filters, and filtrate concentrates 30ml, adds water-saturated n-butanol and extracts 2 times, and each 30ml merges n-butanol extracting liquid, puts evaporate to dryness in the water-bath, and residue adds methanol 1ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene-ethyl acetate-glacial acetic acid (4: 4: 0.4), launch, take out, dry, spray is with 1% vanillin sulfuric acid solution, daylight is observed down, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical pinkish speckle.It is noiseless in the relevant position to lack the Pericarpium Granati negative control.Conclusion: the discrimination method that not can be used as Pericarpium Granati.

Method (3): get 10 of Chinese medicine compound capsules of the present invention, porphyrize adds water 50ml, add hydrochloric acid 2ml, reflux is 1 hour in the water-bath, puts coldly, filters, filtrate adds chloroform and extracts 2 times, each 30ml, the combined chloroform extracting solution is put evaporate to dryness in the water-bath, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Pericarpium Granati control medicinal material 1g, adds water 100ml, decocts 1 hour, filters, and filtrate concentrates 50ml, adds hydrochloric acid 2ml, and reflux is 1 hour in the water-bath, puts coldly, and filtration is shone medical material solution in pairs with legal system; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene one glacial acetic acid-formic acid (15: 5: 2), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.Lack the Pericarpium Granati negative control and be equipped with interference in corresponding positions.Conclusion: the discrimination method that not can be used as Pericarpium Granati.

Annotate: Pericarpium Granati control medicinal material: through being accredited as the dry peel of Punicaceae plant Punica granatum L. Punica granatumL..

2. Herb Polygoni Chinensis, Pericarpium Granati: get 10 of Chinese medicine compound capsules of the present invention, porphyrize, add water 30ml heated and stirred and made dissolving in 10 minutes, filter, filtrate adds water-saturated n-butanol extracts 2 times, each 30ml, merge n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Pericarpium Granati, each 1g of Herb Polygoni Chinensis's control medicinal material, adds water 100ml respectively, decocts 1 hour, filters, filtrate concentrates 30ml, adds water-saturated n-butanol and extracts 2 times, merges n-butanol extracting liquid, put evaporate to dryness in the water-bath, residue adds methanol 1ml makes dissolving, in contrast medical material solution; Get the gallic acid reference substance again, add methanol and make the solution that 1ml contains 1mg, in contrast product solution; According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be the silica gel G F of adhesive with the sodium carboxymethyl cellulose ₂₄₅On the lamellae, be developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and observe with toluene-ethyl acetate-glacial acetic acid (4: 4: 0.4); In the test sample chromatograph, with control medicinal material chromatograph, the corresponding position of reference substance chromatograph on, show a speckle of same color.Lack the Herb Polygoni Chinensis, the Pericarpium Granati negative control is noiseless in the relevant position.The result shows that Herb Polygoni Chinensis and Pericarpium Granati all contain gallic acid, and specificity is not strong, so do not intend into technical scheme.

Annotate: Herb Polygoni Chinensis's control medicinal material: through being accredited as Liao Ke plant Herb Polygoni Chinensis Polygonum chinenseL. or coarse wool Herb Polygoni Chinensis Polygonum chinense L.var.HispidumHook.f. dry herb.

Capsule crude drug of the present invention is made up of 5 flavor Chinese medicines such as Herba Oxalidis strictae, and Pericarpium Granati contains the gallic acid composition, and through testing with high performance liquid chromatography, the discovery Herb Polygoni Chinensis is also contained the gallic acid composition, does not have a specificity; Cortex Ilicis Rotundae contains the ligustrin composition, but lacks reference substance, fails to carry out quantitative study; Medical materials such as Herba Oxalidis strictae, Herb Polygoni Chinensis, Herba Plantaginis find no the quality control that known reference substance can be used for carrying out this product at present.Given this, method under the assay item that records with reference to FUKEAN Film coated tablets quality standard is worked out content of total flavone assay method in the capsule of the present invention, and result of the test is seen experimental example 5.

