CN1299734C - Composition of traditional Chinese medicine for large intestine hygropyretic disease and its preparation method - Google Patents
Composition of traditional Chinese medicine for large intestine hygropyretic disease and its preparation method Download PDFInfo
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- CN1299734C CN1299734C CNB031499872A CN03149987A CN1299734C CN 1299734 C CN1299734 C CN 1299734C CN B031499872 A CNB031499872 A CN B031499872A CN 03149987 A CN03149987 A CN 03149987A CN 1299734 C CN1299734 C CN 1299734C
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract
The present invention discloses a traditional Chinese medicine composition for a treating large intestine damp-heat symptom and a preparation method thereof. The composition is mainly composed of rhubarb, sophora flower, atractylodes rhizome, cacumen biotae, notopterygium root, honeysuckle flower, aconite root, red halloysite, bitter apricot seed and areca seed. When the composition of the present invention is prepared, different constituents adopt the methods of decoction, alcohol extraction and distillation to achieve the full performance of effective ingredients. Simultaneously, the present invention also provides a quality control method for the ingredient identification, the content identification and the examination of the composition. The composition has good effects on the treatment of diarrhea and dysentery.
Description
Invention field
The present invention relates to a kind of Chinese medicine composition, particularly be used for the treatment of the Chinese medicine composition of syndrome of dampness-heat in large intestine, relate to the preparation method and the method for quality control of said composition simultaneously.
Background technology
Dysentery, having loose bowels is common clinical, betides summer and autumn modally to be " syndrome of dampness-heat in large intestine ".The present invention ties up on East Guangdong old established firm between light-year of cleaning the street " the exceedingly high Ji pharmacy " basis, side's of secretly handing down (not disclosing), is improved according to modern clinical experimental research.
(300 examples: there is significant difference 100 examples) P＜0.05 to clinical warp with adding flavor Xianglian Wan (production of Chinese medicine two factories of group of Tongrentang) contrast.Experimentation confirms: the present invention has heat clearing away, antidiarrheal, analgesia, and escherichia coli, golden staphylococci, bacillus pyocyaneus, Candida albicans are had inhibitory action.
Summary of the invention
One object of the present invention is to disclose a kind of Chinese medicine composition of new treatment syndrome of dampness-heat in large intestine; Another object of the present invention is the method for the Chinese medicine composition of a kind of new treatment syndrome of dampness-heat in large intestine of open preparation.The object of the invention also is to disclose a kind of method of quality control of new Chinese medicine composition.
The crude drug of pharmaceutical composition of the present invention is formed and proportioning following (by weight):
Radix Et Rhizoma Rhei 300-400 weight portion Flos Sophorae 20-50 weight portion
Rhizoma Atractylodis 220-280 weight portion Cacumen Platycladi 20-50 weight portion
Rhizoma Et Radix Notopterygii 140-200 weight portion Flos Lonicerae 50-110 weight portion
Radix Aconiti Preparata 140-200 weight portion Halloysitum Rubrum 50-110 weight portion
Semen Armeniacae Amarum 35-90 weight portion Semen Arecae 40-90 weight portion.
The preferred Flos Sophorae parch to black of Flos Sophorae; The preferred Rhizoma Atractylodis infusion of Rhizoma Atractylodis; Cacumen Platycladi preferential side Cacumen Platycladi (Cacumen Biotae) parch to black; Halloysitum Rubrum is preferably made Halloysitum Rubrum; The preferred Semen Arecae (parched) of Semen Arecae.
The preparation method of the present composition is as follows:
More than ten the flavor, get Radix Et Rhizoma Rhei, Rhizoma Atractylodis, each 15-25 weight portion of Rhizoma Et Radix Notopterygii, Halloysitum Rubrum (system), each 3-8 weight portion of Semen Armeniacae Amarum, Radix Aconiti 10-25 weight portion, Flos Sophorae 5-15 weight portion, Cacumen Platycladi 3-10 weight portion are ground into fine powder, and be standby; The residue Radix Et Rhizoma Rhei is made solvent with 50-70% ethanol, and slowly percolation is collected percolate, and reclaim under reduced pressure is to not having the alcohol flavor and being condensed into the thick paste that relative density is 1.30-1.50 (50-80 a ℃), and is standby; Residue Rhizoma Atractylodis, Rhizoma Et Radix Notopterygii add Flos Lonicerae and extract volatile oil with steam distillation, and be standby; Aqueous solution after distillation device is in addition preserved; Medicinal residues and Semen Arecae and remaining Radix Aconiti, Semen Armeniacae Amarum, Halloysitum Rubrum, Cacumen Platycladi, Flos Sophorae merge, decoct with water 2-4 time each 1-3 hour, collecting decoction, filter, filtrate adds the aqueous solution after the distillation, and being condensed into relative density is the thick paste of 1.30-1.50 (50-80 ℃), add above-mentioned fine powder and thick paste, mixing, through conventional operation directly or add pharmaceutically acceptable excipient and make clinical acceptable forms, as tablet, oral liquid, capsule, granule, injection etc.
The method of quality control that the present composition is made medicament comprises assay and/or discriminating and/or inspection:
Assay: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 D), chromatographic condition and system suitability test, be filler: 80-90 with octadecylsilane chemically bonded silica: 10-20 methanol-0.1% phosphoric acid solution is a mobile phase; The detection wavelength is 254nm; Number of theoretical plate calculates by the emodin peak should be not less than 2000; The preparation of reference substance solution, precision take by weighing emodin and the chrysophanol reference substance is an amount of, adds 1-3 respectively: the mixed solution of 1-2 dehydrated alcohol-ethyl acetate is made the solution that contains emodin 1 μ g, chrysophanol 2 μ g among every 1ml, promptly; 20 in present composition tablet is got in the preparation of need testing solution, removes sugar-coat, the accurate title, decide, and porphyrize is crossed sieve No. three, and precision takes by weighing and is equivalent to 1 weight in right amount approximately, put in the conical flask accurate ethanol 25ml, the close plug of adding, claim to decide weight, reflux 1-2 hour, put cold, claim to decide weight, supply the weight that subtracts mistake with ethanol, filter, precision is measured subsequent filtrate 10ml, put in the conical flask, evaporate to dryness, residue add 30% ethanol-hydrochloric acid with 8-12: the mixed solution 15ml of 1-2 ratio, reflux 1-2 hour, cooling rapidly, in the dislocation separatory funnel, extract 4 times each 15ml with the chloroform jolting, combined chloroform liquid, evaporate to dryness, residue adds 1-3: the mixed solution of 1-2 dehydrated alcohol-ethyl acetate makes dissolving in right amount, in the dislocation 25ml measuring bottle, add 1-3: the mixed solution of 1-2 dehydrated alcohol-ethyl acetate is diluted to scale, shake up, filter with microporous filter membrane, promptly; Algoscopy, accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Present composition preparation per unit amount contains Radix Et Rhizoma Rhei with emodin (C
15H
10O
5) and chrysophanol (C
15H
10O
4) the total amount meter, must not be less than 0.10-0.20mg;
Discrimination method comprises a kind of and/or several in the following method: a. gets the need testing solution 20ml under the assay item, and evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system; Get emodin, chrysophanol reference substance again, add ethyl acetate and make the mixed solution that every 1ml contains emodin 0.5mg, chrysophanol 1mg, product solution in contrast; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 10 μ l of above-mentioned three kinds of solution, put on same silica gel g thin-layer plate respectively, with 10-20: 4-6: the upper solution of 1-2 petroleum ether (60-90 ℃)-Ethyl formate-formic acid is developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show five identical orange-yellow fluorescence speckles; With the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle; B. get 10 in present composition tablet, remove sugar-coat; Porphyrize, the 10ml that adds diethyl ether, the ultrasonic 15-30 of place minute, filter, filtrate is waved to 1ml, as need testing solution; Other gets Rhizoma Atractylodis 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 2000 B), draw above-mentioned need testing solution 20 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with 55-65: 1-2 petroleum ether (60-90 ℃)-ethyl acetate is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; C. get Rhizoma Et Radix Notopterygii control medicinal material 0.5g, make control medicinal material solution according to the preparation method of differentiating the control medicinal material solution under the b item; Other gets the isoimperatorin reference substance, adds diethyl ether to make the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, draw according to need testing solution 10 μ l and above-mentioned control medicinal material and each 1 μ l of reference substance solution of differentiating under the b item, put respectively on same silica gel g thin-layer plate, with 6-12: 1-3 benzene-ethyl acetate is developing solvent, launches, and exhibition is apart from about 5cm, take out, dry, again with 6-12: 1-3 petroleum ether (30-60 ℃)-butanone is developing solvent, launches, exhibition is apart from about 10cm, take out, dry, put under the ultra-violet lamp 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; Check: aconitine limit, get 8 in present composition tablet, remove sugar-coat, porphyrize, after 10% sodium carbonate liquor moistening, 50ml adds diethyl ether, supersound process 10-25 minute, filter, filtrate is extracted 2 times with 2% hydrochloric acid solution jolting, each 30ml, merge acid solution, regulate pH value to 11.5-12.5, extract 2 times with the ether jolting with strong ammonia solution, each 30ml, merge ether solution, extract 2 times, each 30ml with 2% hydrochloric acid solution jolting, merge acid liquid, regulate pH value to 11.5-12.5 with strong ammonia solution, extract 2 times, each 30ml with the ether jolting, merge ether solution, evaporate to dryness, residue add methanol make in right amount the dissolving and move in the 2ml measuring bottle, add methanol and be diluted to scale, shake up, as need testing solution; Other gets the aconitine reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), accurate above-mentioned need testing solution 10 μ 1, the reference substance solution 5 μ l of drawing, put respectively on same silica gel g thin-layer plate, with 6-10: 5-8: 1-2 cyclohexane extraction-ethyl acetate-diethylamine is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of appearance should or speckle not occur less than the speckle of reference substance.
Described per unit amount is meant the finished medicines dosage of suitable crude drug 1.3g.
Present composition preparation has heat clearing and damp drying, and the effect of relieving dysentery with astringents is suffered from abdominal pain to being used for enteritis, watery diarrhea, and the dysentery taking convenience, onset is rapid, and effect is obvious, and toxicity is low.Following experimental example is used to further specify the present invention.Below experiment is damp and hot with present composition preparation.
Experimental example 1 clinical data
Observe case 400 examples, 130 examples of wherein having loose bowels, 100 examples are organized in treatment, and cure-remarkable-effectiveness rate is 64.00%, total effective rate is 92.00%, matched group 30 examples, cure-remarkable-effectiveness rate 50.00%, total effective rate 73.33%, credit is analysed by statistics, and two groups of curative effects relatively have significant difference (P＜0.05).
Dysentery 270 examples, 200 examples are organized in treatment, and cure-remarkable-effectiveness rate is 63.50%, and total effective rate is 89.50%, matched group 70 examples, cure-remarkable-effectiveness rate is 57.14%, and total effective rate is 85.71%, and credit is analysed by statistics, and two groups of curative effects compare no difference of science of statistics (P＞0.05).Untoward reaction is not found in the clinical observation of treatment group, and is as follows in detail:
One, physical data
The case source: 400 routine patients, be selected from outpatient service and in-patient department patient, all case all meets the case choice criteria.
