CN1891285A - Chinese medicine composition, and its preparing method and quality control method - Google Patents
Chinese medicine composition, and its preparing method and quality control method Download PDFInfo
- Publication number
- CN1891285A CN1891285A CN 200510200382 CN200510200382A CN1891285A CN 1891285 A CN1891285 A CN 1891285A CN 200510200382 CN200510200382 CN 200510200382 CN 200510200382 A CN200510200382 A CN 200510200382A CN 1891285 A CN1891285 A CN 1891285A
- Authority
- CN
- China
- Prior art keywords
- solution
- methanol
- reference substance
- chinese medicine
- medicine composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Medicinal Preparation (AREA)
Abstract
The present invention discloses a Chinese medicine composition for effectively curing women's pelvic inflammation with good therapeutic effect. Said Chinese medicine composition is made up by using 12 Chinese medicinal materials of lonicera flower, scutellaria root, dandelion, Yedo violet, red peony root, ligusticum root and others through a certain preparation process. Said invention also provides its preparation process and its quality control method.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition for the treatment of women's chronic pelvic inflammatory disease and preparation method thereof and method of quality control, belong to the field of Chinese medicines.
Background technology
Women's chronic pelvic inflammatory disease disease is commonly encountered diseases and the frequently-occurring disease in the gynaecopathia, causes very big misery to the patient, the object of the present invention is to provide a kind of evident in efficacy, the Chinese medicine composition of the treatment women's chronic pelvic inflammatory disease that has no side effect of taking convenience.
Summary of the invention
The present invention seeks to be achieved through the following technical solutions
Medicine of the present invention is made by following component:
Flos Lonicerae 15-25 part Radix Scutellariae 15-25 part Herba Taraxaci 10-20 part
5 parts-15 parts Spina Gleditsiae 10-20 part Radix Paeoniae Rubra of Herba Violae 10-20 part
5 parts-15 parts of 5 parts of-15 parts of Rhizoma Chuanxiongs of Caulis Spatholobi 15-25 part rhizoma sparganic
5 parts-15 parts of 5 parts of-15 parts of Semen Vaccariae of 5 parts of-15 parts of Rhizoma Corydalis of Rhizoma Cyperi
Medicine optimum weight part proportioning of the present invention is:
15 parts of 20 parts of Herba Taraxacis of 20 parts of Radix Scutellariaes of Flos Lonicerae
15 parts of 15 parts of Radix Paeoniae Rubra of 10 parts of Spina Gleditsiaes of Herba Violae
10 parts of 10 parts of Rhizoma Chuanxiongs of 20 parts of rhizoma sparganic of Caulis Spatholobi
10 parts of 10 parts of Semen Vaccariae of 10 parts of Rhizoma Corydalis of Rhizoma Cyperi
In the above crude drug, Rhizoma Cyperi and Rhizoma Corydalis are good with the vinegar goods, and Semen Vaccariae is good with parched medicinal material then.
Use above crude drug, can make acceptable various regular dosage forms on clinical or the pharmaceutics, comprise tablet, capsule, granule, soft capsule and pill etc.
Accomplish above dosage form, can pass through following processing step:
Two of purpose of the present invention can realize by following technical measures:
Get crude drug, pulverize, decoct with water secondary, collecting decoction filters, and filtrate is concentrated into clear paste, and stirring slowly adds ethanol down, fully stirs, and leaves standstill, and the leaching supernatant reclaims ethanol to clear paste, gets Chinese medicine composition; This Chinese medicine composition is added suitable adjuvant, make required dosage form.Such as:
Add disintegrating agent, binding agent, granulate, add volatile oil, add lubricant, be pressed into tablet.
Add disintegrating agent, binding agent, granulate, add volatile oil, add lubricant, incapsulate, make capsule.
Add substrate, suspending agent, wetting agent, be prepared into soft capsule.
Add distilled water, static, supernatant is got in cold preservation 24 hours, filters, and adds sedan-chair flavor agent and/or cosolvent and/or antiseptic, is prepared into oral solution.
Add sedan-chair flavor agent and excipient, be prepared into granule.