Experimental example 5 content of total flavone assay method experimental studies

1, instrument and reagent

UV2501 PC ultraviolet spectrophotometer (day island proper Tianjin); KQ-100 ultrasonic washing instrument (Kunshan Ultrasonic Instruments Co., Ltd.).Control substance of Rutin (lot number: 0080-9705 is for assay usefulness, and Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides).Capsule of the present invention (lot number: 20030901,20030902,20030903).Reagent: be analytical pure.

2, the preparation of reference substance solution

Precision takes by weighing at 120 ℃ of drying under reduced pressure an amount of to the control substance of Rutin of constant weight, adds 60% ethanol and makes the solution that every 1ml contains 0.2mg, promptly.

3, the preparation of need testing solution

Get the content under the capsule content uniformity item of the present invention, mixing is got about 0.2g, and accurate the title decides, put in the round-bottomed flask, add methanol 25ml, shake up, reflux 1 hour, take out, be cooled to room temperature, filter, filter paper adds methanol 25ml again together with residue, reflux 1 hour is taken out, and cooling filters, merging filtrate, residue washs with methanol 15ml gradation, and washing liquid and filtrate merge, evaporate to dryness, residue adds 60% ethanol makes dissolving, is transferred in the 50ml measuring bottle and is diluted to scale, shakes up, promptly.

(1) selection of extraction solvent:

Take by weighing sample (lot number 20030901) respectively, add different solvents, all the other prepare need testing solution as stated above, press the condition colour developing under the preparation of standard curve again, and mensuration the results are shown in Table 9.

Table 9

Solvent	Methanol	50% ethanol	70% ethanol	Ethanol
Solvent	Methanol	50% ethanol	70% ethanol	Ethanol	Content (mg/ grain)	13.236	13.715	13.365	12.913

By The above results as can be known, except that alcoholic acid extraction content was low slightly, the extraction result of its excess-three kind solvent is close, and was best with 50% ethanol, but 50% ethanol and 70% ethanol extract color are darker, and impurity is more relatively; Methanol extract liquid is evaporate to dryness easily, handled easily, and particular methanol is made extraction solvent.

(2) selection of extracting method:

Extract by different way, all the other prepare need testing solution as stated above, press the condition colour developing under the preparation of standard curve again, and mensuration the results are shown in Table 10.

Table 10

Method	Merceration 24h	Cocurrent flow 1h secondary	Supersound process 1h secondary	Soxhlet is extracted 6h
Method	Merceration 24h	Cocurrent flow 1h secondary	Supersound process 1h secondary	Soxhlet is extracted 6h	Content (mg/ grain)	12.365	13.219	12.545	12.706

By The above results as can be known, the extraction efficiency of reflux is best, so the selective extraction method is a reflux.

(3) selection of reflux time, number of times:

Select the different reflux time, all the other prepare need testing solution as stated above, press the condition colour developing under the preparation of standard curve again, measure, and the results are shown in Table 11.

Table 11

Return time (h/ time)	0.5	1	2
Return time (h/ time)	0.5	1	2	Content (mg/ grain)	12.602	13.140	13.154

Select different heating number of times, all the other prepare need testing solution as stated above, press the condition colour developing under the preparation of standard curve again, measure, and the results are shown in Table 12.

Table 12

Extraction time (inferior)	1	2	3
Extraction time (inferior)	1	2	3	Content (mg/ grain)	11.900	13.140	12.890

By The above results as can be known, the reflux secondary extracted flavones ingredient fully in each 1 hour, and in conjunction with the recovery test result, so select the reflux secondary, reflux extracting time is each 1 hour.

4, measure the selection of wavelength

Get control substance of Rutin solution (0.2008mg/ml) and each 2ml of need testing solution, press the condition colour developing under the preparation of standard curve, in the interscan of 400～600nm wave-length coverage, reference substance solution and need testing solution have absorption maximum at the wavelength place of 507nm, 508nm respectively as a result, trap at 500～515nm wavelength place changes little, is λ=510nm so can select to measure wavelength.