(1) sex: see (table 1-1, table 1-2)
Two groups of patient's sex ratios of table 1-1 dysentery (damp-heat syndrome)
| Group | The example number | The man | (％) | The woman | (％) | P |
| Treatment group matched group | 200 -70 | 113 41 | (56.50) (58.57) | 87 29 | (43.50) (41.43) | ＞0.05 ＞0.05 |
Through x
2Check, two groups of patient's sex ratios are than no difference of science of statistics (P＞0.05).
Table 1-2 has loose bowels (damp-heat syndrome) two groups of patient's sex ratios
| Group | The example number | The man | (％) | The woman | (％) | P |
| Treatment group matched group | 100 30 | 59 17 | (59.00) (56.67) | 41 13 | (41.00) (43.33) | ＞0.05 ＞0.05 |
Through x
2Check, two groups of patient's sex ratios are than no difference of science of statistics (P＞0.05).
(2) age: see (table 2-1, table 2-2)
Two groups of patient ages of table 2-1 dysentery (damp-heat syndrome) distribute relatively
| Group | The example number | Age distribution (year) | Mean age (year) | P | |||||
| 18～30 | (％) | 31～50 | (％) | 51～65 | (％) | X±SD | |||
| Treatment group matched group | 200 70 | 95 31 | (47.50) (44.29) | 72 26 | (36.00) (37.14) | 33 13 | (16.50) (18.57) | 35.55±182 36.44±3.04 | ＞0.05 ＞0.05 |
Treatment group minimal ages 18 years old, maximum 65 years old age, 35.55 years old mean age; Matched group minimal ages 18 years old, maximum 65 years old age, 36.44 years old mean age.
Through the t check, two groups of patient ages distribute and compare no difference of science of statistics (P＞0.05).
Table 2-2 has loose bowels (damp-heat syndrome) two groups of patient ages distributions relatively
| Group | The example number | Age distribution (year) | Mean age (year) | P | |||||
| 18～30 | (％) | 31～50 | (％) | 51～65 | (％) | X±SD | |||
| Treatment group matched group | 100 30 | 50 13 | (50.00) (43.33) | 31 10 | (31.00) (33.33) | 19 7 | (19.00) (23.33) | 36.00±2.55 37.00±4.50 | ＞0. 05 |
Treatment group minimal ages 18 years old, maximum 65 years old age, 36 years old mean age; Matched group minimal ages 19 years old, maximum 65 years old age, 37 years old mean age.
Through the t check, two groups of patient ages distribute and compare no difference of science of statistics (P＞0.05).
(3) course of disease: see (table 3-1, table 3-2)
Two groups of patient's courses of disease of table 3-1 dysentery (damp-heat syndrome) relatively
| Group | The example number | ≤ 3 days | 3 days～1 week | ＞1 week |
| Example number (%) | Example number (%) | Example number (%) | ||
| Treatment group matched group | 200 70 | 124(62.00) 37(52.86) | 61(30.5) 26(37.14) | 15(％) 7(10.00) |
Analyze through Ridit, two groups of patient's courses of disease distribute and compare no difference of science of statistics (P＞0.05).
Table 3-2 has loose bowels (damp-heat syndrome) two groups of patient's courses of disease relatively
| Group | The example number | ≤ 3 days | 3 days～1 week | ＞1 week |
| Example number (%) | Example number (%) | Example number (%) | ||
| Treatment group matched group | 100 30 | 68(68.00) 16(53.33) | 24(24.00) 9(30.00) | 8(8.00) 5(16.67) |
Analyze through Ridit, two groups of patient's courses of disease distribute and compare no difference of science of statistics (P＞0.05).
(4) tcm symptom: see (table 4-1, table 4-2)
Two groups of patient's tcm symptoms of table 4-1 dysentery (damp-heat syndrome) relatively
| Symptom | The treatment group | (％) | Matched group | (％) | P |
| Have loose bowels urgently let out and the rare water of the thirsty scanty drak urine stool red white Mucous Stool of yellowish-brown and smelly diarrhea of not well tenesmus burning sensation of the anus stomachache dysphoria with smothery sensation just | 49 148 193 167 200 174 163 26 180 192 22 | (24.50) (74.00) (96.50) (83.50) (100.00) (87.00) (81.50) (13.00) (90.00) (96.00) (11.00) | 14 53 67 63 70 60 56 10 61 67 7 | (20.00) (75.71) (95.71) (90.00) (100.00) (85.71) (80.00) (14.29) (87.14) (95.71) (10.00) | ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 |
Through x
2Analyze, two groups of patient's symptoms distribute and compare no difference of science of statistics (P＞0.05).
Table 4-2 has loose bowels (damp-heat syndrome) two groups of patient's tcm symptoms relatively
| Symptom | The treatment group | (％) | Matched group | (％) | P |
| Have loose bowels urgently let out and the rare water of the thirsty scanty drak urine stool red white Mucous Stool of yellowish-brown and smelly diarrhea of not well tenesmus burning sensation of the anus stomachache dysphoria with smothery sensation just | 85 86 2 88 100 91 65 59 0 0 41 | (85.00) (86.00) (2.00) (88.00) (100.00) (91.00) (65.00) (59.00) (0) (0) (41.00) | 24 26 0 28 30 24 16 21 0 0 9 | (80.00) (86.67) (0) (93.33) (100.00) (80.00) (53.33) (70.00) (0) (0) (30.00) | ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 |
Through x
2Analyze, two groups of patient's symptoms distribute and compare no difference of science of statistics (P＞0.05).
(5) tongue, pulse condition: see (table 5-1, table 5-2)
Two groups of patient's tongues of table 5-1 dysentery (damp-heat syndrome), pulse condition are relatively
| Group | The example number | Picture of the tongue | The example number | Pulse condition | P | ||
| Unusually | Normally | Unusually | Normally | ||||
| Treatment group matched group | 200 70 | 194 67 | 6 3 | 200 70 | 200 70 | 0 0 | ＞0.05 ＞0.05 |
Through x
2Check, two groups of patient's tongues, pulse conditions distribute and compare no difference of science of statistics (P＞0.05).
Table 5-2 has loose bowels (damp-heat syndrome) two groups of patient's tongues, pulse condition distribution relatively
| Group | The example number | Picture of the tongue | The example number | Pulse condition | P | ||
| Unusually | Normally | Unusually | Normally | ||||
| Treatment group matched group | 100 30 | 90 28 | 10 2 | 100 30 | 100 30 | 0 0 | ＞0.05 ＞0.05 |
Through x
2Check, two groups of patient's tongues, pulse conditions distribute and compare no difference of science of statistics (P＞0.05).
(6) hemogram and stool routine examination: see (table 6-1, table 6-2)
Two groups of differential blood counts of table 6-1 dysentery (damp-heat syndrome), stool routine examination are checked situation
| Project | The example number | The treatment group | The example number | Matched group | P | ||
| Unusually | Normally | Unusually | Normally | ||||
| The differential blood count stool routine examination | 200 200 | 75 200 | 125 0 | 70 70 | 220 70 | 48 0 | ＞0.05 ＞0.05 |
Through x
2Check, two groups of patient's differential blood counts, stool routine examination inspection situations compare no difference of science of statistics (P＞0.05).
Situation is checked in have loose bowels (damp-heat syndrome) two groups of differential blood counts, stool routine examination of table 6-2
| Project | The example number | The treatment group | The example number | Matched group | P | ||
| Unusually | Normally | Unusually | Normally | ||||
| The differential blood count stool routine examination | 100 100 | 29 100 | 71 0 | 30 30 | 10 30 | 20 0 | ＞0.05 ＞0.05 |
Through x
2Check, two groups of patient's differential blood counts, stool routine examination inspection situations compare than no difference of science of statistics (P＞0.05).
Two, diagnosis and dialectical standard
(1) tcm diagnosis: (according to high Chinese medicine universities and colleges' teaching materials " Chinese Internal Medicine " dysentery, the relevant chapters and sections of having loose bowels).
Dysentery is that the red white pus and blood of dysentery is a primary symptom, is mainly in summer and autumn with stomachache, tenesmus.The many gas damp and hot by being subjected to outward, that epidemic disease is malicious of primary disease, internal injury diet raw food, impairing the spleen and stomach and internal organs and form.
Having loose bowels is meant that defecation frequency increases, and feces is thin, even gushes as water sample.All can take place throughout the year, summer and autumn see more.
(2) Chinese medical discrimination: damp-heat syndrome
1, have loose bowels urgent or rush down and not well, it is yellowish-brown and smelly to defecate.
2, tenesmus, dysentery is red assorted mutually in vain.
3, burning sensation of the anus.
4, dysphoria with smothery sensation is thirsty.
5, stomachache.
6, oliguria with reddish urine.
7, yellowish fur.
8, soft and rapid pulse or sliding number.
(3) include the case standard in
Meet have loose bowels, the patient of dysentery diagnosis and Chinese medical discrimination standard, can include the test case in.
(4) get rid of case standard (comprising inadaptation or rejecting standard)
1, gestation or women breast-feeding their children are to this medicine allergy sufferers at under-18s or over-65s the age.
2, be associated with serious primary disease such as liver, kidney and hemopoietic system, psychotic.
3, all standards of including in that do not meet, not medication in accordance with regulations can't be judged that curative effect or data are not congruent to affect the treatment or safety judgement person.
Three, observational technique
(1) single at random blind method controlled trial is taked in this observation, matched group is no less than 1: 3 with the ratio of treatment group case load, the method of simple randomization grouping is adopted in the case grouping, with qualified study subject by the pro rate of 1: 1 or 1: 3 in matched group and treatment group, tried case and require some inpatient, clinic case is wanted strict control variable factor.
(2) clinical treatment group (1 group): damp and hot, for oral administration, each 5, every day 3 times, 1 week of logotype.
(3) matched group (2 groups): add the flavor Xianglian Wan, each 6 grams, serve on for 1 week at every day 3 times.
Four, observation index
(1) safety observation:
1, general health check-up project.
2, blood, urine, just routine test.
3, liver function.
(2) health giving quality observation:
1, stool character: bloody purulent stool, Mucous Stool, rare water are just.
2, stool routine examination inspection: erythrocyte, leukocyte and pyocyte quantity, indigestion food fiber in the stool.
3, primary symptom, sign change.
(3) untoward reaction:
Whether primary part observation causes that blood pressure reduces, dizzy, erythra and whether anaphylaxis etc. is arranged.And with itemized record such as its extent of reaction, time of occurrence, treatment measures in observing case history, and with regard to untoward reaction and the relation between the medicine make judgement (as relevant, may be relevant, irrelevant, can not affirm), and the case that untoward reaction is ended should be made a follow-up survey itemized record result.
(4) observe requirement:
In strict accordance with the plan requirement, record faithfully, before treatment (during prescription on individual diagnosis), treat the 4th day, the 7th day difference observed and recorded once.Respectively carry out once before and after the treatment on three big routines, Chest X-rays, liver, renal function, the electrocardiogram detection principle, can detect at any time if necessary, viewing duration must not add with other treatment medicine or other treatment means.Though it is effective to take medicine, add and use other related drugs, can't judge curative effect person, make case and reject processing.Take medicine the invalid drug withdrawal or the person that uses other medicines instead more than 4 days by invalidation, must not reject.
