CN1476853A - Medicine for curing hyperasteogeny and its preparation process - Google Patents
Medicine for curing hyperasteogeny and its preparation process Download PDFInfo
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- CN1476853A CN1476853A CNA021289662A CN02128966A CN1476853A CN 1476853 A CN1476853 A CN 1476853A CN A021289662 A CNA021289662 A CN A021289662A CN 02128966 A CN02128966 A CN 02128966A CN 1476853 A CN1476853 A CN 1476853A
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Abstract
The present invention discloses a Chinese medicine for curing hyperosteogeny and its preparation process. Said medicine composition includes 9-Chinese medicinal materials of cooked rhubarb, cistanche stemp, cibotium root, ligustrum fruit, epimedium and others. The capsule has the effects of supplementing kidney, strengthenikng sinew and bone, promoting blood circulation and stopping pain, and can be used for curing the diseases of hyperplastic spondylitis, cervical syndrome and spur formation, etc.
Description
Technical field
The present invention relates to a kind of medicine and preparation technology thereof, particularly relate to a kind of medicine and preparation technology thereof who treats hyperosteogeny.
Background technology
Hyperosteogeny is the aged a kind of performance of skeleton, also is one of common frequently-occurring disease of old people.Present domestic medical circle treatment hyperosteogeny main method has: traction, massage, surgical operation etc., these Therapeutic Method cause very big misery to the patient, the treatment condition has certain limitation, and dangerous big, the course of treatment is long, human body there is damage, weak effect, cure rate is low, easily recurrence, and stay easily and retreat disease even cause other diseases, cause health paralysis or fatal.
Traditional endo-medicine healing potion has bony spur tablet, bony spur pill, GUXIAN PIAN and GUXIANLING etc.These curative effect of medication neither be fine.
Technology contents:
The object of the invention is to provide a kind of medicine and preparation technology thereof who treats hyperosteogeny, also is to provide a kind of method of quality control of medicament capsule.
The present invention seeks to be achieved through the following technical solutions:
The present invention seeks to be achieved through the following technical solutions:
Radix Rehmanniae Preparata 120-180 weight portion Herba Cistanches 90-120 weight portion
Rhizoma Cibotii 90-120 weight portion Fructus Ligustri Lucidi 40-60 weight portion
Herba Epimedii 90-120 weight portion Caulis Spatholobi 90-120 weight portion
Semen Raphani 40-60 weight portion Rhizoma Drynariae 90-120 weight portion
Radix Achyranthis Bidentatae 90-120 weight portion
More than nine the flavor, get Rhizoma Cibotii, Radix Rehmanniae Preparata 90-120 weight portion, Herba Epimedii 40-60 weight portion, be ground into fine powder, Six-elements such as remaining Radix Rehmanniae Preparata, Herba Epimedii and Semen Raphani decoct with water twice, collecting decoction, filtration, filtrate concentrates salty thick paste shape, adds above-mentioned fine powder, make clinical acceptable forms, as oral liquid, capsule, granule, tablet etc.
Herba Cistanches of the present invention can be to steam, and Rhizoma Cibotii can be a processed with salt, and Fructus Ligustri Lucidi can be a processed with salt, and Semen Raphani can be parch.
The capsular method of quality control of present composition preparation is:
Differentiate: get capsule 's content, put microscopically and observe, the parenchyma taupe brown is to dark brown, and the many shrinkages of cell include brown nuclear shape thing; Scalariform tracheid is faint yellow to golden yellow, pit marshalling, the dark wavy bending of leaf epidermal cell wall;
Get capsule 's content 4g, add methanol 30ml, put in the water-bath reflux 0.5-1.5 hour, filter, filtrate evaporate to dryness, residue add 20-30% sulfuric acid solution 30ml makes dissolving, water-bath backflow 1-2.5 hour, put cold, with ether extraction 1-3 time, 30ml at every turn, merge ether solution, evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Other gets Radix Achyranthis Bidentatae control medicinal material 2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 3-5: 0.5-1.5: 0.3-0.6 toluene one ethyl acetate-formic acid is developing solvent, launch, take out, dry, spray is with the 8-12% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle of same color;
Get capsule 's content, mixing, porphyrize is got 1g, the accurate title, decide, and puts in the 100ml tool plug conical flask, and the accurate Diluted Alcohol that adds (is pressed 102 pages of an appendix regulation of Chinese Pharmacopoeia version in 2000 preparations, this liquid contains ethanol and should be 49.5%-50.5% (ml/ml) in the time of 20 ℃) 40-60ml, close plug claims to decide weight, supersound process 0.5-1.5 hour, put coldly, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, get filtrate 10ml, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 3-6: 0.5-1.5: 1-3: 0.5-1.5 ethyl acetate-acetone-methanol-water is developing solvent, launches, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; Assay: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, and 20-40: 60-80 second eyeball-water is mobile phase, the detection wavelength is 270nm, and number of theoretical plate calculates by the icariin peak should be not less than 1500; It is an amount of that the preparation of reference substance solution, precision take by weighing the icariin reference substance, makes the solution that every 1ml contains 20 μ g with dissolve with methanol, promptly; Capsule 's content is got in the preparation of need testing solution, mixing, porphyrize is got 1g, and accurate the title decides, put in the 100ml tool plug conical flask accurate Diluted Alcohol 40-60ml, the close plug of adding, claim to decide weight, supersound process 0.5-1.5 hour, put cold, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter with 0.35-0.55 μ m microporous filter membrane, promptly; Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, that is, every capsules content contains Herba Epimedii by icariin (C
33H
40O
15) must not count and be less than 0.3mg.