5, standard curve

Precision takes by weighing control substance of Rutin 0.01004g, puts in the 50ml measuring bottle, adds methanol to scale, shake up, accurate reference substance solution 1,2,3,4,5, the 6ml of drawing puts respectively in the 25ml measuring bottle, respectively add 10% sodium nitrite solution 1ml, mixing was placed 6 minutes, add 10% aluminum nitrate solution 1ml, mixing was placed 6 minutes, add 4% caustic lye of soda 4ml, shake up, add 30% ethanol to scale, shaking up, placed 15 minutes, is blank with the corresponding solvent.According to spectrophotography (an appendix V of Chinese Pharmacopoeia version in 2000 B), measure trap at the wavelength place of 510nm, the results are shown in Table 13.

Table 13

C(μg/ml)	8.032	16.064	24.096	32.128	40.160	48.192
C(μg/ml)	8.032	16.064	24.096	32.128	40.160	48.192	Trap (A)	0.101	0.209	0.316	0.420	0.527	0.630

As abscissa, the trap that records is carried out linear regression as vertical coordinate with reference substance concentration, and getting linear equation is Y=1.3172 * 10 ^-2X-3.1333 * 10-3, r=1.000, the range of linearity is 8.032～48.192 μ g/ml.

6, the interference test of adjuvant

Get right amount of auxiliary materials such as starch, carboxymethyl starch sodium, magnesium stearate, handle and measure by the preparation and the assay method of need testing solution, trap is 0.002 as a result, is 0.78% of test sample trap, shows that adjuvant is little to the measurement result influence.

7, precision test

Accurate respectively absorption control substance of Rutin solution (0.2008mg/ml) and same need testing solution (lot number: 20030901) each 2ml, by above-mentioned condition colour developing, measure, the results are shown in Table 14.

Table 14

Sequence number	1	2	3	4	5	Meansigma methods	RSD(％)
Sequence number	1	2	3	4	5	Meansigma methods	RSD(％)	Reference substance trap (A) test sample trap (A)	0.416 0.266	0.416 0.266	0.416 0.266	0.416 0.266	0.416 0.266	0.416 0.266	0 0

8, stability test

Accurate respectively absorption control substance of Rutin solution (0.2008mg/ml) and same need testing solution (lot number: 20030901) each 2ml, by above-mentioned condition colour developing, at room temperature place, measured once every 15 minutes, the result shows that trap is basicly stable in 1 hour after colour developing, the results are shown in Table 15.

Table 15

Minute (min)	0	15	30	45	60	Meansigma methods	RSD(％)
Minute (min)	0	15	30	45	60	Meansigma methods	RSD(％)	Reference substance trap (A) test sample trap (A)	0.314 0.265	0.311 0.264	0.307 0.260	0.305 0.259	0.302 0.256	0.308 0.261	1.55 1.42

9, replica test

Precision take by weighing same test sample (lot number: 20030901) 5 parts, handle and measure by content assaying method, the results are shown in Table 16.

Table 16

Sequence number	1	2	3	4	5	Meansigma methods	RSD(％)
Sequence number	1	2	3	4	5	Meansigma methods	RSD(％)	Content (mg/ grain)	12.681	12.842	12.616	13.274	12.776	12.838	2.02

10, application of sample recovery test

Get 5 parts of each 0.2g of same test sample (lot number: 20030901, content is the 12.838mg/ sheet), accurate claim fixed, accurate respectively reference substance solution (containing rutin 1.9792mg/ml) 8ml, 7ml, mixing, the drying of adding, press content assaying method respectively and handle and measure, and calculate recovery rate.The results are shown in Table 17.