In detail, its preparation process is:
Get crude drug, decoct with water secondary, add 10 times of water gagings for the first time, decocted 2 hours, and added 6 times of water gagings for the second time, decocted 1 hour, collecting decoction, filter, relative density was 1.20～1.25 clear paste when filtrate was concentrated into 80 ℃, added ethanol and made and contain the alcohol amount and reach 50%, left standstill 24 hours, the leaching supernatant reclaims ethanol and is condensed into clear paste, gets Chinese medicine composition; Add in the drug composition hereinto distilled water and correctives and/antiseptic, make oral liquid.
In the process of this Chinese medicine composition of research, the inventor also formulates and has used some method of quality control, and these methods can be estimated the quality of control product.This method of quality control comprises assay and qualitative identification two parts, below narration respectively.
Content assaying method can adopt following method according to the needs of different dosage form:
A, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 10: 90～15: 85 acetonitrile-0.4% phosphoric acid solution is a mobile phase; The detection wavelength is 327 ± 2nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 1000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the chlorogenic acid reference substance, puts in the brown measuring bottle, adds 50% methanol and make the solution that every 1ml contains 40-60 μ g, that is, preserve below 10 ℃;
It is an amount of that this product is got in the preparation of need testing solution, puts in the tool plug conical flask, adds 50% methanol 25-100ml, weigh, and supersound extraction 20-40 minute, add 50% methanol and supply the weight that subtracts mistake, filter, promptly;
Accurate reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid respectively, measures, promptly;
B, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, 45: 55: 0.1～50: 50: 0.2 methanol-water-phosphoric acid is a mobile phase, the detection wavelength is 280 ± 2nm, and theoretical cam curve is pressed the baicalin peak and calculated, and should be not less than 2500;
It is an amount of that the preparation precision of reference substance solution takes by weighing 4 hours baicalin reference substance of 60 ℃ of drying under reduced pressure, adds methanol and make the solution that every 1ml contains 40-60 μ g;
It is an amount of that this product is got in the preparation of need testing solution, and accurate the title decides, and the accurate methanol 25-100ml that adds claims to decide weight, and supersound process 20-40 minute, claim to decide weight, add methanol and supply the weight that subtracts mistake, filtration, promptly;
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;
C, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 10: 90～20: 80 acetonitrile-0.1 phosphoric acid is mobile phase, detects wavelength 230 ± 2nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;
It is an amount of that the preparation precision of the preparation reference substance solution of reference substance solution takes by weighing in phosphorus pentoxide desiccator 36 hours peoniflorin reference substance of drying under reduced pressure, adds mobile phase and make the solution that contains 40-60 μ g among every 1ml, shakes up, promptly;
It is an amount of that this product is got in the preparation of need testing solution, and accurate the title decides, and the accurate methanol 25-100ml that adds claims to decide weight, and supersound process 20-40 minute, claim again to decide weight, add methanol and supply the weight that subtracts mistake, filtration, promptly;
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
Discrimination method then comprises following one or more:
A, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add water 20-50ml, and put hot bath and make dissolving, with n-butanol extraction 2-3 time, each 10-25ml, merging n-butyl alcohol liquid, water bath method, residue add an amount of methanol makes dissolving, as need testing solution; Other gets baicalin, chlorogenic acid reference substance, adds methanol respectively and makes the solution that every 1ml contains 0.1mg, in contrast product solution; According to the thin layer chromatography test, draw each 2-5 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, be developing solvent with acetic acid, launch, take out, dry, put under the ultra-violet lamp 365nm and inspect; For looking in the product chromatograph, with baicalin, the corresponding position of chlorogenic acid reference substance chromatograph on, the fluorescence speckle of apparent same color respectively;
B, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add water 20-50ml, and put hot bath and make dissolving, with n-butanol extraction 2-3 time, each 10-25ml, merging n-butyl alcohol liquid, water bath method, residue add an amount of methanol makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 50-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 40: 15: 10: chloroform-ethyl acetate of 0.2-methanol-formic acid 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 reference substance chromatograph on, be identical bluish violet speckle;
C, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add methanol 20-50ml supersound process 20-40 minute, filter, filtrate evaporate to dryness, residue add water makes dissolving, adds ammonia solution and transfers to alkalescence, ether extraction 2-3 time, each 10-25ml, merge extractive liquid,, evaporate to dryness, residue adds an amount of methanol makes dissolving, as need testing solution; Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 5-10 μ l, reference substance solution 1 μ l respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with cyclohexane extraction-chloroform-methanols of 10: 6: 1 was developing solvent, launch, take out, dry, after putting in the iodine vapor smoked several seconds kind, put under the ultra-violet lamp 365nm and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
D, to get this product an amount of, solution elder generation evaporate to dryness, other dosage forms directly add water 20-50ml, with the dilute hydrochloric acid adjust pH to 2-3, hot bath makes dissolving, put cold, with ether extraction 2-3 time, each 10-25ml merges ether solution, extracts 2-3 time with 2% sodium carbonate liquor, each 10-25ml divides and gets alkali liquor, adds hydrochloric acid and regulates pH value to 2-3, add diethyl ether and extract 2-3 time, each 10-25ml merges ether solution, volatilize, residue adds an amount of methanol makes dissolving, as need testing solution; Other gets the ferulic acid reference substance and adds methanol and make the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer chromatography test, draw each 5-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-glacial acetic acid of 30: 1: 3-methanol is developing solvent, launches, and takes out, dry, under ultra-violet lamp 365nm, inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
This product can be used for women's chronic pelvic inflammatory disease card and belongs to damp-heat accumulation, and the auxiliary treatment of people who gets stagnation of vital energy and blood stasis for determining drug effect, has been carried out pharmacodynamics test research to this product, and used medicine is best proportioning and optimum process preparation and get according to the present invention in the test.
Concrete test is as follows:
Test an external bacteriostasis
Adopting golden yellow glucose coccus, staphylococcus epidermidis is test strain.
Test method: adopt agar dilution.With making doubling dilution in the agar culture medium that be added in by the reagent thing to have melted, pour into the plating medium that becomes to contain different liquor strengths.With the method for reduced turbidity, each bacterial strain is diluted to 1/2 of No. 1 standard pipe in Maxwell, dibbling is on the plating medium of variable concentrations respectively for the bacterium liquid that dilution is good, and every 10 μ l cultivated 18～24 hours for 37 ℃.Be provided with the contrast of blank and penicillin positive drug simultaneously.Write down the growing state of each bacterial strain on different pharmaceutical concentration culture medium, the least concentration that this medicine suppresses bacteria growing is minimal inhibitory concentration, and minimal inhibitory concentration (MIC) expression bacteriostatic level is adopted in this test.
Result of the test shows that this product oral solutions has the vitro inhibition effect to golden Portugal bacterium and form staph.Result of the test sees Table 1.
The external bacteriostasis of table 1 is table as a result
| Test strain | Bacterial strain number (strain) | The antibacterial contrast | Penicillin contrast (100U/ml) | MIC scope (mg/ml) |
| Gold Portugal bacterium | 20 | + | - | 20.6～100 |
| Form staph | 20 | + | - | 15.5～100 |
Test the influence of two xylol induced mice auricle edemas
Experimental technique faces with preceding that this product granule is mixed with the 0.10gPml suspension with 0.5% Carboxymethyl cellulose sodium (CMC-Na) is standby, and animal is used healthy Kunming mouse, body weight 20 ± 2 grams.Mice is divided into five groups (matched group normal saline) at random, irritate the long-pending 20mlPkg of being of body of stomach, two weeks of continuous irrigation stomach, once a day, the last administration was applied to mouse right ear with microsyringe with 0.05mlP dimethylbenzene after 30 minutes, put to death mice after 15 minutes, cut two ears along the auricle baseline, dash with the 8mm diameter steel and to lay round auricle in left and right sides auricle same area respectively, torsion balance claims two auricle weight in wet bases,, calculate and respectively organize swelling degree average and standard deviation as the swelling level index with two auricle weight differences, carry out the t check.Inhibitory rate of intumesce equals the difference of average swelling degree of matched group and the average swelling degree of administration group and takes advantage of 100% again divided by the average swelling degree of matched group.
