CN101011533B - Chinese traditional medicine composition for treating kidney-yang deficiency and preparation and quality controlling method thereof - Google Patents
Chinese traditional medicine composition for treating kidney-yang deficiency and preparation and quality controlling method thereof Download PDFInfo
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- CN101011533B CN101011533B CN2007100634539A CN200710063453A CN101011533B CN 101011533 B CN101011533 B CN 101011533B CN 2007100634539 A CN2007100634539 A CN 2007100634539A CN 200710063453 A CN200710063453 A CN 200710063453A CN 101011533 B CN101011533 B CN 101011533B
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Abstract
The invention relates to a method for preparing the traditional drug compound used to treat deficiency of the kidney and relative quality control method. The inventive compound comprises honey powder, bee milk freeze powder, broken gen-seng, dry human placenta and Cordyceps sinensis, to be added with 9-11 times of water to be boiled for 2-3 times, while each time costs 1-3h, to be combined and boiled, filter, concentrated into the clear paste at 1.20-1.25 (55-65Deg. C) density, to be depressurized and dried into dry paste, to be broken into powder and mixed with the honey powder, bee milk freeze powder and red ginseng powder, to be screened and packed into capsule. The invention uses high-effect liquid spectrum to test the content of panaxoside Rb1. The inventive compound can be used to treat insomnia, dizziness or the like caused by the deficiency of vital energy.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof and method of quality control, particularly relate to a kind of Chinese medicine composition for the treatment of insufficiency of kidney-YANG and preparation method thereof and method of quality control.
Background technology
Kidney storing essence, suffering from a deficiency of the kidney with the deficiency of kidney-essence is cardinal symptom.General symptom spiritedness is tired, dizzy, tinnitus, forgetful, waist, seminal emission, sexual impotence etc., and clinical manifestation can be partial to deficiency of the kidney yin, or insufficiency of kidney-YANG.The meaning of losing is not enough, can be the deficiency of function with kidney, is exactly insufficiency of kidney-YANG.If the deficiency of basic substance is exactly a deficiency of the kidney yin.In general, the deficiency of function also can cause the minimizing of basic substance, and both can transform negative and positive mutually.Going down of renal function, the men and women all has, and not only is thicker than the male, is the cacodoxy that the male is incorrectly relayed an erroneous message, or the natural pressure all next with body, and the deficiency of the kidney disease that is caused is more.
For suffering from a deficiency of the kidney is exactly a kind of notion of Chinese medicine originally, and motherland's medical science is for a hack of Therapeutic Method and the effective medicine of having suffered from a deficiency of the kidney, the also better patent medicine of prescription might as well, all very effective.Deficiency of the kidney yin treatment rule is enriching yin and nourishing kidney in general.And insufficiency of kidney-YANG is exactly reinforcing the kidney and supporting YANG certainly, by replenishing the method for kidney yin, allows after the kidney essense abundance, and its inclined to one side Sheng declines partially and just can have been corrected.Insufficiency of kidney-YANG replenishes some medicines of kidney qi, adjusts.The right Testudinis ball of our prescriptions more commonly used, right Testudinis are drawn and are the treatment insufficiency of kidney-YANG.Necessarily be noted that the necessary tonifying kidney-yin of kidney-replenishing when treatment, this is the rule that Chinese traditional treatment is suffered from a deficiency of the kidney.
Summary of the invention
The object of the invention is to provide a kind of Chinese medicine composition for the treatment of insufficiency of kidney-YANG;
The object of the invention also is to provide a kind of Chinese medicine composition preparation method for the treatment of insufficiency of kidney-YANG;
The object of the invention also is to provide a kind of method of quality control for the treatment of the Chinese medicine composition of insufficiency of kidney-YANG.
The present invention seeks to be achieved through the following technical solutions:
The described a kind of Chinese medicine composition for the treatment of insufficiency of kidney-YANG of the object of the invention can be realized by following technical scheme:
Radix Ginseng 70-180 weight portion Placenta Hominis 100-200 weight portion
Radix Polygoni Multiflori Preparata 30-100 weight portion Fructus Lycii 10-70 weight portion
Cordyceps 10-30 weight portion Herba Epimedii (processing) 30-110 weight portion
Rhizoma Polygonati 10-70 weight portion Radix Notoginseng 10-50 weight portion
Bee pollen 10-70 weight portion Radix Glycyrrhizae 10-70 weight portion Lac regis apis (lyophilized powder) 5-25 weight portion.
The Chinese medicine composition of treatment insufficiency of kidney-YANG of the present invention can be made by the crude drug of following weight ratio:
Radix Ginseng Rubra 70-180 weight portion Radix Astragali 70-180 weight portion Cornu Cervi Pantotrichum 10-60 weight portion
Radix Polygoni Multiflori Preparata 30-100 weight portion Fructus Lycii 10-70 weight portion Cordyceps 10-30 weight portion
Herba Epimedii (processing) 30-110 weight portion Rhizoma Polygonati 10-70 weight portion Radix Salviae Miltiorrhizae 30-100 weight portion
Bee pollen 10-70 weight portion Radix Glycyrrhizae 10-70 weight portion Lac regis apis (lyophilized powder) 5-25 weight portion.