Table 17

Sequence number	Test sample amount (g)	Rutin content (mg)	Add reference substance amount (mg)	The amount of recording (mg)	The response rate (%)	Average recovery rate (%)	RSD (％)
Sequence number	Test sample amount (g)	Rutin content (mg)	Add reference substance amount (mg)	The amount of recording (mg)	The response rate (%)	Average recovery rate (%)	RSD (％)	1 2 3 4 5	0.2019 0.2009 0.2014 0.2011 0.2007	12.7118 12.6489 12.6803 12.6615 12.6363	15.8336 15.8336 15.8336 13.8544 13.8544	27.9400 27.9300 27.8475 26.0056 26.4025	96.18 96.51 95.79 96.32 99.36	96.83	1.49

11, sample size is measured

Measure the content of rutin in 3 batch samples by method under the assay item, the results are shown in Table 18.

Table 18

Lot number	Rutin content (mg/ sheet)
	Rutin content (mg/ sheet)			1	2	3
	020,101 020,102 020103 is average	12.706 12.153 12.603	12.687 12.217 12.480	1	2	3	12.70 12.18 12.54 12.47

According to above experimental result, the meansigma methods that 3 batch samples detect is the 12.47mg/ sheet, presses 80% of measured value and calculates, and determines that every of capsule of the present invention contains total flavones with rutin (C ₂₇H ₃₀O ₁₆) meter, must not be less than 10.0mg.

12, medical material assay such as Herba Oxalidis strictae

With reference to the capsular content assaying method of the invention described above, 5 kinds of medical materials such as Herba Oxalidis strictae have been carried out determination of total flavonoids respectively, experimental technique is as follows:

1. the preparation of the preparation of instrument, reagent, reference substance solution and standard curve: the same.

2. the preparation of need testing solution: get the about 1g of medicinal powders such as Herba Oxalidis strictae (crossing sieve No. four), the accurate title, decide, and puts in the round-bottomed flask, add methanol 25ml, shake up, reflux 1 hour is taken out, be cooled to room temperature, filter, filter paper adds methanol 25ml again together with residue, reflux 1 hour, take out, cooling filters merging filtrate, residue washs with methanol 15ml gradation, washing liquid and filtrate merge, and evaporate to dryness, residue add 60% ethanol makes dissolving, be transferred in the 50ml measuring bottle and be diluted to scale, shake up (dilution in case of necessity).

3. algoscopy: precision is measured 2ml, and method under the preparation of sighting target directrix curve from " putting respectively in the 25ml measuring bottle ", is measured trap in accordance with the law, calculates, promptly.The results are shown in Table 19～23.

Table 19 Herba Oxalidis strictae medical material assay result

Lot number	1	2	3
Lot number	1	2	3	Content (%)	2.10	1.96	1.79

Table 20 is rescued the heart and is answered medical material assay result

Lot number	1	2	3
Lot number	1	2	3	Content (%)	16.93	20.15	15.30

Table 21 Pericarpium Granati medical material assay result

Lot number	1	2	3
Lot number	1	2	3	Content (%)	1.98	2.24	2.13

Table 22 Herb Polygoni Chinensis medical material assay result

Lot number	1	2	3
Lot number	1	2	3	Content (%)	2.01	1.88	1.70

Table 23 Herba Plantaginis medical material assay result

Lot number	1	2	3
Lot number	1	2	3	Content (%)	1.95	1.62	1.76

By The above results as can be known, 5 kinds of medical materials such as Herba Oxalidis strictae all contain flavones ingredient, and are wherein the highest with Cortex Ilicis Rotundae medical material content.

13, Pericarpium Granati, Herb Polygoni Chinensis contain gallic acid in the prescription, use the HPLC method and measure the wherein content of gallic acid, and experimental technique is as follows:

1. chromatographic condition: strong to close silica gel be filler with octadecylsilane; Methanol-water-phosphoric acid (15: 85: 0.3) is a mobile phase; The detection wavelength is 270nm.

2. the preparation of reference substance solution: it is an amount of that precision takes by weighing the gallic acid reference substance, adds methanol and make the solution that contains gallic acid 40 μ g among every 1ml, promptly.