Five, curative effect determinate standard
Clinical recovery: Syndrome in TCM marquis's 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.
Six, result
(1) total effects: see (table 7-1, table 7-2)
Two groups of total effectses of table 7-1 dysentery (damp-heat syndrome) relatively
| Group | The example number | Clinical recovery (%) | Produce effects (%) | Effectively (%) | Invalid (%) | Total effective rate (%) |
| Treatment group matched group | 200 70 | 80(40.00) 18(25.71) | 47(23.50) 22(31.43) | 52(26.00) 20(28.57) | 21(10.50) 10(14.29) | (89.50) (85.71) |
Treatment group cure-remarkable-effectiveness rate 63.50%, total effective rate 89.50%, matched group cure-remarkable-effectiveness rate 57.14%, total effective rate 85.71%.
Analyze through Ridit, two groups of treatment back curative effects compare no difference of science of statistics (P＞0.05).
Table 7-2 has loose bowels (damp-heat syndrome) two groups of total effectses relatively
| Group | The example number | Clinical recovery (%) | Produce effects (%) | Effectively (%) | Invalid (%) | Total effective rate (%) |
| Treatment group matched group | 120 30 | 33(33.00) 6(20.00) | 31(31.00) 9(30.00) | 28(28.00) 7(23.33) | 8(8.000) 8(26.67) | (92.00) (73.33) |
Treatment group cure-remarkable-effectiveness rate 64.00%, total effective rate 92.00%, matched group cure-remarkable-effectiveness rate 50.00%, total effective rate 73.33%.
Analyze through Ridit, two groups of treatment back curative effects compare, and the treatment group is better than matched group significant difference (P＜0.05).
(2) different course of disease curative effects: see (table 8-1, table 8-2)
Two groups of different course of disease curative effects of table 8-1 dysentery (damp-heat syndrome) relatively
| The course of disease | The example number | The treatment group | Total effective rate (%) | The example number | Matched group | Total effective rate (%) | ||||||
| Clinical recovery | Produce effects | Effectively | Invalid | Clinical recovery | Produce effects | Effectively | Invalid | |||||
| ≤ 3 days 3 days～1 week＞1 weeks | 124 61 15 | 49 26 5 | 30 12 5 | 34 16 2 | 11 7 3 | (91.13) (88.52) (80.00) | 37 26 7 | 10 7 1 | 12 8 2 | 10 8 2 | 5 3 2 | (86.49) (88.46) (71.43) |
Analyze through Ridit, treatment is organized between the variant course of disease curative effect relatively, and two groups of different course of disease curative effects no difference of science of statistics (P＞0.05) relatively.
Table 8-2 has loose bowels (damp-heat syndrome) two groups of different course of disease curative effects relatively
| The course of disease | The example number | The treatment group | Total effective rate (%) | The example number | Matched group | Total effective rate (%) | ||||||
| Clinical recovery | Produce effects | Effectively | Invalid | Clinical recovery | Produce effects | Effectively | Invalid | |||||
| ≤ 3 days 3 days～1 week＞1 weeks | 68 24 8 | 22 10 1 | 24 5 2 | 18 7 3 | 4 2 2 | (94.12) (91.67 (75.00) | 16 9 5 | 4 1 1 | 5 3 1 | 3 2 2 | 4 3 1 | (75.00) (66.67) (80.00) |
Analyze through Ridit, between two groups and in each group between the different courses of disease curative effect relatively, and two groups of different course of disease curative effects no difference of science of statistics (P＞0.05) relatively.
(3) symptom curative effect: see (table 9-1, table 9-2)
Two groups of symptom curative effects of table 9-1 dysentery (damp-heat syndrome) relatively
| Symptom | The example number | The treatment group | Total effective rate (%) | The example number | Matched group | Total effective rate (%) | P | ||||||
| Disappear | Produce effects | Effectively | Invalid | Disappear | Produce effects | Effectively | Invalid | ||||||
| Have loose bowels urgently let out and the rare water of the thirsty scanty drak urine stool red white Mucous Stool of yellowish-brown and smelly diarrhea of not well tenesmus burning sensation of the anus stomachache dysphoria with smothery sensation just | 49 148 193 167 200 174 163 26 180 192 22 | 24 41 101 43 118 36 33 5 76 89 7 | 14 50 45 42 57 36 37 9 60 53 6 | 6 43 30 63 17 62 68 7 37 39 7 | 5 14 17 19 8 140 25 5 7 11 2 | (89.80) (90.54) (91.19) (88.62) (96.00) (77.01) (84.66) (80.77) (96.11) (94.27) (90.91) | 14 53 67 63 70 60 56 10 61 67 7 | 5 14 26 24 16 17 19 4 19 20 2 | 2 13 20 14 18 17 15 3 17 15 2 | 4 14 11 17 24 15 11 1 14 22 1 | 3 12 10 8 12 11 11 2 11 10 2 | (78.57) (77.36) (85.07) (87.30) (82.86) (81.67) (80.36) (80.00) (81.97) (85.17) (71.43) | ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 |
Analyze through Ridit, the treatment group is better than matched group (P＜0.05) to red white, the Mucous Stool symptom curative effect of stomachache, dysentery, and significant difference is arranged; Two groups of curative effects of all the other symptoms are compared no difference of science of statistics (P＞0.05).
Table 9-2 has loose bowels (damp-heat syndrome) two groups of symptom curative effects relatively
| Symptom | The example number | The treatment group | Total effective rate (%) | The example number | Matched group | Total effective rate (%) | P | ||||||
| Disappear | Produce effects | Effectively | Invalid | Disappear | Produce effects | Effectively | Invalid | ||||||
| Have loose bowels urgently let out and the rare water of the thirsty scanty drak urine stool red white Mucous Stool of yellowish-brown and smelly diarrhea of not well tenesmus burning sensation of the anus stomachache dysphoria with smothery sensation just | 85 86 2 88 100 91 65 59 0 0 41 | 31 33 0 32 51 24 13 13 0 0 12 | 19 17 0 33 17 30 21 31 0 0 17 | 27 30 1 15 28 29 22 12 0 0 10 | 8 6 1 8 4 8 9 3 0 0 2 | (90.59) (93.02) (50.00) (90.91) (96.00) (91.21) (86.15) (94.92) (0) (0) (95.12) | 24 26 0 28 30 240 16 21 0 0 9 | 45 6 0 6 5 3 2 3 0 0 2 | 6 9 0 10 7 10 2 7 0 0 3 | 3 4 0 7 8 6 4 3 0 0 2 | 11 7 0 5 10 5 8 8 0 0 2 | (54.17) (73.08) (0) (82.14) (66.67) (79.17) (50.00) (61.90) (0) (0) (77.78) | ＜0.05 ＞0.05 ＞0.05 ＞0.05 ＜0.05 ＞0.05 ＜0.05 ＜0.05 ＞0.05 ＞0.05 ＞0.05 |
Analyze through Ridit, the treatment group is urgent to having loose bowels, stomachache, oliguria with reddish urine, stool are yellowish-brown and smelly, the symptom curative effect be better than matched group (P＜0.05), significant difference is arranged; All the other symptom curative effects are compared no difference of science of statistics (P＞0.05) for two groups.
(4) tongue, pulse condition change: see (table 10-1, table 10-2)
Two groups of tongues of table 10-1 dysentery (damp-heat syndrome), pulse condition change
| Group | Picture of the tongue | Pulse condition | ||||
| Unusual before treating | Improve (%) before the treatment | Treat the back and change normal (%) | Unusual before treating | Improve (%) before the treatment | Treat the back and change normal (%) | |
| Treatment group matched group | 194 67 | 89(45.88) 25(37.31) | 48(24.74) 15(22.39) | 200 17 | 69(34.50) 17(24.29) | 43(21.50) 12(17.14) |
Through x
2Check, two groups of treatment back tongues, pulse conditions change relatively no difference of science of statistics (P＞0.05).
Have loose bowels (damp-heat syndrome) two groups of tongues, pulse condition of table 10-2 change
| Group | Picture of the tongue | Pulse condition | ||||
| Unusual before treating | Improve (%) before the treatment | Treat the back and change normal (%) | Unusual before treating | Improve (%) before the treatment | Treat the back and change normal (%) | |
| Treatment group matched group | 194 67 | 89(45.88) 25(37.31) | 48(24.74) 15(22.39) | 200 17 | 69(34.50) 17(24.29) | 43(21.50) 12(17.14) |
Through x
2Check, two groups of treatment back tongues, pulse conditions change relatively no difference of science of statistics (P＞0.05).
(5) hemogram, stool routine examination inspection change: see (table 11-1, table 11-2)
Table 11-1 dysentery (damp-heat syndrome) two groups of numeration of leukocyte classification, stool routine examination inspections change
| Group | Picture of the tongue | Pulse condition | ||||
| Unusual before treating | Improve (%) before the treatment | Treat the back and change normal (%) | Unusual before treating | Improve (%) before the treatment | Treat the back and change normal (%) | |
| Treatment group matched group | 75 22 | 33(44.00) 9(40.91) | 25(33.33) 15(27.27) | 200 70 | 92(46.00) 29(41.43) | 94(47.00) 20(28.57) |
Through x
2Check, the improvement rate of treatment group treatment back numeration of leukocyte classification and change normal rate and matched group compares no difference of science of statistics (P＞0.05); The normal rate of commentaries on classics of treatment group treatment back stool routine examination and matched group relatively have significant difference (P＜0.05).
Table 11-2 has loose bowels, and (damp-heat syndrome) two groups of numeration of leukocyte are classified, stool routine examination inspections change
| Group | Picture of the tongue | Pulse condition | ||||
| Unusual before treating | Improve (%) before the treatment | Treat the back and change normal (%) | Unusual before treating | Improve (%) before the treatment | Treat the back and change normal (%) | |
| Treatment group matched group | 29 67 | 89(45.88) 25(37.31) | 48(24.74) 15(22.39) | 200 17 | 69(34.50) 17(24.29) | 43(21.50) 12(17.14) |
Through x
2Check, the improvement rate of treatment group treatment back numeration of leukocyte classification and change normal rate and matched group compares no difference of science of statistics (P＞0.05); The treatment group is treated the improvement rate of back stool routine examination and is changeed normal rate and the matched group comparison, and significant difference (P＜0.05) is arranged.
(6) age and curative effect: see (table 12-1, table 12-2)
Table 12-1 dysentery (damp-heat syndrome) treatment group age and therapeutic effect relationship
| Age (year) | The example number | Recovery from illness | Produce effects | Effectively | Invalid | Total effective rate (%) | P |
| 18～30 31～50 51～65 | 95 72 33 | 43 24 13 | 20 20 7 | 22 21 9 | 10 7 4 | 89.47 90.28 87.88 | ＞0.05 |
Analyze through Ridit, no difference of science of statistics (P＞0.05) is compared to all ages and classes section patient curative effect in treatment group treatment back.
Table 12-2 have loose bowels (damp-heat syndrome) treatment group age and therapeutic effect relationship
| Age (year) | The example number | Recovery from illness | Produce effects | Effectively | Invalid | Total effective rate (%) | P |
| 18～30 31～50 51～65 | 50 31 19 | 20 7 6 | 15 11 5 | 13 10 5 | 2 3 3 | 96.00 90.32 84.21 | ＞0.05 |
Analyze through Ridit, no difference of science of statistics (P＞0.05) is compared to all ages and classes section patient curative effect in treatment group treatment back.