The Chinese medicine composition of treatment insufficiency of kidney-YANG of the present invention is preferably as follows that the crude drug of weight ratio makes:
Radix Ginseng Rubra 79-90 weight portion Radix Astragali 120-180 weight portion Cornu Cervi Pantotrichum 50-60 weight portion
Radix Polygoni Multiflori Preparata 70-100 weight portion Fructus Lycii 50-70 weight portion Cordyceps 10-15 weight portion
Herba Epimedii (processing) 90-110 weight portion Rhizoma Polygonati 50-70 weight portion Radix Salviae Miltiorrhizae 80-100 weight portion
Bee pollen 40-70 weight portion Radix Glycyrrhizae 10-15 weight portion Lac regis apis (lyophilized powder) 5-10 weight portion.
The Chinese medicine composition of treatment insufficiency of kidney-YANG of the present invention is preferably as follows that the crude drug of weight ratio makes:
The Radix Ginseng Rubra 75 weight portion Radixs Astragali 130 weight portion Cornu Cervi Pantotrichums 55 weight portions
Radix Polygoni Multiflori Preparata 75 weight portion Fructus Lycii 60 weight portion Cordyceps 13 weight portions
Herba Epimedii (processing) 95 weight portion Rhizoma Polygonatis 60 weight portion Radix Salviae Miltiorrhizaes 90 weight portions
Bee pollen 60 weight portion Radix Glycyrrhizaes 12 weight portion Lac regis apis (lyophilized powder) 8 weight portions.
The Chinese medicine composition of treatment insufficiency of kidney-YANG of the present invention is preferably as follows that the crude drug of weight ratio makes:
The Radix Ginseng Rubra 85 weight portion Radixs Astragali 160 weight portion Cornu Cervi Pantotrichums 58 weight portions
Radix Polygoni Multiflori Preparata 85 weight portion Fructus Lycii 65 weight portion Cordyceps 14 weight portions
Herba Epimedii (processing) 100 weight portion Rhizoma Polygonatis 60 weight portion Radix Salviae Miltiorrhizaes 85 weight portions
Bee pollen 65 weight portion Radix Glycyrrhizaes 15 weight portion Lac regis apis (lyophilized powder) 7 weight portions.
The preparation method of Chinese medicinal composition capsules preparation of the present invention is:
Choose crude drug:
Radix Ginseng 70-180 weight portion Placenta Hominis 100-200 weight portion
Radix Polygoni Multiflori Preparata 30-100 weight portion Fructus Lycii 10-70 weight portion
Cordyceps 10-30 weight portion Herba Epimedii (processing) 30-110 weight portion
Rhizoma Polygonati 10-70 weight portion Radix Notoginseng 10-50 weight portion
Bee pollen 10-70 weight portion Radix Glycyrrhizae 10-70 weight portion Lac regis apis (lyophilized powder) 5-25 weight portion.
Except that bee pollen, Lac regis apis lyophilized powder, Radix Ginseng, Placenta Hominis, Cordyceps are ground into fine powder, all the other Six-elements, adding 9-11 times of water gaging decocts 2-3 time, each 1-3 hour, collecting decoction filtered, filtrate is concentrated into the clear paste that relative density is 1.20-1.25 (55-65 a ℃), drying under reduced pressure becomes dry extract, is ground into fine powder, sieves with fine powder mixings such as above-mentioned bee pollen, Lac regis apis lyophilized powder and Radix Ginseng Rubra, incapsulate, promptly.
The preparation method of Chinese medicinal composition capsules preparation of the present invention is:
Choose crude drug:
Radix Ginseng Rubra 70-180 weight portion Radix Astragali 70-180 weight portion Cornu Cervi Pantotrichum 10-60 weight portion
Radix Polygoni Multiflori Preparata 30-100 weight portion Fructus Lycii 10-70 weight portion Cordyceps 10-30 weight portion
Herba Epimedii (processing) 30-110 weight portion Rhizoma Polygonati 10-70 weight portion Radix Salviae Miltiorrhizae 30-100 weight portion
Bee pollen 10-70 weight portion Radix Glycyrrhizae 10-70 weight portion Lac regis apis (lyophilized powder) 5-25 weight portion.
Except that bee pollen, Lac regis apis lyophilized powder, Radix Ginseng Rubra, Cornu Cervi Pantotrichum, Cordyceps are ground into fine powder, seven flavors such as all the other Radixs Astragali, adding 9-11 times of water gaging decocts 2-3 time, each 1-3 hour, collecting decoction filtered, filtrate is concentrated into the clear paste that relative density is 1.20-1.25 (55-65 a ℃), drying under reduced pressure becomes dry extract, is ground into fine powder, sieves with fine powder mixings such as above-mentioned bee pollen, Lac regis apis lyophilized powder and Radix Ginseng Rubra, incapsulate, promptly.