The results are shown in Table 2, the result shows that two dosage groups of this product granule and matched group compare, and auricle swelling degree obviously alleviates, and significant differences is arranged, and illustrates that this product has good antiinflammatory action.
The influence of table 2 xylol induced mice auricle edema
| Group | Dosage (gPkg) | Animal (only) | Average swelling degree (mg) | Suppression ratio (%) |
| Matched group | 8 | 25.07±5.67 | ||
| Gynecological's a thousand pieces of gold group | 210 | 8 | 17.04±3.59* | 34.58 |
| This product granule | 440 | 8 | 13.85±5.04** | 28.35 |
| 220 | 8 | 17.49±3.63* | 37.95 |
Annotate: matched group is * P＜0.05 relatively, * * P＜0.01
Further specify technical scheme of the present invention by the following examples, but the present invention to protect preparation be not limited in the described dosage form of embodiment.
The specific embodiment:
Embodiment 1
[prescription] Flos Lonicerae 200g Radix Scutellariae 200g Herba Taraxaci 150g
Herba Violae 100g Spina Gleditsiae 150g Radix Paeoniae Rubra 150g
Caulis Spatholobi 200g rhizoma sparganic 100g Rhizoma Chuanxiong 100g
Rhizoma Cyperi (vinegar system) 100g Rhizoma Corydalis (vinegar system) 100g Semen Vaccariae (stir-fry) 100g
[method for making] above 12 flavors are given as one thinks fit cataclasmly, decoct with water secondary, for the first time add 10 times of water gagings, decocted 2 hours, add 6 times of water gagings for the second time, decocted 1 hour, collecting decoction filters, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (80 ℃), stir and slowly to add ethanol down and make and contain the alcohol amount and reach 50%, fully stir, left standstill 24 hours, the leaching supernatant reclaims the clear paste of ethanol to relative density 1.30～1.35 (80 ℃).Get 1 part of clear paste, 3 parts of sucrose, 1 part in dextrin and ethanol are an amount of, granulate, and drying is made 1000g, promptly.
Embodiment 2
[prescription] Flos Lonicerae 250g Radix Scutellariae 250g Herba Taraxaci 200g
Herba Violae 150g Spina Gleditsiae 200g Radix Paeoniae Rubra 200g
Caulis Spatholobi 250g rhizoma sparganic 150g Rhizoma Chuanxiong 150g
Rhizoma Cyperi 150g Rhizoma Corydalis 150g Semen Vaccariae 150g
[method for making] gets crude drug, decocts with water secondary, adds 10 times of water gagings for the first time, decocted 2 hours, and added 6 times of water gagings for the second time, decocted 1 hour, collecting decoction filters, and relative density was 1.20～1.25 clear paste when filtrate was concentrated into 80 ℃, add ethanol and make and contain the alcohol amount and reach 50%, left standstill the leaching supernatant 24 hours, reclaim ethanol and be condensed into clear paste, add a small amount of ethyl hydroxybenzoate, and adding distil water gets oral liquid to 1000ml.
Granule carries out quality examination among embodiment 3 embodiment
This product 5g is got in [discriminating] (1), adds water 50ml, puts hot bath and makes dissolving, uses n-butanol extraction 2 times, and each 20ml merges n-butyl alcohol liquid, and water bath method, residue add 2ml methanol makes dissolving, as need testing solution.Other gets baicalin, chlorogenic acid reference substance, adds methanol respectively and makes the solution that every 1ml contains 0.1mg, in contrast product solution.According to the thin layer chromatography test, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, be developing solvent with acetic acid, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.For looking in the product chromatograph, with baicalin, the corresponding position of chlorogenic acid reference substance chromatograph on, the fluorescence speckle of apparent same color respectively.
(2) get the peoniflorin reference substance, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw reference substance solution and discriminating (1) item each 10 μ l of need testing solution down, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform-ethyl acetate-methanol-formic acid (40: 15: 10: 0.2) be 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 reference substance chromatograph on, be identical bluish violet speckle.