(7) two kinds of curative effect of disease: see (table 13)
Two kinds of curative effect of disease of table 13 relatively
| Disease | The example number | Recovery from illness | Produce effects | Effectively | Invalid | Total effective rate (%) |
| Dysentery | 100 200 | 33 80 | 31 47 | 28 52 | 8 21 | (92.00) (89.50) |
Analyze through Ridit, two kinds of curative effect of disease compare no difference of science of statistics (P＞0.05).
(8) safety is observed
1, untoward reaction: the treatment group is not found side effect and anaphylaxis during clinical observation.
2, lab testing: except that routine blood test, just conventional meeting the abnormal change of dysentery, do not find other ANOMALOUS VARIATIONS before and after the treatment.Routine urinalysis, liver function and Electrocardioscopy there is no abnormal change.
Seven, model case
Example one: open *, the man, 21 years old, individuality, Shijiazhuang City Pingshan County people was in first visit on July 26 in 1998.The patient is watery stool because of diarrhoea, stomachache, stool, and day rushes down 7-8 time, once in local clinic diagnosis and treatment, gives oral " HUOXIANG ZHENGQI SHUI " treatment, and the state of an illness is not felt any better, and comes me institute to go to a doctor.The patient is the crapulence cold drink before 4 days, gastral cavilty portion discomfort, and the stomachache that occurs having loose bowels is rushed down down urgently, rushes down and not well, rushes down back alleviation of pain, burning sensation of the anus, oliguria with yellow urine.Red tongue, yellow and greasy fur, soft and rapid pulse.
Have a medical check-up: 37.2 ℃ of T, P 82 times/minute, BP110/80mmHg; Cardiopulmonary (one), abdomen is soft, gastral cavilty portion tenderness (+), no rebound tenderness, bowel sound hyperaction; Lab testing: routine blood test: RBC 4.3 * 10
12/ L, WBC10.0 * 10
9/ L, N56%; Just conventional: loose stool, accidental leukocyte under the mirror.Tcm diagnosis: have loose bowels (syndrome of dampness-heat in large intestine).Be used for oral damp and hot, each 5, every day 3 times, serve on for 1 week.Behind the medicine 3 days, patient's number of times of suffering from diarrhoea reduced, and every day 3-4 time, gastral cavilty portion is uncomfortable to disappear, and suffering from abdominal pain obviously alleviates.Took medicine 7 days, appetite increases, and stool is configured as soft stool, and all diseases disappear, pale tongue, white and thin fur, pulse condition string and strong.Look into: just conventional microscopy (); Clinical genus is cured.
Example two: Zhao * *, the man, 28 years old, main cause stomachache, diarrhoea, stool containing pus and blood, tenesmus 2 days were generated heat 1 day, went to a doctor on August 9th, 1998.The patient crossed before 2 days and drinks cold medicated beer and stomachache, diarrhoea, 8-10 time/day of stool appear in the greasy back of feed raw food, and a small amount of mucus and pus and blood are arranged, and with low grade fever, obeyed medicines such as furazolidone, norfloxacin certainly, and symptom has alleviation slightly.Look into: T38.1 ℃, P92 time/minute.Cardiopulmonary (one) abdomen is soft, umbilicus week and left lower quadrant tenderness (++), and borborygmus are hyperfunction.Blood routine examination WBC11.2 * 10
9, N78%.Stool microscopy: visible leukocyte, erythrocyte, pyocyte.The patient is conscious, and dysphoria with smothery sensation is thirsty, oliguria with reddish urine, and it is not well to defecate, red tongue, yellowish fur, slippery and rapid pulse.Western medicine diagnose: bacillary dysentery.Tcm diagnosis: dysentery (damp-heat syndrome).Give damp and hot 5, oral, every day three times.Took medicine 1 day, the patient is conscious, and stomachache alleviates.Took medicine the 3rd day, stool mucus, pus and blood obviously reduce, and times of defecation is reduced to 3-4 time/day, and body temperature is reduced to 37.4 ℃.Took medicine 7 days, patient's stomachache, diarrhoea, tenesmus, stool containing pus and blood mucus all disappear, and body temperature is normal.Look into: routine blood test is normal, the stool routine examination chemical examination, and rarely seen small quantities of leukocytes is not seen pyocyte, erythrocyte.The sick clinical recovery that belongs to.
Eight, conclusion
Damp and hot is used for the treatment of have loose bowels (damp-heat syndrome), the syndrome of dampness-heat in large intestine of dysentery (damp-heat syndrome), to add flavor Xianglian Wan (production of Chinese medicine two factories of Beijing group of Tongrentang) is the contrast medicine, by Affiliated Hospital of Hebei Academy of Medical Science, No.1 Hospital, Shanxi Medical Univ, from the 6-11 month in 1998 it having been carried out clinical verification, adopt the method for single blind contrast at random to investigate its curative effect and untoward reaction.Learn by statistics and handle, now the Supreme People's Court and the Supreme People's Procuratorate's Clinical results is reported as follows:
(1) dysentery (damp-heat syndrome) observed result:
1, clinical observation 270 examples, wherein 200 examples are organized in treatment, cure-remarkable-effectiveness rate 63.50%, total effective rate 89.50%, matched group 70 examples, cure-remarkable-effectiveness rate 57.14%, 85.71%, two group of curative effect of total effective rate is relatively, learn by statistics and handle two groups of curative effects similar (P＞0.05), no difference of science of statistics.
2, treatment group has significant difference (P＜0.05) for stomachache, red white, the Mucous Stool symptom curative effect comparison of dysentery, and the treatment group is better than matched group.
3, treatment group changes normal rate for stool routine examination and matched group compares, and significant difference (P＜0.05) is arranged, and the treatment group is better than matched group.
(2) (damp-heat syndrome) observed result of having loose bowels:
1, clinical observation 130 examples, wherein 100 examples are organized in treatment, cure-remarkable-effectiveness rate 64.00%, total effective rate 92.00%, matched group 30 examples, cure-remarkable-effectiveness rate 50.00%, total effective rate 73.33%, two groups of curative effects are learned processing (P＜0.05) more by statistics, and significant difference is arranged, and the treatment group is better than matched group.
2, treatment group is urgent for having loose bowels, stomachache, oliguria with reddish urine, the yellowish-brown and smelly symptom curative effect of stool relatively, significant difference (P＜0.05) is arranged, the treatment group is better than matched group.
3, treatment group is for stool routine examination improvement rate and change normal rate and the matched group comparison, and significant difference (P＜0.05) is arranged, and the treatment group is better than matched group.
(3) through clinical observation and checking, damp and hot treatment had loose bowels and all do not found untoward reaction such as toxic and side effects and allergy with dysentery.
Clinical results shows: damp and hot syndrome of dampness-heat in large intestine determined curative effect to having loose bowels with dysentery, and safety, reliable.
Experimental example 2 pharmacodynamic experiments
1, test objective
Observe damp and hot heat clearing away, antidiarrheal, analgesia and bacteriostasis, for clinical practice provides reference.
2, medicine and instrument
Damp and hot (include Radix Et Rhizoma Rhei, Rhizoma Atractylodis, Radix Aconiti, Rhizoma Et Radix Notopterygii, Semen Arecae, Halloysitum Rubrum etc., lot number is 0111011, and adult's consumption is oral 2-3 time of every day, and each 4, every heavily is 434mg) provided by Xingning City, Guangdong Province jewel pharmaceutcal corporation, Ltd; Day and night the hundred clothes sheet (lot number 0203561, every contains acetaminophen 500mg) of giving repeated exhortations is executed expensive precious pharmaceutical Co. Ltd by Shanghai and is produced; Dry yeast (lot number is 011013) is produced by Guangdong Dan Baoli Yeast Co., Ltd; Aspirin sheet (lot number is 20020101) is produced by Harbin Glarey Pharmaceutical Co., Ltd; Dioctahedral smectite (lot number is H33Y, the 3g/ bag) is produced by France beneficial Pu Sheng drugmaker; Medicinal castor oil (lot number is 001201) is produced by asparagus cochinchinensis field, Hubei pharmaceutcal corporation, Ltd; All the other reagent are commercially available analytical pure.
Omron thermometer (precision is 0.05 ℃) is produced by Japanese Omron Corp.
3, experimental animal
Healthy no pregnant NIH mice (quality certification number be 2001A044) and SD rat (quality certification number be 2001A046) and standard feed thereof provide by Guangdong Medical Lab Animal Center.
4, method and result
4.1 heat clearing away effect to rat fever due to the dry yeast
[1]
Get 60 of the SD rats of body weight 180-220g, be divided into 6 groups at random, 10 every group, equal male and female half and half.Wherein 3 groups are damp and hot high, medium and low dosage group, and dosage sees Table 1, are equivalent to 20 times, 10 times of Coming-of-Age Day consumption 72.3mg/kg and 5 times (this experiment becomes body weight for humans by 60kg by oral 10 of adult every day) respectively; Model group and blank group give isopyknic normal saline, and irritate stomach 1 above-mentioned 5 groups of every days, for three days on end; Positive controls gives day and night hundred clothes and gives repeated exhortations (being calculated as 250mg/kg by acetaminophen), irritates stomach 1 time.Last is respectively organized rat all immediately in back subcutaneous injection dry yeast distilled water suspension (20g/100ml after irritating stomach except that the blank group, the 1ml/100g Mus is heavy), respectively organize behind 1h, 2h, 3h, 4h, 5h, the 6h after the record administration rat the body temperature increasing degree (℃), the results are shown in Table 1.
Damp and hot of table 1 to dry yeast cause rat fever the heat clearing away effect (X ± SD, n=10)
| Group | Dosage (g/kg) | Body temperature increasing degree behind the rat skin lower injection dry yeast (℃) | |||||
| 1h | 2h | 3h | 4h | 5h | 6h | ||
| Damp and hot group of blank group model group acetaminophen group | - - 0.25 0.362 0.723 1.45 | 0.28±0.12 0.33±0.14 0.24±0.11 0.31±0.17 0.32±0.16 0.22±0.13 | 0.32±0.06* 0.45±0.15 0.29±0.10* 0.44±0.08 0.39±0.15 0.33±0.14 | 0.40±0.10** 0.91±0.38 0.40±0.21** 0.94±0.23 0.57±0.27* 0.55±0.18* | 0.54±0.19* 0.74±0.16 0.27±0.09** 0.61±0.22 0.60±0.17 0.44±0.12** | 0.34±0.11** 1.90±0.33 0.58±0.13** 1.58±0.58 1.52±0.48 1.26±0.28** | 0.33±0.12** 2.20±0.42 0.41±0.13** 1.89±0.41 1.88±0.31 1.37±0.34** |
Compare * P＜0.05 * * P＜0.01 with model group, down together
Table 1 result shows that hundred clothes are given repeated exhortations and damp and hot rat fever that the subcutaneous injection dry yeast is caused of high dose group has tangible antagonism, and damp and hot of middle dosage group also has tangible antagonism behind 3h, show that hundred clothes are given repeated exhortations and damp and hot have the heat clearing away effect.