The preparation method of Chinese medicinal composition capsules preparation of the present invention is preferably:
Choose crude drug:
Radix Ginseng Rubra 70-90 weight portion Radix Astragali 120-180 weight portion Cornu Cervi Pantotrichum 50-60 weight portion
Radix Polygoni Multiflori Preparata 70-100 weight portion Fructus Lycii 50-70 weight portion Cordyceps 10-15 weight portion
Herba Epimedii (processing) 90-110 weight portion Rhizoma Polygonati 50-70 weight portion Radix Salviae Miltiorrhizae 80-100 weight portion
Bee pollen 40-70 weight portion Radix Glycyrrhizae 10-15 weight portion Lac regis apis (lyophilized powder) 5-10 weight portion.
Except that bee pollen, Lac regis apis lyophilized powder, Radix Ginseng Rubra, Cornu Cervi Pantotrichum, Cordyceps are ground into fine powder, seven flavors such as all the other Radixs Astragali, add 10 times of water gagings and decoct secondary, each 2 hours, collecting decoction filtered, filtrate is concentrated into the clear paste that relative density is 1.20-1.25 (60 ℃), drying under reduced pressure becomes dry extract, is ground into fine powder, sieves with fine powder mixings such as above-mentioned bee pollen, Lac regis apis lyophilized powder and Radix Ginseng Rubra, incapsulate, promptly.
Pharmaceutical composition method of quality control of the present invention comprises one or more in following discrimination method and/or the assay:
Differentiate:
(1) gets ginsenoside Rb, Re, Rg and astragaloside reference substance, add methanol and make the mixed solution that every 1ml contains 1mg, in contrast product solution; The need testing solution preparation: get the content under the present composition capsule content uniformity item, mixing is got about 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, puts in the water-bath heating and refluxing extraction 1-3 hour, take out, put coldly, claim to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured filtrate 25ml, puts in the evaporating dish evaporate to dryness, residue adds water 25ml separates solution, and move in the separatory funnel, add the chloroform jolting and extract 1-3 time, each 15ml, discard chloroform solution, water liquid extracts 3-5 time with water saturated n-butyl alcohol jolting, and each 20ml merges n-butyl alcohol liquid, add ammonia solution 30ml washing, discard cleaning mixture, n-butyl alcohol liquid places evaporate to dryness in the water-bath, and residue adds quantity of methyl alcohol makes dissolving; And quantitatively be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly;
Test according to thin layer chromatography, draw need testing solution 10 μ l, above-mentioned reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, (11-15: 6-9: 1-3) lower floor's solution of placing below 10 ℃ is developing solvent, launches, and takes out with chloroform-methanol-water, dry, spray is with the 9-11% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing, puts respectively under daylight and the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle or the fluorescence speckle of same color;
(2) get the icariin reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution;
The preparation of need testing solution is got the content under the present composition capsule content uniformity item, mixing, get about 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, put in the water-bath heating and refluxing extraction 1-2 hour, and took out, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured filtrate 25ml, puts in the evaporating dish, evaporate to dryness, residue add water 25ml separates solution, and moves in the separatory funnel, adding the chloroform jolting extracts 2-3 time, each 15ml discards chloroform solution, and water liquid extracts 3-5 time with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, add ammonia solution 30ml washing, discard cleaning mixture, n-butyl alcohol liquid places evaporate to dryness in the water-bath, and residue adds quantity of methyl alcohol makes dissolving; And quantitatively be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly; Test according to thin layer chromatography, draw each 5 μ l of need testing solution and above-mentioned reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (9-11: 1-2: 1-2: 1-2) be developing solvent, launch, take out, dry, spray, is put under the ultra-violet lamp (365nm) and is inspected 105C heating several minutes with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(3) get present composition capsule content 5g, add methanol 50m; , put in the water-bath reflux 1-2 hour, take out, put coldly, filter, filtrate evaporate to dryness, residue add water 20ml makes solution, extract 2-3 time with the chloroform jolting, 15ml at every turn, combined chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Fructus Lycii control medicinal material 1g, decoct with water 10-20 minute, filter, filtrate is shone medical material solution in pairs with legal system, test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform one ethyl acetate one methanol (3-5: 2-4: 0.2-0.5) be 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 the fluorescence 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; Acetonitrile-water (27-31: 69-74) be mobile phase; The detection wavelength is 203nm; Column temperature 38-42C.Number of theoretical plate calculates by the ginsenoside Rb1 peak should be not less than 2500.
The preparation of reference substance solution, precision take by weighing ginsenoside Rb
1Reference substance 7.5mg puts in the 25ml measuring bottle, adds methanol and makes solution, and be diluted to scale, shakes up, and promptly gets (to contain ginsenoside Rb among every 1ml
10.3mg).
The preparation of need testing solution is got the content under the present composition capsule content uniformity item, mixing, get about 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, put in the water-bath heating and refluxing extraction 1-2 hour, and took out, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured filtrate 25ml, puts in the evaporating dish, evaporate to dryness, residue add water 25ml separates solution, and moves in the separatory funnel, adding the chloroform jolting extracts 2-3 time, each 15ml discards chloroform solution, and water liquid extracts 3-5 time with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, add ammonia solution 30ml washing, discard cleaning mixture, n-butyl alcohol liquid places evaporate to dryness in the water-bath, and residue adds quantity of methyl alcohol makes dissolving.And quantitatively be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly.