3. the preparation of need testing solution: get the content under the capsule content uniformity item of the present invention, mixing is got about 0.2g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 50% methanol 25ml that adds, close plug claims to decide weight, puts in the water-bath reflux 1 hour, put coldly, claim again to decide weight, supply the weight that subtracts mistake with 50% methanol, shake up, filter, get subsequent filtrate, promptly.

4. algoscopy: accurate respectively each the 10 μ l of reference substance solution and need testing solution that draw, inject chromatograph of liquid, mensuration, promptly.

Experimental result shows that Pericarpium Granati and Herb Polygoni Chinensis are all contained gallic acid, and consistent with experimental example 4 thin layer chromatography identification results, both is negative noiseless, but because both are not monarch's medicines, so do not intend into technical scheme.

The following embodiment of the present invention all can reach the effect of above-mentioned experimental example.

Embodiment 1: Chinese medicine compound capsule of the present invention

Get Herba Oxalidis strictae 200g, Herb Polygoni Chinensis 200g, Herba Plantaginis 66g, Cortex Ilicis Rotundae 134g, Pericarpium Granati 66g; The above five tastes decoct with water secondary, add 12 times of water gagings for the first time, for the second time add 10 times of water gagings, each 2 hours, collecting decoction, filter, it is 1.08～1.10 (85～90 ℃) that filtrate is concentrated into relative density, adds ethanol and makes and contain the alcohol amount and reach 65%, left standstill 24 hours, and filtered, residue with 65% washing with alcohol once, leave standstill, filter, merge secondary filtrate, reclaim ethanol, be condensed into thick paste, cold drying, pulverize, add starch, carboxymethyl starch sodium is an amount of, makes granule with 70% ethanol, dry, it is an amount of to add magnesium stearate, and mixing is adorned capsule No. 2, make 1000, promptly.Oral, one time 2,3 times on the one.

Embodiment 2: the method for quality control of Chinese medicine compound capsule of the present invention

Differentiate:

A. get the content of 10 of Chinese medicine compound capsules of the present invention, add methanol 30ml, reflux 30 minutes, put cold, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with the ethyl acetate jolting, each 20ml merges ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Herba Oxalidis strictae control medicinal material 1g, adds water 50ml, decocts 30 minutes, filters, and filtrate is concentrated into 20ml, shines medical material solution in pairs with legal system; According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid (9: 4: 1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

B. get the content of 15 of Chinese medicine compound capsules of the present invention, add ethanol 50ml, reflux 30 minutes, put coldly, filter, filtrate is put and is concentrated into about 2ml in the water-bath, adding neutral alumina 1g mixes thoroughly in water-bath, drying adds the neutral alumina post (100～200 orders, the 4g that have filled, on the internal diameter 10～15mm), with ethyl acetate-dehydrated alcohol (6: 4) 80ml eluting, discard eluent, reuse ethyl acetate-dehydrated alcohol (2: 8) 50ml eluting earlier, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Ilicis Rotundae control medicinal material 1.5g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, (9: 3: 3: 1) be developing solvent, expansion was taken out with toluene-butanone-methanol-formic acid, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 90 ℃, puts respectively under daylight and the ultra-violet lamp (365nm) and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle or the fluorescence speckle of same color respectively.

Embodiment 3: the method for quality control of Chinese medicine compound capsule of the present invention

Assay:

Embodiment 4: the method for quality control of Chinese medicine compound capsule of the present invention

Differentiate:

Assay:

Embodiment 5: Chinese medicine compound capsule preparation of the present invention and method of quality control

Herba Oxalidis strictae 200g, Herb Polygoni Chinensis 200g, Herba Plantaginis 66g, Cortex Ilicis Rotundae 134g, Pericarpium Granati 66g;