4.2 to the antagonism of Oleum Ricini induced mice diarrheal
[2]
Get body weight and be 60 of the NIH mices of 18-22g, grouping and dosage are the same, and positive controls gives dioctahedral smectite 2g/kg once; Last is irritated stomach after half an hour, except that the blank group is irritated the stomach normal saline, all irritates stomach for all the other 5 groups and only gives medicinal castor oil 0.2ml/.Animal is placed respectively in the transparent observing cage that is lined with diameter 15cm filter paper, and every interval was changed packing paper in 1 hour and was counted the diarrhea of mouse number of times, and the accumulation of different time diarrhoea number of times the results are shown in Table 2 between comparable group.
Damp and hot of table 2 to Oleum Ricini cause diarrhea of mouse antagonism (X ± SD, n=10)
| Group | Dosage (g/kg) | Mice accumulation diarrhoea number of times (inferior) | |||
| 1h | 2h | 3h | 4h | ||
| Damp and hot group of blank group model group smecta group | - - 2.0 0.362 0.723 1.45 | 5.20±1.81 7.40±4.67 4.30±2.36 4.60±1.26 5.30±1.64 4.80±2.62 | 8.90±1.97** 25.40±7.75 12.40±2.17** 22.10±4.01 18.70±2.45* 14.60±4.38** | 14.10±4.04** 33.20±7.21 17.70±3.74** 29.2±8.36 26.60±4.40* 19.50±3.89** | 16.00±4.32** 36.00±6.82 19.30±4.00** 32.60±8.78 28.5±6.38* 21.60±5.36** |
Table 2 result shows that dioctahedral smectite and damp and hot height, middle dosage all have tangible antagonism to the diarrhea of mouse that Oleum Ricini causes, shows that dioctahedral smectite and damp and hot have antidiarrheal efficacy.
4.3 Dichlorodiphenyl Acetate causes that mice pain turns round the influence of body
[3]
Get 50 of the NIH mices of 18-22g, be divided into 5 groups at random, male and female half and half, damp and hot high, medium and low dosage group irritated stomach and given damp and hot (dosage is the same), the blank group gives normal saline, more than respectively organize administration every day 1 time, continuous three days; Positive controls gives aspirin sheet 0.01g/kg once; Behind the last gastric infusion 1h, mouse peritoneal is injected 0.6% acetic acid 0.2ml/20g, and that observes and write down mice in 15 minutes turns round the body number of times, the results are shown in Table 3.
Damp and hot Dichlorodiphenyl Acetate of table 3 cause mice pain turn round the influence of body (X ± SD, n=10)
| Group | Dosage (g/kg) | Mice pain is turned round the number of times (inferior) of body |
| The wet sheet group of blank group aspirin group heat | - 0.01 0.362 0.723 1.45 | 12.90±4.93 4.70±1.57** 10.90±2.96 8.20±2.53* 6.70±1.83** |
Table 3 can find out, the mice pain that aspirin and damp and hot middle high dose Dichlorodiphenyl Acetate causes is turned round body all tangible antagonism.Prompting aspirin and damp and hot has the analgesic effect.
4.4 bacteriostatic test (liquid tube bacteriostatic method)
[4]
4.4.1 antibacterial bacteriostatic test
Get damp and hot of sterilization, with bactericidal nurishing meat soup be mixed with 0.2,0.1,0.05,0.025, the 0.0125g/ml isoconcentration, parallel 4 pipes of doing of each concentration, every pipe 1ml, the about 50-100 of fresh viable bacteria that adds corresponding bacterial strain (seeing Table 4) in each pipe respectively is individual, put 37 ℃ and cultivate 18-24h, on the corresponding isolation medium flat board of each bacterial strain, rule, put 37 ℃ of cultivation 18-24h again and observe whether bacteria growing is arranged, the highest drug dilution degree that each antibacterial does not grow is the minimum inhibitory concentration (MIC) of this medicine, sets up feminine gender and positive control simultaneously.Various bacterial strains that above-mentioned test is adopted and corresponding culture medium are Nat'l Pharmaceutical ﹠ Biological Products Control Institute to be provided, and the results are shown in Table 4.
4.4.2 fungus bacteriostatic test
Get damp and hot of sterilization, be diluted to above-mentioned concentration with the sterilization fungi culture medium, basic skills is the same, and bacterial strain uses therefor is a candida albicans, and twice cultivation temperature is 25-28 ℃, sets up feminine gender and positive control simultaneously.Above-mentioned bacterial strains and corresponding culture medium are Nat'l Pharmaceutical ﹠ Biological Products Control Institute to be provided, and the results are shown in Table 4.
The bacteriostatic test result that table 4 is damp and hot
| Strain | Damp and hot concentration (g/kg) | Negative control | Positive control | ||||
| 0.2 | 0.1 | 0.05 | 0.025 | 0.0125 | |||
| Escherichia coli (44102) bacillus pyocyaneus (10104) Salmonellas (50094) golden Portugal bacterium (26003) Candida albicans (98001) | - - - - - | + + - - - | + + + + - | + + + + + | + + + + + | - - - - - | + + + + + |
Table 4 result shows: damp and hot all has certain inhibitory action to 5 kinds of test organismss when 0.2g/ml, especially to Candida albicans, its MTC is 0.05g/ml, shows that damp and hot has certain bacteriostasis.
5, conclusion
Damp and hot has significantly heat clearing away, antidiarrheal, analgesic activity, escherichia coli, golden Fructus Vitis viniferae, bacillus pyocyaneus, Salmonella and Candida albicans is also had certain bacteriostasis.
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment 1 tablet
Radix Et Rhizoma Rhei 340g Flos Sophorae (parch to black) 34g Rhizoma Atractylodis (bubble) 255g
Cacumen Platycladi (parch to black) 34g Rhizoma Et Radix Notopterygii 170g Flos Lonicerae 85g
Radix Aconiti Preparata 170g Halloysitum Rubrum (system) 84g Semen Armeniacae Amarum 60g
Semen Arecae (stir-fry) 68g
More than ten the flavor, get Radix Et Rhizoma Rhei, Rhizoma Atractylodis, each 20g of Rhizoma Et Radix Notopterygii, Halloysitum Rubrum (system), each 5g of Semen Armeniacae Amarum, Radix Aconiti 15g, Flos Sophorae 10g, Cacumen Platycladi 6g are ground into fine powder, and be standby.The residue Radix Et Rhizoma Rhei is according to method under fluid extract and extractum (an appendix I of Chinese Pharmacopoeia version in 2000 the O) item, make solvent with 60% ethanol, slowly percolation is collected percolate, reclaim under reduced pressure is to not having the alcohol flavor and being condensed into the thick paste that relative density is 1.35-1.45 (50-80 a ℃), and is standby.Residue Rhizoma Atractylodis, Rhizoma Et Radix Notopterygii add Flos Lonicerae and extract volatile oil with steam distillation, and be standby; Aqueous solution after distillation device is in addition preserved; Medicinal residues and Semen Arecae and remaining Radix Aconiti, Semen Armeniacae Amarum, Halloysitum Rubrum, Cacumen Platycladi, Flos Sophorae merge, decoct with water three times, and 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filtered, and filtrate adds the aqueous solution after the distillation, being condensed into relative density is the thick paste of 1.35-1.45 (50-80 ℃), adds above-mentioned fine powder and thick paste, mixing, make granule, drying sprays into volatile oil, mixing, airtight, tabletting, sugar coating promptly, is made 1000.Function cures mainly: heat clearing and damp drying, relieving dysentery with astringents.Be used for suffering from abdominal pain, have loose bowels, dysentery, belong to syndrome of dampness-heat in large intestine.Usage and dosage: oral, one time 4,2-3 time on the one.Taboo: be not taken by pregnant women.Specification: the heavy 0.25g of substrate
Embodiment 2 capsules
Radix Et Rhizoma Rhei 380g Flos Sophorae (parch to black) 40g Rhizoma Atractylodis (bubble) 270g
Cacumen Platycladi (parch to black) 45g Rhizoma Et Radix Notopterygii 190g Flos Lonicerae 100g
Radix Aconiti Preparata 190g Halloysitum Rubrum (system) 100g Semen Armeniacae Amarum 80g
Semen Arecae (stir-fry) 85g
More than ten the flavor, get Radix Et Rhizoma Rhei, Rhizoma Atractylodis, each 20g of Rhizoma Et Radix Notopterygii, Halloysitum Rubrum (system), each 5g of Semen Armeniacae Amarum, Radix Aconiti 15g, Flos Sophorae 10g, Cacumen Platycladi 6g are ground into fine powder, and be standby.The residue Radix Et Rhizoma Rhei is according to method under fluid extract and extractum (an appendix I of Chinese Pharmacopoeia version in 2000 the O) item, make solvent with 60% ethanol, slowly percolation is collected percolate, reclaim under reduced pressure is to not having the alcohol flavor and being condensed into the thick paste that relative density is 1.35-1.45 (50-80 a ℃), and is standby.Residue Rhizoma Atractylodis, Rhizoma Et Radix Notopterygii add Flos Lonicerae and extract volatile oil with steam distillation, and be standby; Aqueous solution after distillation device is in addition preserved; Medicinal residues and Semen Arecae and remaining Radix Aconiti, Semen Armeniacae Amarum, Halloysitum Rubrum, Cacumen Platycladi, Flos Sophorae merge, and decoct with water 2 hours for the first time three times, 2 hours for the second time, 1 hour for the third time, collecting decoction, filter, filtrate adds the aqueous solution after the distillation, and being condensed into relative density is the thick paste of 1.35-1.45 (50-80 ℃), add above-mentioned fine powder and thick paste, mixing is made granule, drying sprays into volatile oil, mixing, airtight, make 1000 of capsules.
Embodiment 3 granules
Radix Et Rhizoma Rhei 310g Flos Sophorae (parch to black) 30g Rhizoma Atractylodis (bubble) 235g
Cacumen Platycladi (parch to black) 25g Rhizoma Et Radix Notopterygii 150g Flos Lonicerae 65g
Radix Aconiti Preparata 180g Halloysitum Rubrum (system) 70g Semen Armeniacae Amarum 50g
Semen Arecae (stir-fry) 50g
More than ten the flavor, get Radix Et Rhizoma Rhei, Rhizoma Atractylodis, each 20g of Rhizoma Et Radix Notopterygii, Halloysitum Rubrum (system), each 5g of Semen Armeniacae Amarum, Radix Aconiti 15g, Flos Sophorae 10g, Cacumen Platycladi 6g are ground into fine powder, and be standby.The residue Radix Et Rhizoma Rhei is according to method under fluid extract and extractum (an appendix I of Chinese Pharmacopoeia version in 2000 the O) item, make solvent with 60% ethanol, slowly percolation is collected percolate, reclaim under reduced pressure is to not having the alcohol flavor and being condensed into the thick paste that relative density is 1.35-1.45 (50-80 a ℃), and is standby.Residue Rhizoma Atractylodis, Rhizoma Et Radix Notopterygii add Flos Lonicerae and extract volatile oil with steam distillation, and be standby; Aqueous solution after distillation device is in addition preserved; Medicinal residues and Semen Arecae and remaining Radix Aconiti, Semen Armeniacae Amarum, Halloysitum Rubrum, Cacumen Platycladi, Flos Sophorae merge, and decoct with water 2 hours for the first time three times, 1.5 hours for the second time, 1 hour for the third time, collecting decoction, filter, filtrate adds the aqueous solution after the distillation, and being condensed into relative density is the thick paste of 1.35-1.45 (50-80 ℃), add above-mentioned fine powder and thick paste, mixing is made granule, drying sprays into volatile oil, mixing, airtight, promptly.