Algoscopy, accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, measure, promptly.Every of present composition capsule contains ginsenoside Rb
1(C
54H
92O
23), must not be less than 0.40mg.
Pharmaceutical composition method of quality control of the present invention is preferably as follows one or more in discrimination method and/or the assay:
Differentiate:
A, get ginsenoside Rb, Re, Rg and astragaloside reference substance, add methanol and make the mixed solution that every 1ml contains 1mg, in contrast product solution; The need testing solution preparation: get the content under the present composition capsule content uniformity item, mixing is got about 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, puts in the water-bath heating and refluxing extraction 1.5 hours, take out, put coldly, claim to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured filtrate 25ml, puts in the evaporating dish evaporate to dryness, residue adds water 25ml separates solution, and move in the separatory funnel, add the chloroform jolting and extract 2 times, each 15ml, discard chloroform solution, water liquid extracts 4 times with water saturated n-butyl alcohol jolting, and each 20ml merges n-butyl alcohol liquid, add ammonia solution 30ml washing, discard cleaning mixture, n-butyl alcohol liquid places evaporate to dryness in the water-bath, and residue adds quantity of methyl alcohol makes dissolving; And quantitatively be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly;
Test according to thin layer chromatography, draw need testing solution 10 μ l, above-mentioned reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water (13: 7: 2) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing, puts respectively under daylight and the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle or the fluorescence speckle of same color;
B, get the icariin reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution;
The preparation of need testing solution is got the content under the present composition capsule content uniformity item, mixing, get about 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, put in the water-bath heating and refluxing extraction 1.5 hours, and took out, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured filtrate 25ml, puts in the evaporating dish, evaporate to dryness, residue add water 25ml separates solution, and moves in the separatory funnel, adding the chloroform jolting extracts 2 times, each 15ml discards chloroform solution, and water liquid extracts 4 times with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, add ammonia solution 30ml washing, discard cleaning mixture, n-butyl alcohol liquid places evaporate to dryness in the water-bath, and residue adds quantity of methyl alcohol makes dissolving; And quantitatively be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly; Test according to thin layer chromatography, draw each 5 μ l of need testing solution and above-mentioned reference substance solution, put respectively on same silica gel g thin-layer plate, (10: 1: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, spray, is put under the ultra-violet lamp (365nm) and is inspected 105C heating several minutes with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
C, get present composition capsule content 5g, add methanol 50m; , put in the water-bath reflux 1 hour, take out, put coldly, filter, filtrate evaporate to dryness, residue add water 20ml makes solution, extracts 2 times with the chloroform jolting, each 15ml, combined chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Fructus Lycii control medicinal material 1g, decoct with water 15 minutes, filter, filtrate is shone medical material solution in pairs with legal system, test according to thin layer chromatography, drawing each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with chloroform one ethyl acetate, one methanol (4: 2: 0.3), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
Assay:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-water (29: 71) is a mobile phase; The detection wavelength is 203nm; Column temperature 40C; Number of theoretical plate is by ginsenoside Rb
1The peak calculates should be not less than 2500;
The preparation of reference substance solution, precision take by weighing ginsenoside Rb
1Reference substance 7.5mg puts in the 25ml measuring bottle, adds methanol and makes solution, and be diluted to scale, shakes up, and promptly gets (to contain ginsenoside Rb among every 1ml
10.3mg);
The preparation of need testing solution is got the content under the present composition capsule content uniformity item, mixing, get about 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, put in the water-bath heating and refluxing extraction 1.5 hours, and took out, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured filtrate 25ml, puts in the evaporating dish, evaporate to dryness, residue add water 25ml separates solution, and moves in the separatory funnel, adding the chloroform jolting extracts 2 times, each 15ml discards chloroform solution, and water liquid extracts 4 times with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, add ammonia solution 30ml washing, discard cleaning mixture, n-butyl alcohol liquid places evaporate to dryness in the water-bath, and residue adds quantity of methyl alcohol makes dissolving; And quantitatively be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly;
Algoscopy, accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, measure, promptly; Every of present composition capsule contains ginsenoside Rb
1(C
54H
92O
23), must not be less than 0.40mg.
The present composition has good drug effect, has the QI invigorating replenishing essence, reinforcing the kidney and supporting YANG, and effect, to deficiency of vital energy damage of essence, the spiritlessness and weakness that insufficiency of kidney-YANG causes, insomnia is dizzy,, soreness of the waist and knees, aversion to cold and cold limbs, inappetence, diseases such as shortness of breath and palpitation have good effect.Compare existing preparation and also show outstanding drug effect, and scope of the present invention through screening, finds in some scope of compositions, more outstanding drug effect is arranged realizing pharmacological effect of the present invention simultaneously unexpectedly.
The method of quality control of Chinese medicine composition provided by the present invention, be by obtaining behind the creative experiment sieving of big measuring, pass through screening in the discrimination method to sample treatment, the selection of developing solvent, make and differentiate that specificity is fine, and method is economic and practical, the result is quick, and can both use different lamellaes.Pass through screening in the content assaying method to sample, test sample processing method, the selection of developing solvent, make content assaying method effectivelyly to carry out quality control, and will compare more stable that product that additive method measures shows on pharmacological effect with the product that this method is measured to product.