The present invention is through the influence experiment to the swelling of rat chondrus ocellatus Holmes property foot pawl, the rat granuloma induced by implantation of cotton pellets influence experiment, xylol cause the white mice auricle edema influence experiment, Dichlorodiphenyl Acetate cause white mice turn round the influence experiment of body, to a zhang white mouse drawer tail method analgesic influence experiment, influence experimental results show that pharmaceutical preparation of the present invention has the effect of antiinflammatory, analgesia, microcirculation improvement to white mice auricle note of the ancient Chinese circulation.
Capsule of the present invention has mends the waist kidney, and bone and muscle strengthening is invigorated blood circulation, the effect of promoting the circulation of QI, pain relieving; Be used for hyperplastic spondylitis (hypertrophy thoracic vertebra inflammation, fertile human nature spondylitis of lumbar vertebra), cervical vertebra syndrome, bony spur, case 640 examples are observed in clinical observation altogether, wherein treat thin 320 examples at random, at random matched group 320 examples.Result of the test shows: treatment group clinical cure example 12 (3.75%), produce effects example 86 (26.8%), effective 218 examples (68.1%), total effective rate 98.8%, determined curative effect.
Embodiment:
Radix Rehmanniae Preparata 175g Herba Cistanches (steaming) 117g Rhizoma Cibotii (processed with salt) 117g
Fructus Ligustri Lucidi (processed with salt) 58g Herba Epimedii 117g Caulis Spatholobi 117g
Semen Raphani (stir-fry) 58g Rhizoma Drynariae 117g Radix Achyranthis Bidentatae 117g
Make 1000, more than nine the flavor, get Rhizoma Cibotii, Radix Rehmanniae Preparata 117g, Herba Epimedii 58g, be ground into fine powder, Six-elements such as remaining Radix Rehmanniae Preparata, Herba Epimedii and Semen Raphani decoct with water collecting decoction, filtration 2 times, filtration is condensed into the thick paste shape, adds above-mentioned fine powder and an amount of refined honey, mixing, drying is ground into fine powder, incapsulates, make 1000, every dress 0.44g, oral, one time 5,3 times on the one.
Differentiate: get capsule 's content, put microscopically and observe, the parenchyma taupe brown is to dark brown, and the many shrinkages of cell include brown nuclear shape thing; Scalariform tracheid is faint yellow to golden yellow, pit marshalling, the dark wavy bending of leaf epidermal cell wall;
Get capsule 's content 4g, add methanol 30ml, put in the water-bath reflux 1 hour, filter, filtrate evaporate to dryness, residue add 25% sulfuric acid solution 30ml makes dissolving, water-bath refluxed 2 hours, put cold, with ether extraction 2 times, each 30ml, merge ether solution, evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution.Other gets Radix Achyranthis Bidentatae control medicinal material 2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 4: 1: 0.5 toluene one ethyl acetate-formic acid was developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle of same color;
Get capsule 's content, mixing, porphyrize, get 1g, the accurate title, decide, and puts in the 100ml tool plug conical flask, the accurate Diluted Alcohol 50ml that adds, close plug claims to decide weight, supersound process 1 hour is put coldly, supplies the weight that subtracts mistake with Diluted Alcohol, shake up, filter, get filtrate 10ml, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be the silica gel H F of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, with 5: 1: 2: 1 ethyl acetate-acetone-methanol-water is developing solvent, launches, and takes out, and dries, and puts under the 254nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the 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, and 30: 70 second eyeball-water is mobile phase, the detection wavelength is 270nm, and number of theoretical plate calculates by the icariin peak should be not less than 1500; It is an amount of that the preparation of reference substance solution, precision take by weighing the icariin reference substance, makes the solution that every 1ml contains 20 μ g with dissolve with methanol, promptly; Capsule 's content is got in the preparation of need testing solution, mixing, porphyrize is got 1g, and accurate the title decides, put in the 100ml tool plug conical flask accurate Diluted Alcohol 50ml, the close plug of adding, claim to decide weight, supersound process 1 hour is put cold, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter with 0.45 μ m microporous filter membrane, promptly; Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, that is, every contains Herba Epimedii by icariin (C
33H
40O
15) must not count and be less than 0.3mg.