(3) get this product 5g, porphyrize adds methanol 50ml supersound process 30 minutes, filters the filtrate evaporate to dryness, residue adds water makes dissolving, adds ammonia solution and transfers to alkalescence, ether extraction 3 times, each 15ml, merge extractive liquid,, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 1 μ l respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with cyclohexane extraction-chloroform-methanol (10: 6: 1) is developing solvent, launch, take out, dry, after putting in the iodine vapor smoked several seconds kind, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(4) get this product 10g, add water 50ml, with dilute hydrochloric acid adjust pH to 2～3, hot bath makes dissolving, put cold, with ether extraction 3 times, each 20ml merges ether solution, extracts 3 times with 2% sodium carbonate liquor, each 15ml divides and gets alkali liquor, adds hydrochloric acid and regulates pH value to 2～3, add diethyl ether and extract 3 times, each 15ml merges ether solution, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the ferulic acid reference substance and adds methanol and make the solution that every 1ml contains 1mg, in contrast product solution.According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-glacial acetic acid-methanol (30: 1: 3) is developing solvent, launches, and takes out, dry, under ultra-violet lamp (365nm), inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
[assay] is according to high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-0.4% phosphoric acid solution (13: 87) is a mobile phase; The detection wavelength is 327nm.Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 1000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the chlorogenic acid reference substance, puts in the brown measuring bottle, adds 50% methanol and make the solution that every 1ml contains 40 μ g, promptly gets (preserving below 10 ℃).
This product is got in the preparation of need testing solution, porphyrize, and precision takes by weighing 5g, put in the tool plug conical flask, add 50% methanol 30ml, supersound extraction 25 minutes, filter, residue is with 50% washed with methanol 3 times, 5ml at every turn, filter, merging filtrate quantitatively shifts in the 100ml measuring bottle, adds 50% methanol and is diluted to scale, shake up, promptly.
Accurate reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid respectively, measure, promptly.
The every 10g of this product contains chlorogenic acid (C16H18O9) must not be less than 7.0mg.
Claims (10)
1. Chinese medicine composition for the treatment of women's chronic pelvic inflammatory disease is characterized in that this Chinese medicine composition made by following raw medicaments in portion by weight:
Flos Lonicerae 15-25 part Radix Scutellariae 15-25 part Herba Taraxaci 10-20 part
Herba Violae 5-15 part Spina Gleditsiae 10-20 part Radix Paeoniae Rubra 10-20 part
Caulis Spatholobi 15-25 part rhizoma sparganic 5-15 part Rhizoma Chuanxiong 5-15 part
Rhizoma Cyperi 5-15 part Rhizoma Corydalis 5-15 part Semen Vaccariae 5-15 part.
2. Chinese medicine composition as claimed in claim 1 is characterized in that the optimum weight ratio of each crude drug is:
15 parts of 20 parts of Herba Taraxacis of 20 parts of Radix Scutellariaes of Flos Lonicerae
15 parts of 15 parts of Radix Paeoniae Rubra of 10 parts of Spina Gleditsiaes of Herba Violae
10 parts of 10 parts of Rhizoma Chuanxiongs of 20 parts of rhizoma sparganic of Caulis Spatholobi
10 parts of 10 parts of Semen Vaccariae of 10 parts of Rhizoma Corydalis of Rhizoma Cyperi.
3. Chinese medicine composition as claimed in claim 1 or 2 is characterized in that Rhizoma Cyperi and the Rhizoma Corydalis in the crude drug is good with the vinegar goods, and Semen Vaccariae is good with parched medicinal material then.
4. as Chinese medicine composition as described in the claim 1,2 or 3, it is characterized in that to make acceptable various regular dosage forms on clinical or the pharmaceutics, comprise tablet, capsule, granule, soft capsule and pill etc.
5. as the preparation method of Chinese medicine composition as described in each in the claim 1 to 4, it is characterized in that this method is: get crude drug, pulverize, decoct with water secondary, collecting decoction filters, and filtrate is concentrated into clear paste, stir and slowly add ethanol down, fully stir, leave standstill the leaching supernatant, reclaim ethanol to clear paste, get Chinese medicine composition; This Chinese medicine composition is added suitable adjuvant, make required dosage form.