The method of quality control of embodiment 4 tablets
Assay: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 D), chromatographic condition and system suitability test, be filler with octadecylsilane chemically bonded silica: methanol-0.1% phosphoric acid solution (85: 15) is a mobile phase; The detection wavelength is 254nm.Number of theoretical plate calculates by the emodin peak should be not less than 2000.The preparation of reference substance solution, precision take by weighing emodin and the chrysophanol reference substance is an amount of, and the mixed solution that adds dehydrated alcohol-ethyl acetate (2: 1) is respectively made the solution that contains emodin 1 μ g, chrysophanol 2 μ g among every 1ml, promptly.20 of this product are got in the preparation of need testing solution, remove sugar-coat, and accurate the title decides, porphyrize (crossing sieve No. three), precision takes by weighing in right amount (being equivalent to 1 weight approximately), puts in the conical flask, the accurate ethanol 25ml that adds, close plug claims to decide weight, reflux 1 hour is put coldly, claims to decide weight, supply the weight that subtracts mistake with ethanol, filter, precision is measured subsequent filtrate 10ml, put in the conical flask, evaporate to dryness, residue add the mixed solution 15ml of 30% ethanol-hydrochloric acid (10: 1), reflux 1 hour, cooling rapidly is in the dislocation separatory funnel, extract 4 times with the chloroform jolting, each 15ml, combined chloroform liquid, evaporate to dryness, the mixed solution that residue adds dehydrated alcohol-ethyl acetate (2: 1) makes dissolving in right amount, in the dislocation 25ml measuring bottle, the mixed solution that adds dehydrated alcohol-ethyl acetate (2: 1) is diluted to scale, shakes up, filter with microporous filter membrane (0.45 μ m), promptly.Algoscopy, accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.Every of this product contains Radix Et Rhizoma Rhei with emodin (C
15H
10O
5) and chrysophanol (C
15H
10O
4) the total amount meter, must not be less than 0.15mg.
Differentiate: a. gets the need testing solution 20ml under [assay] item, and evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system.Get emodin, chrysophanol reference substance again, add ethyl acetate and make the mixed solution that every 1ml contains emodin 0.5mg, chrysophanol 1mg, product solution in contrast.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 10 μ l of above-mentioned three kinds of solution, put on same silica gel g thin-layer plate respectively, upper solution with petroleum ether (60-90 ℃)-Ethyl formate-formic acid (15: 5: 1) is developing solvent, 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 five identical orange-yellow fluorescence speckles; With the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle.B. get 10 of this product, remove sugar-coat; Porphyrize, the 10ml that adds diethyl ether, ultrasonic place 20 minutes filters, and filtrate is waved to 1ml, as need testing solution.Other gets Rhizoma Atractylodis 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 2000 B), draw above-mentioned need testing solution 20 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with petroleum ether (60-90 ℃)-ethyl acetate (50: 1) is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.C. get Rhizoma Et Radix Notopterygii control medicinal material 0.5g, make control medicinal material solution according to the preparation method of the control medicinal material solution under the item of [discriminating] (2).Other gets the isoimperatorin reference substance, adds diethyl ether to make the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, draw need testing solution 10 μ l and above-mentioned control medicinal material and each 1 μ l of reference substance solution under the item of [discriminating] (2), put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate (8: 2) is developing solvent, launches, and exhibition is apart from about 5cm, take out, drying, is developing solvent with petroleum ether (30-60 ℃)-butanone (8: 2) again, launches, exhibition is apart from about 10cm, 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.
Check: aconitine limit, get 8 of this product, remove sugar-coat, porphyrize, after 10% sodium carbonate liquor moistening, 50ml adds diethyl ether, supersound process 15 minutes filters, and filtrate is extracted 2 times with 2% hydrochloric acid solution jolting, each 30ml merges acid solution, regulates pH value to 12 with strong ammonia solution, extract 2 times with the ether jolting, each 30ml merges ether solution, extract 2 times with 2% hydrochloric acid solution jolting, each 30ml merges acid liquid, regulate pH value to 12 with strong ammonia solution, extract 2 times, each 30ml with the ether jolting, merge ether solution, evaporate to dryness, residue add methanol make in right amount the dissolving and move in the 2ml measuring bottle, add methanol and be diluted to scale, shake up, as need testing solution.Other gets the aconitine reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), accurate above-mentioned need testing solution 10 μ l, the reference substance solution 5 μ l of drawing, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate-diethylamine (8: 6: 1) is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of appearance should or speckle not occur less than the speckle of reference substance.
Claims (15)
1. Chinese medicine composition for the treatment of damp-heat in the large intestine disease is characterized in that this Chinese medicine composition made by following raw material medicaments:
Radix Et Rhizoma Rhei 300-400 weight portion Flos Sophorae 20-50 weight portion Rhizoma Atractylodis 220-280 weight portion
Cacumen Platycladi 20-50 weight portion Rhizoma Et Radix Notopterygii 140-200 weight portion Flos Lonicerae 50-110 weight portion
Radix Aconiti Preparata 140-200 weight portion Halloysitum Rubrum 50-110 weight portion Semen Armeniacae Amarum 35-90 weight portion
Semen Arecae 40-90 weight portion.
2. Chinese medicine composition as claimed in claim 1 is characterized in that this Chinese medicine composition made by following raw material medicaments:
Radix Et Rhizoma Rhei 340 weight portion Flos Sophoraes 34 weight portion Rhizoma Atractylodis 255 weight portions
Cacumen Platycladi 34 weight portion Rhizoma Et Radix Notopterygiis 170 weight portion Flos Loniceraes 85 weight portions
Radix Aconiti Preparata 170 weight portion Halloysitum Rubrums 84 weight portion Semen Armeniacae Amarums 60 weight portions
Semen Arecae 68 weight portions.
3. Chinese medicine composition as claimed in claim 1 is characterized in that this Chinese medicine composition made by following raw material medicaments:
Radix Et Rhizoma Rhei 380 weight portion Flos Sophoraes 40 weight portion Rhizoma Atractylodis 270 weight portions
Cacumen Platycladi 45 weight portion Rhizoma Et Radix Notopterygiis 190 weight portion Flos Loniceraes 100 weight portions
Radix Aconiti Preparata 190 weight portion Halloysitum Rubrums 100 weight portion Semen Armeniacae Amarums 80 weight portions
Semen Arecae 85 weight portions.
4. as the arbitrary described Chinese medicine composition of claim 1-3, it is characterized in that Flos Sophorae is the Flos Sophorae parch to black; Rhizoma Atractylodis are the Rhizoma Atractylodis infusion; Cacumen Platycladi is the Cacumen Platycladi parch to black; Halloysitum Rubrum is the system Halloysitum Rubrum; Semen Arecae is a Semen Arecae (parched).
5. the preparation method of Chinese medicine composition as claimed in claim 4, it is characterized in that this method is: above ten flavors, get Radix Et Rhizoma Rhei, Rhizoma Atractylodis, each 15-25 weight portion of Rhizoma Et Radix Notopterygii, Halloysitum Rubrum, each 3-8 weight portion of Semen Armeniacae Amarum, Radix Aconiti 10-25 weight portion, Flos Sophorae 5-15 weight portion, Cacumen Platycladi 3-10 weight portion, be ground into fine powder, standby; The residue Radix Et Rhizoma Rhei is made solvent with 50-70% ethanol, and slowly percolation is collected percolate, and reclaim under reduced pressure is to not having the alcohol flavor and be condensed into 50-80 ℃ of relative density the thick paste that is 1.30-1.50, and is standby; Residue Rhizoma Atractylodis, Rhizoma Et Radix Notopterygii add Flos Lonicerae and extract volatile oil with steam distillation, and be standby; Aqueous solution after distillation device is in addition preserved; Medicinal residues and Semen Arecae and remaining Radix Aconiti, Semen Armeniacae Amarum, Halloysitum Rubrum, Cacumen Platycladi, Flos Sophorae merge, decoct with water 2-4 time each 1-3 hour, collecting decoction, filter, filtrate adds the aqueous solution after the distillation, and the thick paste that to be condensed into 50-80 ℃ of relative density be 1.30-1.50 adds above-mentioned fine powder and thick paste, mixing, excipient direct through conventional operation or that adding is pharmaceutically accepted is made tablet, capsule, the granule of clinical acceptance.
6. the preparation method of Chinese medicine composition as claimed in claim 5, the preparation method that it is characterized in that tablet is: above ten flavors, get Radix Et Rhizoma Rhei, Rhizoma Atractylodis, each 20 weight portion of Rhizoma Et Radix Notopterygii, Halloysitum Rubrum, each 5 weight portion of Semen Armeniacae Amarum, Radix Aconiti 15 weight portions, Flos Sophorae 10 weight portions, Cacumen Platycladi 6 weight portions, be ground into fine powder, standby; The residue Radix Et Rhizoma Rhei is made solvent with 60% ethanol, and slowly percolation is collected percolate, and reclaim under reduced pressure is to not having the alcohol flavor and be condensed into 50-80 ℃ of relative density the thick paste that is 1.35-1.45, and is standby; Residue Rhizoma Atractylodis, Rhizoma Et Radix Notopterygii add Flos Lonicerae and extract volatile oil with steam distillation, and be standby; Aqueous solution after distillation device is in addition preserved; Medicinal residues and Semen Arecae and remaining Radix Aconiti, Semen Armeniacae Amarum, Halloysitum Rubrum, Cacumen Platycladi, Flos Sophorae merge, decoct with water three times, and 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filtered, filtrate adds the aqueous solution after the distillation, and the thick paste that to be condensed into 50-80 ℃ of relative density be 1.35-1.45 adds above-mentioned fine powder and thick paste, mixing is made granule, drying, spray into volatile oil, mixing, airtight, tabletting, sugar coating, promptly.
7. the method for quality control of Chinese medicinal composition preparation as claimed in claim 4, it is characterized in that the content assaying method in this method is: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test, be filler: 80-90 with octadecylsilane chemically bonded silica: 10-20 methanol-0.1% phosphoric acid solution is a mobile phase; The detection wavelength is 254nm; Number of theoretical plate calculates by the emodin peak should be not less than 2000; The preparation of reference substance solution, precision take by weighing emodin and the chrysophanol reference substance is an amount of, adds 1-3 respectively: the mixed solution of 1-2 dehydrated alcohol-ethyl acetate is made the solution that contains emodin 1 μ g, chrysophanol 2 μ g among every 1ml, promptly; 20 in present composition tablet is got in the preparation of need testing solution, removes sugar-coat, the accurate title, decide, and porphyrize is crossed sieve No. three, and precision takes by weighing and is equivalent to 1 weight in right amount, put in the conical flask accurate ethanol 25ml, the close plug of adding, claim to decide weight, reflux 1-2 hour, put cold, claim to decide weight, supply the weight that subtracts mistake with ethanol, filter, precision is measured subsequent filtrate 10ml, put in the conical flask, evaporate to dryness, residue add 30% ethanol-hydrochloric acid with 8-12: the mixed solution 15ml of 1-2 ratio, reflux 1-2 hour, cooling rapidly, in the dislocation separatory funnel, extract 4 times each 15ml with the chloroform jolting, combined chloroform liquid, evaporate to dryness, residue adds 1-3: the mixed solution of 1-2 dehydrated alcohol-ethyl acetate makes dissolving in right amount, in the dislocation 25ml measuring bottle, add 1-3: the mixed solution of 1-2 dehydrated alcohol-ethyl acetate is diluted to scale, shake up, filter with microporous filter membrane, promptly; Algoscopy, accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Present composition preparation per unit amount contains the total amount of Radix Et Rhizoma Rhei in emodin and chrysophanol, must not be less than 0.10-0.20mg.