Claims (8)
1, a kind of preparation method for the treatment of the hyperosteogeny medicine is characterized in that this method is:
Radix Rehmanniae Preparata 120-180 weight portion Herba Cistanches 90-120 weight portion
Rhizoma Cibotii 90-120 weight portion Fructus Ligustri Lucidi 40-60 weight portion
Herba Epimedii 90-120 weight portion Caulis Spatholobi 90-120 weight portion
Semen Raphani 40-60 weight portion Rhizoma Drynariae 90-120 weight portion
Radix Achyranthis Bidentatae 90-120 weight portion
More than nine the flavor, get Rhizoma Cibotii, Radix Rehmanniae Preparata 90-120 weight portion, Herba Epimedii 40-60 weight portion, be ground into fine powder, Six-elements such as remaining Radix Rehmanniae Preparata, Herba Epimedii and Semen Raphani decoct with water 2-3 time, collecting decoction, filtration, filtrate concentrates salty thick paste shape, adds above-mentioned fine powder, makes clinical acceptable forms.
2, preparation method as claimed in claim 1 is characterized in that this method is:
Radix Rehmanniae Preparata 175 weight portion Herba Cistanches (steaming) 117 weight portions
Canis familiaris L. family dependant (processed with salt) 117 weight portion Fructus Ligustri Lucidi (processed with salt) 58 weight portions
Herba Epimedii 117 weight portion Caulis Spatholobis 117 weight portions
Semen Raphani (stir-fry) 58 weight portion Rhizoma Drynariae 117 weight portions
Radix Achyranthis Bidentatae 117 weight portions
More than nine the flavor, get Rhizoma Cibotii, Radix Rehmanniae Preparata 117 weight portions, Herba Epimedii 58 weight portions, be ground into fine powder, Six-elements such as remaining Radix Rehmanniae Preparata, Herba Epimedii and Semen Raphani decoct with water twice, collecting decoction, filtration, filtering concentrates salty thick paste shape, add above-mentioned fine powder and an amount of refined honey, mixing, drying, be ground into fine powder, make capsule.
3, method prepares capsular discrimination method as claimed in claim 1 or 2, it is characterized in that this method is:
Get capsule 's content, put microscopically and observe, the parenchyma taupe brown is to dark brown, and the many shrinkages of cell include brown nuclear shape thing; Scalariform tracheid is faint yellow to golden yellow, pit marshalling, the dark wavy bending of leaf epidermal cell wall;
Get capsule 's content 4g, add methanol 30ml, put in the water-bath reflux 0.5-1.5 hour, filter, filtrate evaporate to dryness, residue add 20-30% sulfuric acid solution 30ml makes dissolving, water-bath backflow 1-2.5 hour, put cold, with ether extraction 1-3 time, 30ml at every turn, merge ether solution, evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Other gets Radix Achyranthis Bidentatae control medicinal material 2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 3-5: 0.5-1.5: 0.3-0.6 toluene one ethyl acetate-formic acid is developing solvent, launch, take out, dry, spray is with the 8-12% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle of same color;
Get capsule 's content, mixing, porphyrize, get 1g, the accurate title, decide, and puts in the 100ml tool plug conical flask, the accurate Diluted Alcohol 40-60ml that adds, close plug claims to decide weight, supersound process 0.5-1.5 hour, put coldly, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, get filtrate 10ml, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 3-6: 0.5-1.5: 1-3: 0.5-1.5 ethyl acetate one acetone one methanol one water is developing solvent, launches, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
4, as discrimination method as described in the claim 3, it is characterized in that this method is:
Get capsule 's content, put microscopically and observe, the parenchyma taupe brown is to dark brown, and the many shrinkages of cell include brown nuclear shape thing; Scalariform tracheid is faint yellow to golden yellow, pit marshalling, the dark wavy bending of leaf epidermal cell wall;
Get capsule 's content 4g, add methanol 30ml, put in the water-bath reflux 1 hour, filter, filtrate evaporate to dryness, residue add 25% sulfuric acid solution 30ml makes dissolving, water-bath refluxed 2 hours, put cold, with ether extraction 2 times, each 30ml, merge ether solution, evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution.Other gets Radix Achyranthis Bidentatae control medicinal material 2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 4: 1: 0.5 toluene one ethyl acetate-formic acid was developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle of same color;
Get capsule 's content, mixing, porphyrize, get 1g, the accurate title, decide, and puts in the 100ml tool plug conical flask, the accurate Diluted Alcohol 50ml that adds, close plug claims to decide weight, supersound process 1 hour is put coldly, supplies the weight that subtracts mistake with Diluted Alcohol, shake up, filter, get filtrate 10ml, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be the silica gel H F of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, with 5: 1: 2: 1 ethyl acetate-acetone-methanol-water is developing solvent, launches, and takes out, and dries, and puts under the 254nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