The specific embodiment
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Experimental example 1
The experiment medicine is embodiment 2 preparations, compares with the Chinese patent medicine Yougui Wan, the kidney-Yang-Reinforcing Bolus of existing similar effect, and according to following experimental technique, at spiritlessness and weakness, insomnia is dizzy, soreness of the waist and knees, and aversion to cold and cold limbs, inappetence, all there is better effect disease aspects such as shortness of breath and palpitation.
Experimental example 2
Prescription I:
Radix Ginseng Rubra 75g Radix Astragali 130g Cornu Cervi Pantotrichum 55g
Radix Polygoni Multiflori Preparata 75g Fructus Lycii 60g Cordyceps 13g
Herba Epimedii (processing) 95g Rhizoma Polygonati 60g Radix Salviae Miltiorrhizae 90g
Bee pollen 60g Radix Glycyrrhizae 12g Lac regis apis (lyophilized powder) 8g
Prescription II:
Radix Ginseng Rubra 85g Radix Astragali 160g Cornu Cervi Pantotrichum 58g
Radix Polygoni Multiflori Preparata 85g Fructus Lycii 65g Cordyceps 14g
Herba Epimedii (processing) 100g Rhizoma Polygonati 60g Radix Salviae Miltiorrhizae 85g
Bee pollen 65g Radix Glycyrrhizae 15g Lac regis apis (lyophilized powder) 7g
Matched group:
Radix Ginseng Rubra 108g Radix Astragali 108g Cornu Cervi Pantotrichum 36g
Radix Polygoni Multiflori Preparata 60g Fructus Lycii 36g Cordyceps 20g
Herba Epimedii (processing) 72g Rhizoma Polygonati 36g Radix Salviae Miltiorrhizae 60g
Bee pollen 24g Radix Glycyrrhizae 28g Lac regis apis (lyophilized powder) 12g
According to the prescription ratio weighting raw materials material of medicine group I, medicine group II and matched group, according to the foregoing description 1 prepared, relatively treat the sexual impotence effect, the results are shown in following table.
Medicine of the present invention is to the influence of castrated rats weight of reproductive organs
Annotate: * medicine group I, II compare P＜0.05 with matched group.
The result shows: the control drug composition capsule to the influence and the medicine group I of castrated rats weight of reproductive organs, there were significant differences for the II capsule (P＜0.05), medicine group I, II to the influence of castrated rats weight of reproductive organs apparently higher than control drug pharmaceutical capsules group.
Experimental example 3 tranquilizing effects
Get 20 of Kunming mouses, body weight 18-22g, the male and female dual-purpose is divided into 2 groups at random, 10 every group.Normal saline matched group (matched group): give normal saline 0.2ml/10g and irritate stomach, every day 1 time, totally 3 days.JIEYUANSHEN KELI group (medicine of the present invention): get the drug sample liquid 0.2ml/10g of the present invention for preparing and irritate stomach (be equivalent to people's consumption 9 times), per 1 time, they 3 days.Each is organized last and irritates 1h behind the stomach, after mice is put into the spontaneous activity instrument and adapts to 3 minutes, begins to measure the spontaneous activity number of times and sleep surpasses 2 hours the length of one's sleep.The results are shown in following table:
Influence to the spontaneous activity in mice number of times and the length of one's sleep
| Group | Dosage (g/kg) | The spontaneous activity number of times | The length of one's sleep (min) |
| Matched group | - | 169.7±63.1 | 40.0±15.5 |
| Medicine of the present invention | 1.5 | 102.6±57.7* | 49.7±14.8* |
| Medicine of the present invention | 3.0 | 89.2±51.3* | 61.3±15.9* |
| Medicine of the present invention | 4.0 | 70.4±22.3** | 77.8±25.0** |
Annotate: compare * P＜0.05, * * P＜0.01 with matched group
The result shows: the high, medium and low dosage group of medicine of the present invention all has tranquilizing effect, along with the increasing tranquilizing effect enhancing of dosage.
Experimental example 4 promotes the stomach function
1, to the influence of rat gastric juice secretory function
40 of rats, be divided into 4 groups at random, first, second, third group are irritated stomach medicine 1.5,3.0 of the present invention, 4.0g/kg respectively, and the fourth group is irritated stomach with the volume normal saline, successive administration 7 days, fasting 24 hours (can't help water) after the last administration, etherization is opened the abdominal cavity, the ligation pylorus, inject above-mentioned various medicine 1.8ml (0.9g) through duodenum, sew up the abdominal cavity then, the exhausted water 5 hours of going on a hunger strike.Reuse etherization after 5 hours, open the abdominal cavity, the ligation cardia, take off stomach, filter gastric juice with two layers of cloth respectively, to the scale test tube, with the centrifugal 15min of 3000r/min, record supernatant liquid measure is a gastric juice, uses acidometer xylometric measurement, the special capillary test method of wheat respectively, and mensuration free acidity, total acidity the results are shown in following table:
Influence to rat gastric juice secretory function
| Group | Dosage (g/kg) | Gastric juice amount (ml/5h) | Free acidity (mol) | Total acidity (mol) |
| N.S | 6.6±1.6 | 33.7±11.2 | 77.8±15.8 | |
| Medicine of the present invention | 1.5 | 10.3±1.8 * | 40.7±12.5 * | 117.3±19.1 * |
| Medicine of the present invention | 3.0 | 11.2±1.6 * | 49.5±14.1 * | 120.8±7.2 * |
| Medicine of the present invention | 4.0 | 13.8±2.1 * | 62.8±14.8 * | 134.3±18.4 * |
Annotate: compare * P＜0.05, * * P＜0.01 with matched group
The result shows: high, medium and low dose of medicine of the present invention can promote at the Mus gastric secretion, improve free acidity and total acidity output, and pepsin activity is strengthened, and its effect is strengthened along with the increasing of dosage.