6. as the preparation method of Chinese medicine composition as described in the claim 5, it is characterized in that this method is: get crude drug, decoct with water secondary, for the first time add 10 times of water gagings, decocted 2 hours, add 6 times of water gagings for the second time, decocted 1 hour, collecting decoction filters, relative density was 1.20～1.25 clear paste when filtrate was concentrated into 80 ℃, add ethanol and make and contain the alcohol amount and reach 50%, left standstill the leaching supernatant 24 hours, reclaim ethanol and be condensed into clear paste, get Chinese medicine composition; This Chinese medicine composition is added suitable adjuvant, make required dosage form.
7. as the preparation method of Chinese medicine composition as described in the claim 6, the preparation method that it is characterized in that mixture wherein in concentrating the Chinese medicine composition that obtains, add distilled water and correctives and/antiseptic, make oral liquid.
8. as the method for quality control of Chinese medicine composition as described in each in the claim 1 to 4, it is characterized in that this method comprises one or more of following content assaying method:
A, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 10: 90～15: 85 acetonitrile-0.4% phosphoric acid solution is a mobile phase; The detection wavelength is 327 ± 2nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 1000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the chlorogenic acid reference substance, puts in the brown measuring bottle, adds 50% methanol and make the solution that every 1ml contains 40-60 μ g, that is, preserve below 10 ℃;
It is an amount of that this product is got in the preparation of need testing solution, puts in the tool plug conical flask, adds 50% methanol 25-100ml, weigh, and supersound extraction 20-40 minute, add 50% methanol and supply the weight that subtracts mistake, filter, promptly;
Accurate reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid respectively, measures, promptly;
B, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, 45: 55: 0.1～50: 50: 0.2 methanol-water-phosphoric acid is a mobile phase, the detection wavelength is 280 ± 2nm, and theoretical cam curve is pressed the baicalin peak and calculated, and should be not less than 2500;
It is an amount of that the preparation precision of reference substance solution takes by weighing 4 hours baicalin reference substance of 60 ℃ of drying under reduced pressure, adds methanol and make the solution that every 1ml contains 40-60 μ g;
It is an amount of that this product is got in the preparation of need testing solution, and accurate the title decides, and the accurate methanol 25-100ml that adds claims to decide weight, and supersound process 20-40 minute, claim to decide weight, add methanol and supply the weight that subtracts mistake, filtration, promptly;
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly;
C, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 10: 90～20: 80 acetonitrile-0.1 phosphoric acid is mobile phase, detects wavelength 230 ± 2nm; Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;
It is an amount of that the preparation precision of the preparation reference substance solution of reference substance solution takes by weighing in phosphorus pentoxide desiccator 36 hours peoniflorin reference substance of drying under reduced pressure, adds mobile phase and make the solution that contains 40-60 μ g among every 1ml, shakes up, promptly;
It is an amount of that this product is got in the preparation of need testing solution, and accurate the title decides, and the accurate methanol 25-100ml that adds claims to decide weight, and supersound process 20-40 minute, claim again to decide weight, add methanol and supply the weight that subtracts mistake, filtration, promptly;
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
9. as the method for quality control of Chinese medicine composition as described in the claim 8, it is characterized in that this method comprises one or more in the following discrimination method:
A, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add water 20-50ml, and put hot bath and make dissolving, with n-butanol extraction 2-3 time, each 10-25ml, merging n-butyl alcohol liquid, water bath method, residue add an amount of methanol makes dissolving, as need testing solution; Other gets baicalin, chlorogenic acid reference substance, adds methanol respectively and makes the solution that every 1ml contains 0.1mg, in contrast product solution; According to the thin layer chromatography test, draw each 2-5 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, be developing solvent with acetic acid, launch, take out, dry, put under the ultra-violet lamp 365nm and inspect; For looking in the product chromatograph, with baicalin, the corresponding position of chlorogenic acid reference substance chromatograph on, the fluorescence speckle of apparent same color respectively;
B, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add water 20-50ml, and put hot bath and make dissolving, with n-butanol extraction 2-3 time, each 10-25ml, merging n-butyl alcohol liquid, water bath method, residue add an amount of methanol makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 50-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 40: 15: 10: chloroform-ethyl acetate of 0.2-methanol-formic acid 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 reference substance chromatograph on, be identical bluish violet speckle;
C, to get this product an amount of, solution elder generation evaporate to dryness, and other dosage forms directly add methanol 20-50ml supersound process 20-40 minute, filter, filtrate evaporate to dryness, residue add water makes dissolving, adds ammonia solution and transfers to alkalescence, ether extraction 2-3 time, each 10-25ml, merge extractive liquid,, evaporate to dryness, residue adds an amount of methanol makes dissolving, as need testing solution; Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 5-10 μ l, reference substance solution 1 μ l respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 10: 6: 1 cyclohexane extraction, one chloroform-methanol is developing solvent, launch, take out, dry, after putting in the iodine vapor smoked several seconds kind, put under the ultra-violet lamp 365nm and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
D, to get this product an amount of, solution elder generation evaporate to dryness, other dosage forms directly add water 20-50ml, with the dilute hydrochloric acid adjust pH to 2-3, hot bath makes dissolving, put cold, with ether extraction 2-3 time, each 10-25ml merges ether solution, extracts 2-3 time with 2% sodium carbonate liquor, each 10-25ml divides and gets alkali liquor, adds hydrochloric acid and regulates pH value to 2-3, add diethyl ether and extract 2-3 time, each 10-25ml merges ether solution, volatilize, residue adds an amount of methanol makes dissolving, as need testing solution; Other gets the ferulic acid reference substance and adds methanol and make the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer chromatography test, draw each 5-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-glacial acetic acid of 30: 1: 3-methanol is developing solvent, launches, and takes out, dry, under ultra-violet lamp 365nm, inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
10. be used for the treatment of the women's chronic pelvic inflammatory disease card as Chinese medicine composition as described in the claim 1,2 or 3 in preparation and belong to damp-heat accumulation, the application in the medicine of people who gets stagnation of vital energy and blood stasis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510200382A CN100574792C (en) | 2005-07-08 | 2005-07-08 | A kind of effective ingredient detection method of Chinese medicine composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510200382A CN100574792C (en) | 2005-07-08 | 2005-07-08 | A kind of effective ingredient detection method of Chinese medicine composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1891285A true CN1891285A (en) | 2007-01-10 |
| CN100574792C CN100574792C (en) | 2009-12-30 |
Family
ID=37596646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200510200382A Active CN100574792C (en) | 2005-07-08 | 2005-07-08 | A kind of effective ingredient detection method of Chinese medicine composition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100574792C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101940746A (en) * | 2010-09-10 | 2011-01-12 | 哈药集团三精千鹤望奎制药有限公司 | Jinji blood stasis eliminating pills and preparation method thereof |
| CN101940745A (en) * | 2010-09-07 | 2011-01-12 | 哈药集团三精千鹤望奎制药有限公司 | Jinji blood stasis eliminating particles and preparation method thereof |
| CN101019981B (en) * | 2007-03-15 | 2011-08-17 | 北京同御康泰科技有限公司 | Chinese medicine preparation and its preparing process |
| CN101849999B (en) * | 2009-03-31 | 2012-05-23 | 江苏康缘药业股份有限公司 | Chinese medicinal composition for treating pelvic inflammation and preparation method thereof |
| CN102973731A (en) * | 2011-09-05 | 2013-03-20 | 王成光 | Pelvic inflammatory disease and dysmenorrheal treatment liquid agent and preparation method thereof |
-
2005
- 2005-07-08 CN CN200510200382A patent/CN100574792C/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101019981B (en) * | 2007-03-15 | 2011-08-17 | 北京同御康泰科技有限公司 | Chinese medicine preparation and its preparing process |