The above five tastes decoct with water secondary, add 12 times of water gagings for the first time, for the second time add 10 times of water gagings, each 2 hours, collecting decoction, filter, it is 1.08～1.10 (85～90 ℃) that filtrate is concentrated into relative density, adds ethanol and makes and contain the alcohol amount and reach 65%, left standstill 24 hours, and filtered, residue with 65% washing with alcohol once, leave standstill, filter, merge secondary filtrate, reclaim ethanol, be condensed into thick paste, cold drying, pulverize, add starch, carboxymethyl starch sodium is an amount of, makes granule with 70% ethanol, dry, it is an amount of to add magnesium stearate, and mixing is adorned capsule No. 2, make 1000, promptly get Chinese medicine compound capsule of the present invention.

The method of quality control of Zhi Bei Chinese medicine compound capsule of the present invention is as stated above:

Differentiate:

Assay:

Claims

1, a kind of Chinese medicine compound capsule for the treatment of acute gastroenteritis is characterized in that this capsule is prepared from as follows:

Herba Oxalidis strictae 165-245 weight portion, Herb Polygoni Chinensis 165-245 weight portion, Herba Plantaginis 50-80 weight portion, Cortex Ilicis Rotundae 105-165 weight portion, Pericarpium Granati 50-80 weight portion; Above five tastes crude drug decocts with water 2-3 time, adds 10-12 times of water gaging at every turn, each 2 hours, collecting decoction filtered, it is 1.08～1.10 that filtrate is concentrated into 85～90 ℃ of relative densities, adds ethanol and makes and contain the alcohol amount and reach 65%, leaves standstill, filter, residue with 65% washing with alcohol once leaves standstill, filter, merge secondary filtrate, reclaim ethanol, be condensed into thick paste, cold drying is pulverized, and adds starch, carboxymethyl starch sodium is an amount of, make granule with 70% ethanol, drying, the adding magnesium stearate is an amount of, mixing, adorn capsule No. 2, promptly.

2, the Chinese medicine compound capsule of treatment acute gastroenteritis as claimed in claim 1 is characterized in that this capsule is prepared from as follows:

Herba Oxalidis strictae 200 weight portions, Herb Polygoni Chinensis's 200 weight portions, Herba Plantaginis 66 weight portions, Cortex Ilicis Rotundae 134 weight portions, Pericarpium Granati 66 weight portions; Above five tastes crude drug decocts with water secondary, adds 12 times of water gagings for the first time, for the second time add 10 times of water gagings, each 2 hours, collecting decoction, filter, it is 1.08～1.10 that filtrate is concentrated into 85～90 ℃ of relative densities, adds ethanol and makes and contain the alcohol amount and reach 65%, left standstill 24 hours, and filtered, residue with 65% washing with alcohol once, leave standstill, filter, merge secondary filtrate, reclaim ethanol, be condensed into thick paste, cold drying, pulverize, add starch, carboxymethyl starch sodium is an amount of, makes granule with 70% ethanol, drying, it is an amount of to add magnesium stearate, mixing is adorned capsule No. 2, promptly.

3, a kind of preparation method for the treatment of the Chinese medicine compound capsule of acute gastroenteritis is characterized in that this method is:

4, the preparation method of the Chinese medicine compound capsule of treatment acute gastroenteritis as claimed in claim 3 is characterized in that this method is:

5, the method for quality control of Chinese medicine compound capsule as claimed in claim 1 or 2 is characterized in that this method comprises one or more in the following discrimination method:

A. get the content of 10 of Chinese medicine compound capsules of the present invention, add methanol 30ml, reflux 30 minutes, put cold, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with the ethyl acetate jolting, each 20ml merges ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Herba Oxalidis strictae control medicinal material 1g, adds water 50ml, decocts 30 minutes, filters, and filtrate is concentrated into 20ml, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 8-10: 3-5: toluene-ethyl acetate-formic acid of 1 is developing solvent, launches, and takes out, and dries, and puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