2, to the influence of rat gastric juice secretory function
40 of rats, be divided into 4 groups at random, irritate the basic, normal, high dosage group 1.5,3.0 of stomach drug suspension of the present invention, 4.0g/kg respectively, the blank group is irritated stomach with the volume normal saline, successive administration 7 days, fasting 24 hours (can't help water) after the last administration, irritating the Weishang respectively states medicine and is made into physiological water and contains each suspension 0.2ml/10g body weight of 10% of carbon powder and arabic gum, with the cervical vertebra dislocation method mice is put to death after 15 minutes, cut open immediately by literature method and operate, calculate the intestinal propulsion rate, the results are shown in Table:
| Group | Dosage (g/kg) | Pepsin (IU) |
| N.S | 60.54±5.21 | |
| Medicine of the present invention | 1.5 | 81.18±4.73 * |
| Medicine of the present invention | 2.0 | 82.27±5.48 * |
| Medicine of the present invention | 4.0 | 84.23±4.15 * |
Annotate: compare * P＜0.01 with matched group
The result shows: this product can promote the motion of mouse small intestine, with the normal saline matched group significant difference P＜0.01 is arranged relatively,
3, the influence of Dichlorodiphenyl Acetate type gastric ulcer
40 of rats are divided into 4 groups at random, the same one group of method and dosage, fasting is 24 hours then, can't help water, under etherization, cut abdomen open by the sterile working and draw stomach, behind 2 dipping glacial acetic acid of the Lu scraps of paper with diameter 5mm, be posted on the 30Second of serous coat place, greater gastric curvature both sides, remove the Lu scraps of paper rapidly, and dry with rayon balls, the reduction body of stomach is sewed up stomach wall.Postoperative begins feed and gastric infusion next day, grouping, dosage, through medicine with experiment 1, fasting is 24 hours after the last administration, dislocation is put to death, cut open the belly immediately and get stomach and use 1% formalin fixed, write down gastric pathological changes situation, with ulcer length summation mm as ulcer index, carry out statistical procedures, the results are shown in Table:
The influence of Dichlorodiphenyl Acetate type gastric ulcer
| Group | Dosage (g/kg) | Stomach egg (IU) |
| N.S | 140±2.83 | |
| Medicine of the present invention | 2.0 | 5.6±0.12 *** |
| Medicine of the present invention | 3.0 | 2.9±0.10 *** |
| Medicine of the present invention | 4.0 | 3.2±0.11 *** |
Annotate: compare * * * P＜0.001 with matched group
The result shows: medicine of the present invention has the obvious suppression effect to rat acetic acid type gastric ulcer, with the normal saline matched group significant differences P＜0.001 is arranged relatively.
Experimental example 5 treatment cardiopalmus effects
To the pant influence of time of the disconnected cranium of mice: get 80 of body weight 18-22g mices, be divided into 4 groups at random, 20 every group, each 10 of male and female.Animal fasting 16h before the experiment.Each treated animal gives high, medium and low dose of medicine of the present invention respectively, blank group equivalent normal saline.The disconnected cranium of 1h mice cervical region behind the medicine is opened one's mouth the time of panting with stopwatch record mice simultaneously.The results are shown in following table
XINNAOKANG JIAONANG is to the pant influence of time of the disconnected cranium of mice
Annotate: compare with the blank group,
* *P＜0.01
The result shows: medicine of the present invention can obviously prolong panting the time of mice.
Experimental example 6 treatment sexual impotence
1, to castration rat genitals's influence
Get from 60 of 1 month Wistar male rats of breast, body weight 90-110g, (0.6%, 7.5ml/kg) under the anesthesia, bilateral testes is extractd in the skin of scrotum sterilization at pentobarbital sodium.Postoperative muscle notes lining benzylpenicillin (20,000 units/kg) for three days on end.The castration operation was divided into 5 groups at random with 50 castrated rats after 3 days:
Castration model group distilled water is irritated stomach (1ml/100g).
The plain group of propanoic acid highland ball subcutaneous injection administration (0.2mg/ only).
The heavy dose of group of medicine of the present invention is mixed with 1ml/100g concentration with preceding (4g/kg) with distilled water and irritates stomach.
The dosage group is mixed with 1ml/100g concentration with preceding (2g/kg) with distilled water and irritates stomach in the medicine of the present invention.