8. the method for quality control of Chinese medicinal composition preparation as claimed in claim 7, the content assaying method that it is characterized in that tablet is: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test, be filler with octadecylsilane chemically bonded silica: methanol-0.1% phosphoric acid solution was a mobile phase in 85: 15; The detection wavelength is 254nm; Number of theoretical plate calculates by the emodin peak should be not less than 2000; The preparation of reference substance solution, precision take by weighing emodin and the chrysophanol reference substance is an amount of, and the mixed solution that adds 2: 1 dehydrated alcohol-ethyl acetates is respectively made the solution that contains emodin 1 μ g, chrysophanol 2 μ g among every 1ml, promptly; 20 of this product are got in the preparation of need testing solution, remove sugar-coat, the accurate title, decide, and porphyrize is crossed sieve No. three, and precision takes by weighing and is equivalent to 1 weight in right amount, put in the conical flask accurate ethanol 25ml, the close plug of adding, claim to decide weight, reflux 1 hour is put cold, claim to decide weight, supply the weight that subtracts mistake, filter with ethanol, precision is measured subsequent filtrate 10ml, puts in the conical flask evaporate to dryness, residue adds the mixed solution 15ml of 30% ethanol-hydrochloric acid with 10: 1 ratios, reflux 1 hour, cooling rapidly, in the dislocation separatory funnel, extract 4 times each 15ml with the chloroform jolting, combined chloroform liquid, the mixed solution that evaporate to dryness, residue add 2: 1 dehydrated alcohol-ethyl acetates makes dissolving in right amount, in the dislocation 25ml measuring bottle, the mixed solution that adds 2: 1 dehydrated alcohol-ethyl acetates is diluted to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly; Algoscopy, accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Every of this product contains the total amount of Radix Et Rhizoma Rhei in emodin and chrysophanol, must not be less than 0.15mg.
9. the method for quality control of Chinese medicinal composition preparation as claimed in claim 4; It is characterized in that discrimination method in the method comprises one or more in the following discriminating: the preparation of a. need testing solution; Get 20 in present composition tablet; Remove sugar-coat; Accurately weighed; Porphyrize is crossed sieve No. three, and precision takes by weighing and is equivalent in right amount 1 weight, puts in the conical flask; The accurate ethanol 25ml that adds; Close plug, weighed weight adds hot reflux 1-2 hour; Let cool; Weighed weight is supplied the weight that subtracts mistake with ethanol, filters; Precision is measured subsequent filtrate 10ml; Put in the conical flask, evaporate to dryness, residue add 30% ethanol-hydrochloric acid with 8-12: the mixed solution 15ml of 1-2 ratio; Add hot reflux 1-2 hour; Rapidly cooling in the dislocation separatory funnel, is extracted 4 times with the chloroform jolting; Each 15ml; Combined chloroform liquid, evaporate to dryness, residue adds 1-3: the mixed solution of 1-2 absolute ethyl alcohol-ethyl acetate makes dissolving in right amount; In the dislocation 25ml measuring bottle; Add 1-3: the mixed solution of 1-2 absolute ethyl alcohol-ethyl acetate is diluted to scale, shakes up, and filters with miillpore filter; Get 20ml; Evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system; Get emodin, chrysophanol reference substance again, add ethyl acetate and make the mixed solution that every 1ml contains emodin 0.5mg, chrysophanol 1mg, product solution in contrast; According to thin layer chromatography test, draw each 10 μ l of above-mentioned three kinds of solution, put on same silica gel g thin-layer plate respectively, 60-90 ℃-Ethyl of with 10-20:4-6:the upper solution of formate-formic acid of 1-2 petroleum ether is developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show five identical orange-yellow fluorescence speckles; With the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle;
B. get 10 in present composition tablet, remove sugar-coat; Porphyrize, the 10ml that adds diethyl ether, the ultrasonic 15-30 of place minute, filter, filtrate is waved to 1ml, as need testing solution; Other gets Rhizoma Atractylodis control medicinal material 0.5g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw above-mentioned need testing solution 20 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with 55-65: 60-90 ℃-ethyl acetate of 1-2 petroleum ether is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C. get Rhizoma Et Radix Notopterygii control medicinal material 0.5g, make control medicinal material solution according to the preparation method of differentiating the control medicinal material solution under the b item; Other gets the isoimperatorin reference substance, adds diethyl ether to make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw according to need testing solution 10 μ l and above-mentioned control medicinal material and each 1 μ l of reference substance solution of differentiating under the b item, put respectively on same silica gel g thin-layer plate, with 6-12: 1-3 benzene-ethyl acetate is developing solvent, launches, and exhibition is apart from 5cm, take out, dry, again with 6-12: 30-60 ℃-butanone of 1-3 petroleum ether is developing solvent, launches, exhibition is apart from 10cm, take out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and contrast chromatograph corresponding position on, show the fluorescence speckle of same color.
10. the method for quality control of Chinese medicinal composition preparation as claimed in claim 9; The discrimination method that it is characterized in that tablet comprises one or more in the following discriminating: the preparation of a. need testing solution; Get 20 of this product; Remove sugar-coat; Accurately weighed; Porphyrize is crossed sieve No. three, and precision takes by weighing and is equivalent in right amount 1 weight, puts in the conical flask; The accurate ethanol 25ml that adds; Close plug, weighed weight added hot reflux 1 hour; Let cool; Weighed weight is supplied the weight that subtracts mistake with ethanol, filters; Precision is measured subsequent filtrate 10ml; Put in the conical flask, evaporate to dryness, residue add 30% ethanol-hydrochloric acid with the mixed solution 15ml of 10: 1 ratios; Added hot reflux 1 hour; Rapidly cooling in the dislocation separatory funnel, is extracted 4 times with the chloroform jolting; Each 15ml; The mixed solution that combined chloroform liquid, evaporate to dryness, residue add 2: 1 absolute ethyl alcohol-ethyl acetates makes dissolving in right amount; In the dislocation 25ml measuring bottle; The mixed solution that adds 2: 1 absolute ethyl alcohol-ethyl acetates is diluted to scale, shakes up, and filters with 0.45 μ m miillpore filter; Get 20ml; Evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system; Get emodin, chrysophanol reference substance again, add ethyl acetate and make the mixed solution that every 1ml contains emodin 0.5mg, chrysophanol 1mg, product solution in contrast; According to thin layer chromatography test, draw each 10 μ l of above-mentioned three kinds of solution, put on same silica gel g thin-layer plate respectively, 60-90 ℃-Ethyl of be developing solvent with the upper solution of 15:5:1 petroleum ether formate-formic acid, 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 five identical orange-yellow fluorescence speckles; With the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle;
B. get 10 of this product, remove sugar-coat; Porphyrize, the 10ml that adds diethyl ether, ultrasonic place 20 minutes filters, and filtrate is waved to 1ml, as need testing solution; Other gets Rhizoma Atractylodis control medicinal material 0.5g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw above-mentioned need testing solution 20 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with 50: 1 petroleum ether 60-90 ℃-ethyl acetates was developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C. get Rhizoma Et Radix Notopterygii control medicinal material 0.5g, make control medicinal material solution according to the preparation method of differentiating the control medicinal material solution under the b item; Other gets the isoimperatorin reference substance, adds diethyl ether to make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw according to need testing solution 10 μ l and above-mentioned control medicinal material and each 1 μ l of reference substance solution of differentiating under the b item, put respectively on same silica gel g thin-layer plate, with 8: 2 benzene-ethyl acetates was developing solvent, launched, and exhibition is apart from 5cm, take out, drying, is developing solvent with 8: 2 petroleum ether 30-60 ℃-butanone again, launches, exhibition is apart from 10cm, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and contrast chromatograph corresponding position on, show the fluorescence speckle of same color.
11. the method for quality control of Chinese medicinal composition preparation as claimed in claim 4 is characterized in that the inspection method in this method is: aconitine limit, get 8 in present composition tablet, remove sugar-coat, porphyrize is after 10% sodium carbonate liquor moistening, the 50ml that adds diethyl ether supersound process 10-25 minute, filters, filtrate is extracted 2 times with 20% hydrochloric acid solution jolting, and each 30ml merges acid solution, regulate pH value to 11.5-12.5 with strong ammonia solution, extract 2 times with the ether jolting, each 30ml merges ether solution, extract 2 times with 2% hydrochloric acid solution jolting, each 30ml merges acid liquid, regulates pH value to 11.5-12.5 with strong ammonia solution, extract 2 times with the ether jolting, each 30ml merges ether solution, evaporate to dryness, residue add methanol make in right amount the dissolving and move in the 2ml measuring bottle, add methanol and be diluted to scale, shake up, as need testing solution; Other gets the aconitine reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to the thin layer chromatography test, accurate above-mentioned offerings solution 10 μ l, the reference substance solution 5 μ l of drawing put respectively on same silica gel g thin-layer plate, with 6-10: 5-8: 1-2 cyclohexane-ethyl acetate-diethylamine is developing solvent, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of appearance should or speckle not occur less than the speckle of reference substance.
12. the method for quality control of Chinese medicinal composition preparation as claimed in claim 11 is characterized in that the inspection method of the tablet in this method is: aconitine limit, get 8 of this product, remove sugar-coat, porphyrize is after 10% sodium carbonate liquor moistening, the 50ml that adds diethyl ether, supersound process 15 minutes filters, filtrate is extracted 2 times with 2% hydrochloric acid solution jolting, and each 30ml merges acid solution, regulate pH value to 12 with strong ammonia solution, extract 2 times with the ether jolting, each 30ml merges ether solution, extract 2 times with 2% hydrochloric acid solution jolting, each 30ml merges acid liquid, regulates pH value to 12 with strong ammonia solution, extract 2 times with the ether jolting, each 30ml merges ether solution, evaporate to dryness, residue add methanol make in right amount the dissolving and move in the 2ml measuring bottle, add methanol and be diluted to scale, shake up, as need testing solution; Other gets the aconitine reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to the thin layer chromatography test, accurate above-mentioned offerings solution 10 μ l, the reference substance solution 5 μ l of drawing put respectively on same silica gel g thin-layer plate, with 8: 6: 1 cyclohexane-ethyl acetate-diethylamine was developing solvent, launched, and took out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of appearance should or speckle not occur less than the speckle of reference substance.