B. get the content of 15 of Chinese medicine compound capsules of the present invention, add ethanol 50ml, reflux 30 minutes, put cold, filter, filtrate is put and is concentrated into 2ml in the water-bath, adds neutral alumina 1g and mix drying thoroughly in water-bath, on 100～200 orders that adding has filled, the neutral alumina post of 4g, internal diameter 10～15mm, use earlier ethyl acetate-dehydrated alcohol 80ml eluting of 5-6: 5-4, discard eluent, the ethyl acetate of reuse 1-3: 7-9-dehydrated alcohol 50ml eluting, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Ilicis Rotundae control medicinal material 1.5g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 8-10: 2-4: 2-4: toluene-butanone of 1-methanol-formic acid is 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 at 90 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle or the fluorescence speckle of same color respectively.

6, the method for quality control of Chinese medicine compound capsule as claimed in claim 5 is characterized in that this method comprises one or more in the following discrimination method:

A. get the content of 10 of Chinese medicine compound capsules of the present invention, add methanol 30ml, reflux 30 minutes, put cold, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with the ethyl acetate jolting, each 20ml merges ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Herba Oxalidis strictae control medicinal material 1g, adds water 50ml, decocts 30 minutes, filters, and filtrate is concentrated into 20ml, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with toluene-ethyl acetate-formic acid of 9: 4: 1, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

B. get the content of 15 of Chinese medicine compound capsules of the present invention, add ethanol 50ml, reflux 30 minutes, put coldly, filter, filtrate is put and is concentrated into 2ml in the water-bath, add neutral alumina 1g and mix thoroughly in water-bath, drying adds on the neutral alumina post that has filled, with ethyl acetate-dehydrated alcohol 80ml eluting of 6: 4, discard eluent, 2: 8 ethyl acetate of reuse-dehydrated alcohol 50ml eluting earlier, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Ilicis Rotundae control medicinal material 1.5g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 9: 3: 3: toluene-butanone of 1-methanol-formic acid was developing solvent, launched, and took out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 90 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle or the fluorescence speckle of same color respectively.

7, the method for quality control of Chinese medicine compound capsule as claimed in claim 1 or 2 is characterized in that this method comprises following content assaying method:

Every of Chinese medicine compound capsule of the present invention contains total flavones in rutin, must not be less than 10.0mg.

8, the method for quality control of Chinese medicine compound capsule as claimed in claim 7, the extraction solvent that it is characterized in that need testing solution in the content assaying method can also be 70% ethanol or 50% ethanol.

9, the method for quality control of Chinese medicine compound capsule as claimed in claim 1 or 2 is characterized in that this method is:

Differentiate:

A. get the content of 10 of Chinese medicine compound capsules of the present invention, add methanol 30ml, reflux 30 minutes, put cold, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extract 2 times with the ethyl acetate jolting, each 20ml merges ethyl acetate liquid, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Herba Oxalidis strictae control medicinal material 1g, adds water 50ml, decocts 30 minutes, filters, and filtrate is concentrated into 20ml, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be that toluene-ethyl acetate-formic acid of 9: 4: 1 is developing solvent with ratio, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

B. get the content of 15 of Chinese medicine compound capsules of the present invention, add ethanol 50ml, reflux 30 minutes, put coldly, filter, filtrate is put and is concentrated into 2ml in the water-bath, add neutral alumina 1g and mix thoroughly in water-bath, drying adds on the neutral alumina post that has filled, with ethyl acetate-dehydrated alcohol 80ml eluting of 6: 4, discard eluent, 2: 8 ethyl acetate of reuse-dehydrated alcohol 50ml eluting earlier, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Ilicis Rotundae control medicinal material 1.5g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 9: 3: 3: toluene-butanone of 1-methanol-formic acid was developing solvent, launched, and took out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 90 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle or the fluorescence speckle of same color respectively;

Assay:

10, the method for quality control of Chinese medicine compound capsule as claimed in claim 9, the extraction solvent that it is characterized in that need testing solution in the content assaying method can also be 70% ethanol or 50% ethanol.