((1g/kg) is mixed with 1ml/100g concentration with distilled water and irritates stomach medicine small dose group of the present invention with preceding.
More than 6 groups of equal administrations every day 1 time, continuous 20 days.In addition, establishing one group the same period in addition is the normal control group, and with 10 the not castrated rats raisings same period, distilled water (1ml/100g) is irritated stomach, observes.
After the administration the 21st day, with sacrifice of animal, win preputial glands, seminal fluid capsule, levator ani and prostate rapidly and weigh, calculate organ index, organize a t check.
Medicine of the present invention is to the influence of castrated rats weight of reproductive organs (x ± s)
| Group | Number of animals (n) | Preputial glands (mg) | Levator ani (mg) | Seminal fluid capsule (mg) | Prostate (mg) |
| The normal control group | 10 | 150.5±31.81** | 95.9±34.45** | 325.1± 89.76** | 424.1±60.23** |
| The castration model group | 10 | 60.9±9.55 | 30.1±5.92 | 14.6±1.96 | 79.8±12.25 |
| The androlin group | 10 | 128.9±12.71** | 116.9± 33.12** | 332.1± 90.23** | 492.2±113.55** |
| The heavy dose of group of medicine of the present invention | 10 | 85.0±14.95** | 58.1±10.92** | 25.2±2.84** | 81.3±8.23 |
| Dosage group in the medicine of the present invention | 10 | 81.0±15.93** | 47.9±8.09** | 21.8±4.96** | 79.5±15.64 |
| Medicine small dose group of the present invention | 10 | 78.9±14.45** | 41.0±7.26** | 19.8±4.05** | 75.7±20.56 |
Annotate: compare * * p＜0.01 with the castration model group
The anabolic hormone active function of medicine of the present invention
| Group | Number of animals (n) | Levator ani/prostate |
| The normal control group | 10 | 0.25±0.11 |
| The castration model group | 10 | 0.39±0.11 ** |
| The androlin group | 10 | 0.22±0.13 |
| The heavy dose of group of medicine of the present invention | 10 | 0.80±0.10 ** |
| Dosage group in the medicine of the present invention | 10 | 0.67±0.20 ** |
| Medicine small dose group of the present invention | 10 | 0.60±0.22 ** |
Annotate: compare * * p＜0.01 with the normal control group
2, to the influence of castration rat penile erectile function
Get from 60 of 1 month Wistar male rats of breast, body weight 90-110g, (0.6%, 7.5ml/kg) under the anesthesia, bilateral highland ball is extractd in the skin of scrotum sterilization at pentobarbital sodium.Postoperative muscle notes lining benzylpenicillin (20,000 units/kg) for three days on end.The castration operation was divided into 5 groups at random with 50 castrated rats after 3 days:
Castration model group distilled water is irritated stomach (1ml/100g),
The plain group of propanoic acid highland ball subcutaneous injection administration (0.2mg/ only).
The heavy dose of group of medicine of the present invention is mixed with 1ml/100g concentration with preceding (4g/kg) with distilled water and irritates stomach.
The dosage group is mixed with 1ml/100g concentration with preceding (2g/kg) with distilled water and irritates stomach in the medicine of the present invention.
((1g/kg) is mixed with 1ml/100g concentration with distilled water and irritates stomach medicine small dose group of the present invention with preceding.
More than 6 groups of equal administrations every day 1 time, continuous 20 days.In addition, establishing one group the same period in addition is the normal control group, and with 10 the not castrated rats raisings same period, distilled water (1ml/100g) is irritated stomach, observes.
After administration the 21st day, the stimulating electrode of electricity irritation thrombosis instrument is positioned over rat penis position, give electricity irritation (current intensity is 4mA).Record begins to erect the time (erecing incubation period) to penis from stimulation, and the result organizes a t check.
To the influence of castration rat penile erectile function (x ± s)
| Group | Number of animals (n) | Erection incubation period (s) |
| The normal control group | 10 | 14.53±3.10 ** |
| The castration model group | 10 | 65.01±15.91 |
| The androlin group | 10 | 21.03±6.41 ** |
| The heavy dose of group of medicine of the present invention | 10 | 26.51±6.52 ** |
| Dosage group in the medicine of the present invention | 10 | 28.23±6.94 ** |
| Medicine small dose group of the present invention | 10 | 32.00±8.99 ** |
Annotate: compare * * P＜0.01 with the castration model group
The result finds out that medicine of the present invention can improve the irritability of castrated rats penis to outside stimulus, and under local electricity irritation, each treated animal erection time is significantly shorter than the castration model group, and significant difference is arranged.
3, to the influence of male white mouse mating ability
50 of the male Kunming of animal kind white mice, body weight 20g-22g is divided into 5 groups at random, 10 every group.
Normal control group distilled water is irritated stomach (20ml/kg)
The plain group of propanoic acid highland ball subcutaneous injection administration (0.025mg/ only).
The heavy dose of group of medicine of the present invention is mixed with 2ml/100g concentration with preceding (5g/kg) with distilled water and irritates stomach.
The dosage group is mixed with 2ml/100g concentration with preceding (2.5g/kg) with distilled water and irritates stomach in the medicine of the present invention.