5, method prepares capsular content assaying method as claimed in claim 1 or 2, it is characterized in that this method is:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, and 20-40: 60-80 second eyeball-water is mobile phase, and the detection wavelength is 270nm, and number of theoretical plate calculates by the icariin peak should be not less than 1500; It is an amount of that the preparation of reference substance solution, precision take by weighing the icariin reference substance, makes the solution that every 1ml contains 20 μ g with dissolve with methanol, promptly; Capsule 's content is got in the preparation of need testing solution, mixing, porphyrize is got 1g, and accurate the title decides, put in the 100ml tool plug conical flask accurate Diluted Alcohol 40-60ml, the close plug of adding, claim to decide weight, supersound process 0.5-1.5 hour, put cold, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter with 0.35-0.55 μ m microporous filter membrane, promptly; Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, that is, every capsules content contains Herba Epimedii must not be less than 0.3mg by icariin.
6, as content assaying method as described in the claim 5, it is characterized in that this method is:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, and 30: 70 second eyeball-water is mobile phase, and the detection wavelength is 270nm, and number of theoretical plate calculates by the icariin peak should be not less than 1500; It is an amount of that the preparation of reference substance solution, precision take by weighing the icariin reference substance, makes the solution that every 1ml contains 20 μ g with dissolve with methanol, promptly; Capsule 's content is got in the preparation of need testing solution, mixing, porphyrize is got 1g, and accurate the title decides, put in the 100ml tool plug conical flask accurate Diluted Alcohol 50ml, the close plug of adding, claim to decide weight, supersound process 1 hour is put cold, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter with 0.45 μ m microporous filter membrane, promptly; Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, that is, every contains Herba Epimedii and must not be less than 0.3mg by icariin.
7, method prepares capsular method of quality control as claimed in claim 1 or 2, it is characterized in that this method is:
Get capsule 's content, put microscopically and observe, the parenchyma taupe brown is to dark brown, and the many shrinkages of cell include brown nuclear shape thing; Scalariform tracheid is faint yellow to golden yellow, pit marshalling, the dark wavy bending of leaf epidermal cell wall;
Get capsule 's content 4g, add methanol 30ml, put in the water-bath reflux 0.5-1.5 hour, filter, filtrate evaporate to dryness, residue add 20-30% sulfuric acid solution 30ml makes dissolving, water-bath backflow 1-2.5 hour, put cold, with ether extraction 1-3 time, 30ml at every turn, merge ether solution, evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Other gets Radix Achyranthis Bidentatae control medicinal material 2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 3-5: 0.5-1.5: 0.3-0.6 toluene one ethyl acetate-formic acid is developing solvent, launch, take out, dry, spray is with the 8-12% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle of same color;
Get capsule 's content, mixing, porphyrize, get 1g, the accurate title, decide, and puts in the 100ml tool plug conical flask, the accurate Diluted Alcohol 40-60ml that adds, close plug claims to decide weight, supersound process 0.5-1.5 hour, put coldly, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, get filtrate 10ml, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 3-6: 0.5-1.5: 1-3: 0.5-1.5 ethyl acetate-acetone-methanol-water is developing solvent, launches, take out, dry, put under the ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay: according to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, and 20-40: 60-80 second eyeball-water is mobile phase, the detection wavelength is 270nm, and number of theoretical plate calculates by the icariin peak should be not less than 1500; It is an amount of that the preparation of reference substance solution, precision take by weighing the icariin reference substance, makes the solution that every 1ml contains 20 μ g with dissolve with methanol, promptly; Capsule 's content is got in the preparation of need testing solution, mixing, porphyrize is got 1g, and accurate the title decides, put in the 100ml tool plug conical flask accurate Diluted Alcohol 40-60ml, the close plug of adding, claim to decide weight, supersound process 0.5-1.5 hour, put cold, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter with 0.35-0.55 μ m microporous filter membrane, promptly; Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, that is, every capsules content contains Herba Epimedii must not be less than 0.3mg by icariin.