13. the method for quality control of Chinese medicinal composition preparation as claimed in claim 4 is characterized in that this method may further comprise the steps:
Assay: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test, be filler: 80-90 with octadecylsilane chemically bonded silica: 10-20 methanol-0.1% phosphoric acid solution is a mobile phase; The detection wavelength is 254nm; Number of theoretical plate calculates by the emodin peak should be not less than 2000; The preparation of reference substance solution, precision take by weighing emodin and the chrysophanol reference substance is an amount of, adds 1-3 respectively: the mixed solution of 1-2 dehydrated alcohol-ethyl acetate is made the solution that contains emodin 1 μ g, chrysophanol 2 μ g among every 1ml, promptly; 20 in present composition tablet is got in the preparation of need testing solution, removes sugar-coat, the accurate title, decide, and porphyrize is crossed sieve No. three, and precision takes by weighing and is equivalent to 1 weight in right amount, put in the conical flask accurate ethanol 25ml, the close plug of adding, claim to decide weight, reflux 1-2 hour, put cold, claim to decide weight, supply the weight that subtracts mistake with ethanol, filter, precision is measured subsequent filtrate 10ml, put in the conical flask, evaporate to dryness, residue add 30% ethanol-hydrochloric acid with 8-12: the mixed solution 15ml of 1-2 ratio, reflux 1-2 hour, cooling rapidly, in the dislocation separatory funnel, extract 4 times each 15ml with the chloroform jolting, combined chloroform liquid, evaporate to dryness, residue adds 1-3: the mixed solution of 1-2 dehydrated alcohol-ethyl acetate makes dissolving in right amount, in the dislocation 25ml measuring bottle, add 1-3: the mixed solution of 1-2 dehydrated alcohol-ethyl acetate is diluted to scale, shake up, filter with microporous filter membrane, promptly; Algoscopy, accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Present composition preparation per unit amount contains the total amount of Radix Et Rhizoma Rhei in emodin and chrysophanol, must not be less than 0.10-0.20mg;
Differentiate: a. gets the need testing solution 20ml under the assay item, and evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system; Get emodin, chrysophanol reference substance again, add ethyl acetate and make the mixed solution that every 1ml contains emodin 0.5mg, chrysophanol 1mg, product solution in contrast; According to thin layer chromatography test, draw each 10 μ l of above-mentioned three kinds of solution, put on same silica gel g thin-layer plate respectively, with 10-20: 4-6: the upper solution of 60-90 ℃-Ethyl formate-formic acid of 1-2 petroleum ether is developing solvent, launch, take out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show five identical orange-yellow fluorescence speckles; With the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle;
B. get 10 in present composition tablet, remove sugar-coat; Porphyrize, the 10ml that adds diethyl ether, the ultrasonic 15-30 of place minute, filter, filtrate is waved to 1ml, as need testing solution; Other gets Rhizoma Atractylodis control medicinal material 0.5g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw above-mentioned need testing solution 20 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with 55-65: 60-90 ℃-ethyl acetate of 1-2 petroleum ether is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C. get Rhizoma Et Radix Notopterygii control medicinal material 0.5g, make control medicinal material solution according to the preparation method of differentiating the control medicinal material solution under the b item; Other gets the isoimperatorin reference substance, adds diethyl ether to make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw according to need testing solution 10 μ l and above-mentioned control medicinal material and each 1 μ l of reference substance solution of differentiating under the b item, put respectively on same silica gel g thin-layer plate, with 6-12: 1-3 benzene-ethyl acetate is developing solvent, launches, and exhibition is apart from 5cm, take out, dry, again with 6-12: 30-60 ℃-butanone of 1-3 petroleum ether is developing solvent, launches, exhibition is apart from 10cm, take out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and contrast chromatograph corresponding position on, show the fluorescence speckle of same color;
Check: aconitine limit, get 8 in present composition tablet, remove sugar-coat, porphyrize, after 10% sodium carbonate liquor moistening, 50ml adds diethyl ether, supersound process 10-25 minute, filter, filtrate is extracted 2 times with 2% hydrochloric acid solution jolting, each 30ml, merge acid solution, regulate pH value to 11.5-12.5, extract 2 times with the ether jolting with strong ammonia solution, each 30ml, merge ether solution, extract 2 times, each 30ml with 2% hydrochloric acid solution jolting, merge acid liquid, regulate pH value to 11.5-12.5 with strong ammonia solution, extract 2 times, each 30ml with the ether jolting, merge ether solution, evaporate to dryness, residue add methanol make in right amount the dissolving and move in the 2ml measuring bottle, add methanol and be diluted to scale, shake up, as need testing solution; Other gets the aconitine reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to the thin layer chromatography test, accurate above-mentioned offerings solution 10 μ l, the reference substance solution 5 μ l of drawing put respectively on same silica gel g thin-layer plate, with 6-10: 5-8: 1-2 cyclohexane-ethyl acetate-diethylamine is developing solvent, launches, and takes out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of appearance should or speckle not occur less than the speckle of reference substance.
14. the method for quality control of Chinese medicinal composition preparation as claimed in claim 13 is characterized in that this method may further comprise the steps:
Assay: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test, be filler with octadecylsilane chemically bonded silica: methanol-0.1% phosphoric acid solution was a mobile phase in 85: 15; The detection wavelength is 254nm; Number of theoretical plate calculates by the emodin peak should be not less than 2000; The preparation of reference substance solution, precision take by weighing emodin and the chrysophanol reference substance is an amount of, and the mixed solution that adds 2: 1 dehydrated alcohol-ethyl acetates is respectively made the solution that contains emodin 1 μ g, chrysophanol 2 μ g among every 1ml, promptly; 20 of this product are got in the preparation of need testing solution, remove sugar-coat, the accurate title, decide, and porphyrize is crossed sieve No. three, and precision takes by weighing and is equivalent to 1 weight in right amount, put in the conical flask accurate ethanol 25ml, the close plug of adding, claim to decide weight, reflux 1 hour is put cold, claim to decide weight, supply the weight that subtracts mistake, filter with ethanol, precision is measured subsequent filtrate 10ml, puts in the conical flask evaporate to dryness, residue adds the mixed solution 15ml of 30% ethanol-hydrochloric acid with 10: 1 ratios, reflux 1 hour, cooling rapidly, in the dislocation separatory funnel, extract 4 times each 15ml with the chloroform jolting, combined chloroform liquid, the mixed solution that evaporate to dryness, residue add 2: 1 dehydrated alcohol-ethyl acetates makes dissolving in right amount, in the dislocation 25ml measuring bottle, the mixed solution that adds 2: 1 dehydrated alcohol-ethyl acetates is diluted to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly; Algoscopy, accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Every of this product contains the total amount of Radix Et Rhizoma Rhei in emodin and chrysophanol, must not be less than 0.15mg;
Differentiate: a. gets the need testing solution 20ml under the assay item, and evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Et Rhizoma Rhei control medicinal material 0.1g, shines medical material solution in pairs with legal system; Get emodin, chrysophanol reference substance again, add ethyl acetate and make the mixed solution that every 1ml contains emodin 0.5mg, chrysophanol 1mg, product solution in contrast; According to thin layer chromatography test, draw each 10 μ l of above-mentioned three kinds of solution, put on same silica gel g thin-layer plate respectively, be developing solvent with the upper solution of 15: 5: 1 petroleum ether 60-90 ℃-Ethyl formate-formic acid, 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 five identical orange-yellow fluorescence speckles; With the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle;
B. get 10 of this product, remove sugar-coat; Porphyrize, the 10ml that adds diethyl ether, ultrasonic place 20 minutes filters, and filtrate is waved to 1ml, as need testing solution; Other gets Rhizoma Atractylodis control medicinal material 0.5g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw above-mentioned need testing solution 20 μ l, control medicinal material solution 4 μ l, put respectively on same silica gel g thin-layer plate, with 50: 1 petroleum ether 60-90 ℃-ethyl acetates was developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C. get Rhizoma Et Radix Notopterygii control medicinal material 0.5g, make control medicinal material solution according to the preparation method of differentiating the control medicinal material solution under the b item; Other gets the isoimperatorin reference substance, adds diethyl ether to make the solution that every 1ml contains 0.5mg, in contrast product solution; According to the thin layer chromatography test, draw according to need testing solution 10 μ l and above-mentioned control medicinal material and each 1 μ l of reference substance solution of differentiating under the b item, put respectively on same silica gel g thin-layer plate, with 8: 2 benzene-ethyl acetates was developing solvent, launched, and exhibition is apart from 5cm, take out, drying, is developing solvent with 8: 2 petroleum ether 30-60 ℃-butanone again, launches, exhibition is apart from 10cm, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and contrast chromatograph corresponding position on, show the fluorescence speckle of same color;
Check: aconitine limit, get 8 of this product, remove sugar-coat, porphyrize, after 10% sodium carbonate liquor moistening, 50ml adds diethyl ether, supersound process 15 minutes filters, and filtrate is extracted 2 times with 2% hydrochloric acid solution jolting, each 30ml merges acid solution, regulates pH value to 12 with strong ammonia solution, extract 2 times with the ether jolting, each 30ml merges ether solution, extract 2 times with 2% hydrochloric acid solution jolting, each 30ml merges acid liquid, regulate pH value to 12 with strong ammonia solution, extract 2 times, each 30ml with the ether jolting, merge ether solution, evaporate to dryness, residue add methanol make in right amount the dissolving and move in the 2ml measuring bottle, add methanol and be diluted to scale, shake up, as need testing solution; Other gets the aconitine reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to the thin layer chromatography test, accurate above-mentioned offerings solution 10 μ l, the reference substance solution 5 μ l of drawing put respectively on same silica gel g thin-layer plate, with 8: 6: 1 cyclohexane-ethyl acetate-diethylamine was developing solvent, launched, and took out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of appearance should or speckle not occur less than the speckle of reference substance.
15. the application of Chinese medicine composition as claimed in claim 4 in the big damp-heat syndrome medicine of preparation treatment.
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| CN101199776B (en) * | 2007-12-13 | 2011-03-23 | 骆金根 | Soaking medicament for treating muggy type diarrhea |
| US8489539B2 (en) * | 2009-10-05 | 2013-07-16 | Elc Management, Llc | Computer-aided diagnostic systems and methods for determining skin compositions based on traditional chinese medicinal (TCM) principles |
| CN102590434B (en) * | 2012-03-01 | 2014-08-13 | 西藏奇正藏药股份有限公司 | Detection method of preparation comprising eight Chinese herbal medicines for calming |
| CN103801107B (en) * | 2012-11-15 | 2017-03-01 | 上海家化联合股份有限公司 | A kind of traditional medicine volatile oil with anti-candida albicanses effect |
| CN106198833A (en) * | 2016-06-24 | 2016-12-07 | 广西灵峰药业有限公司 | A kind of quality of production control method of bright pool capsule |
| CN106491937A (en) * | 2016-12-25 | 2017-03-15 | 闫大伟 | A kind of Chinese medicine for treating syndrome of dampness-heat in large intestine |
| CN108956844B (en) * | 2018-07-27 | 2020-09-11 | 河北中医学院 | Multi-information rapid thin-layer identification method for multiple medicinal materials of stomach-nourishing soup freeze-dried powder |
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