| CN101849999B (en) * | 2009-03-31 | 2012-05-23 | 江苏康缘药业股份有限公司 | Chinese medicinal composition for treating pelvic inflammation and preparation method thereof |
| CN101940745A (en) * | 2010-09-07 | 2011-01-12 | 哈药集团三精千鹤望奎制药有限公司 | Jinji blood stasis eliminating particles and preparation method thereof |
| CN101940745B (en) * | 2010-09-07 | 2012-01-18 | 哈药集团三精千鹤望奎制药有限公司 | Jinji blood stasis eliminating particles and preparation method thereof |
| CN101940746A (en) * | 2010-09-10 | 2011-01-12 | 哈药集团三精千鹤望奎制药有限公司 | Jinji blood stasis eliminating pills and preparation method thereof |
| CN102973731A (en) * | 2011-09-05 | 2013-03-20 | 王成光 | Pelvic inflammatory disease and dysmenorrheal treatment liquid agent and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100574792C (en) | 2009-12-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1861153A (en) | Medicinal composition used for treating pharyngitis, its prepn. method and its quality control method | |
| CN102488863A (en) | Chinese herbal medicine compound with anticancer effect, preparation method and detection method thereof | |
| CN101045072A (en) | Extractive of turnipia arguta leaves and its pharmaceutical use | |
| CN1872106A (en) | Application of wild basil circle leaves in treating disease of virulence cold | |
| CN1891285A (en) | Chinese medicine composition, and its preparing method and quality control method | |
| CN1686354A (en) | Compound dandelion freeze dried powder injection and its preparation method | |
| CN101040906A (en) | Injection for treating cardiovascular or cerebrovascular disease and the preparing method and the quality control method | |
| CN1817898A (en) | Use of anti-inflammatory medicine for scheelite total saponin and its saponin compound | |
| CN1698757A (en) | Pharmaceutical preparation for treating upper respiratory tract infection and its preparation process and quality control method | |
| CN1883566A (en) | Anti-inflammation medicine and method for preparing same | |
| CN1233378C (en) | Chinese medicine composition for treating oral cavity and throat diseases and its preparing method | |
| CN1803179A (en) | Traditional Chinese medicine composition and its preparation method and quality control method | |
| CN1292778C (en) | Chinese medicine composition for stopping itching and its preparing method | |
| CN102707009A (en) | Method for detecting rhizoma coptidis pills for clearing away heat of upper part of body | |
| CN103055191B (en) | Preparation method and quality detection method of traditional Chinese medicine for treating hematuresis caused by nephritis | |
| CN102697932B (en) | Medicinal composition for treating skin itch and quality detection method | |
| CN103356812B (en) | A kind of Radix Wikstroemae granule | |
| CN1803178A (en) | Traditional Chinese medicine composition and its preparation method and quality control method | |
| CN1973853A (en) | Hemostatic and analgetic medicine composition and its prepn process | |
| CN101084951B (en) | Medicine for treating diseases concerned with respiratory and preparation method and application thereof | |
| CN1843461A (en) | Pharmaceutical composition, its preparation method and quality control method | |
| CN1891283A (en) | Chinese medicine composition, and its preparing method and quality control method | |
| CN102590436A (en) | Method for identifying liquorice in Huoxiang Zhengqi oral liquid | |
| CN1309373C (en) | Granular preparation for treating cancer and its quality control method | |
| CN1806827A (en) | Chinese medicinal composition, its preparation process and quality control method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: JIANGXI YUXIN PHARMACEUTICAL CO., LTD. Free format text: FORMER OWNER: RENHE DEVELOPMENT GROUP CO., LTD. Effective date: 20110314 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 331200 NO. 158, YAODU SOUTH AVENUE, ZHANGSHU CITY, ZHANGSHU CITY, JIANGXI PROVINCE TO: 336200 NO. 1, YUXIN AVENUE, TONGGU COUNTY, JIANGXI PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20110314 Address after: 336200, No. 1, Yu Xin Road, Tonggu County, Jiangxi Province Patentee after: Jiangxi Yu Xin Pharmaceutical Co., Ltd. Address before: 331200 Zhangshu City, Jiangxi Province, South Road, No. 158 Patentee before: Renhe Development Group Co., Ltd. |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20170720 Address after: 336200, No. 1, Yu Xin Road, Tonggu County, Jiangxi Province Patentee after: Jiangxi Tonggu Renhe Pharmaceutical Co., Ltd. Address before: 336200, No. 1, Yu Xin Road, Tonggu County, Jiangxi Province Patentee before: Jiangxi Yu Xin Pharmaceutical Co., Ltd. |
|
| TR01 | Transfer of patent right |