8, prepare capsular method of quality control as method as described in the claim 7, it is characterized in that this method is:
Get capsule 's content, put microscopically and observe, the parenchyma taupe brown is to dark brown, and the many shrinkages of cell include brown nuclear shape thing; Scalariform tracheid is faint yellow to golden yellow, pit marshalling, the dark wavy bending of leaf epidermal cell wall;
Get capsule 's content 4g, add methanol 30ml, put in the water-bath reflux 1 hour, filter, filtrate evaporate to dryness, residue add 25% sulfuric acid solution 30ml makes dissolving, water-bath refluxed 2 hours, put cold, with ether extraction 2 times, each 30ml, merge ether solution, evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution.Other gets Radix Achyranthis Bidentatae control medicinal material 2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 4: 1: 0.5 toluene one ethyl acetate-formic acid was developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material on, show the speckle of same color;
Get capsule 's content, mixing, porphyrize is got 1g, the accurate title, decide, and puts in the 100ml tool plug conical flask, the accurate Diluted Alcohol 50ml that adds, close plug claims to decide weight, supersound process 1 hour, put coldly, supply the weight that subtracts mistake, shake up with Diluted Alcohol, filter, promptly get solution, get filtrate 10ml, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets the icariin reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be the silica gel H F of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, with 5: 1: 2: 1 ethyl acetate-acetone-methanol-water is developing solvent, launches, and takes out, and dries, and puts under the 254nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the 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, and 30: 70 second eyeball-water is mobile phase, the detection wavelength is 270nm, and number of theoretical plate calculates by the icariin peak should be not less than 1500; It is an amount of that the preparation of reference substance solution, precision take by weighing the icariin reference substance, makes the solution that every 1ml contains 20 μ g with dissolve with methanol, promptly; Capsule 's content is got in the preparation of need testing solution, mixing, porphyrize is got 1g, and accurate the title decides, put in the 100ml tool plug conical flask accurate Diluted Alcohol 50ml, the close plug of adding, claim to decide weight, supersound process 1 hour is put cold, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter with 0.45 μ m microporous filter membrane, promptly; Accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject chromatograph of liquid, measure, that is, every contains Herba Epimedii and must not be less than 0.3mg by icariin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN02128966.2A CN1308001C (en) | 2002-08-23 | 2002-08-23 | Medicine for curing hyperasteogeny and its preparation process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN02128966.2A CN1308001C (en) | 2002-08-23 | 2002-08-23 | Medicine for curing hyperasteogeny and its preparation process |
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| Publication Number | Publication Date |
|---|---|
| CN1476853A true CN1476853A (en) | 2004-02-25 |
| CN1308001C CN1308001C (en) | 2007-04-04 |
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| CN103751481A (en) * | 2014-01-23 | 2014-04-30 | 胡伟 | Oral traditional Chinese medicine for treating heel pain |
| CN107184728A (en) * | 2017-05-22 | 2017-09-22 | 漯河医学高等专科学校 | A kind of collaterals and relieving pain cream and preparation method thereof |
-
2002
- 2002-08-23 CN CN02128966.2A patent/CN1308001C/en not_active Expired - Lifetime
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102768251A (en) * | 2012-08-02 | 2012-11-07 | 江苏康缘药业股份有限公司 | Finger-print detection method of traditional Chinese medicine composition for treating osteoproliferation |
| CN102920887A (en) * | 2012-11-29 | 2013-02-13 | 广西梧州三鹤药业有限公司 | Chinese medicinal composition for treating hyperostosis |
| CN103751481A (en) * | 2014-01-23 | 2014-04-30 | 胡伟 | Oral traditional Chinese medicine for treating heel pain |
| CN103751481B (en) * | 2014-01-23 | 2016-02-17 | 胡伟 | One treats talalgia Chinese medicine for oral administration |
| CN107184728A (en) * | 2017-05-22 | 2017-09-22 | 漯河医学高等专科学校 | A kind of collaterals and relieving pain cream and preparation method thereof |
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