((1.25g/kg) is mixed with 2ml/100g concentration with distilled water and irritates stomach medicine small dose group of the present invention with preceding.
More than each group, irritate stomach every day 1 time on (propanoic acid guilt ball plain group for subcutaneous injection administration), continuous 10 days, every male Mus of beginning in the 5th day was fed with cage with 5 female Mus, injected estradiol benzoate (200ug/kg) down for every female Corium Mus on the 6th day.Female Mus vaginal orifice is respectively organized in the every morning inspection or intravaginal has or not white thing to occur with beginning next day behind the cage, and adularescent thing person takes out it for cloudy bolt occurring from cage; Calculate cloudy bolt occurrence rate.Carry out x
2Relatively, the results are shown in following table between four fold table check group
Medicine of the present invention is to the influence of male mice mating ability
| Group | Number of animals (n) | The Mus number (n) that cloudy bolt occurs | Cloudy bolt occurrence rate (%) |
| The normal control group | 50 | 11 | 22 |
| The androlin group | 50 | 30 | 60 ** |
| The heavy dose of group of medicine of the present invention | 50 | 36 | 75.2 ** |
| Dosage group in the medicine of the present invention | 50 | 30 | 60 ** |
| Medicine small dose group of the present invention | 50 | 25 | 50 ** |
Annotate: compare * * p＜0.01 with the normal control group
The result as seen, large, medium and small dosage group of medicine of the present invention and positive controls (the plain group of propanoic acid highland ball and strengthen the mice mating ability more significantly with the normal control group.
Find that by above experiment medicine of the present invention can improve the irritability of castration male rat penis to outside stimulus, shorten its erection incubation period and strengthen the male mice mating ability, point out this medicine can strengthen penile erectile function and raising sexual potency.Also observe in the experiment, medicine of the present invention has its particularity to the attached gonadal influence of animal, its weight in wet base is increased, but the prostate weight in wet base is increased, show that this medicine not only has the effect of class androgen sample, and the anabolic hormone active function arranged, prompting person in middle and old age impotence patient take this medicine that treatment can not cause or
Impel prostatic hyperplasia.Medicine of the present invention all exists certain dose-effect relationship to the influence of neuter weight of reproductive organs, penile erectile function and intact animal's sexual function simultaneously, and along with the increasing of dosage, effect also strengthens thereupon.
Experimental example 7 is differentiated screening experiment
1, microscopical identification
A few flavor valuable medicinals such as Radix Ginseng Rubra, Cornu Cervi Pantotrichum and Cordyceps are used as medicine for directly pulverizing in the pharmaceutical preparation of the present invention, have so not only reduced the loss of medicine, can also effectively guarantee curative effect of medication, so added microscopical identification:
Concrete discrimination method: get pharmaceutical preparation of the present invention, porphyrize is put microscopically and is observed; Calcium oxalate cluster crystal diameter 20-68 μ m, the sharp point of corner angle.Unossified osseous tissue light gray or closely colourless, edge and surface are all irregular, have irregular block-like protrusions thing, the linear marking that mays be seen indistinctly therebetween, mycelia is elongated, and is colourless, not branch or branch, intensive intersection is agglomerating or fragment into joint.
Micro-characteristics of Radix Ginseng Rubra wherein: calcium oxalate cluster crystal diameter 20～68 μ m, the sharp point of corner angle.
The micro-characteristics of Cornu Cervi Pantotrichum; Unossified osseous tissue light gray or closely colourless, edge and surface are all irregular, have irregular block-like protrusions thing, and linear marking therebetween mays be seen indistinctly.
The micro-characteristics of Cordyceps: mycelia is elongated, and is colourless, not branch or branch, and intensive intersection is agglomerating or fragment into joint.
We get the different preparations of medicine of the present invention, carry out microscopical identification respectively, prove that this discrimination method is stable, are applicable to that the thin layer of all preparations under this its preparation process is differentiated.
2, the thin layer discrimination method of Radix Ginseng, the Radix Astragali:
1) preparation of need testing solution
The preparation method of need testing solution determines that according to the concrete active ingredient of discriminating medicine the discriminating to Radix Ginseng Rubra, the Radix Astragali in the medicine of the present invention mainly is the wherein discriminating of ginsenoside Rb, Re, Rg and astragaloside.Adopt orthogonal test to determine effective separating and extracting process.
We are horizontal factor with solvent species, extraction time, the extraction time of choosing, and get pharmaceutical preparation of the present invention, according to factor level table arrangement test, with ginsenoside Rb
1Content for investigating index, concrete outcome is as follows:
Preferred factor level table
Table 4. factor screening orthogonal experiment data table
Analysis of variance table
Analyze as can be seen from table R value, influence factor's primary and secondary is A＞B＞C, and the intuitive analysis optimum extraction process is A
1B
2C
2, from analysis of variance table as can be seen factor A have significance, and factor B, C do not have significance influence to the result, from saving time consideration, so choose A
1B
2C
1Be the optimum extraction scheme.Get pharmaceutical preparation content of the present invention, about 1.5g accurate claims surely, put in the tool plug conical flask, and the accurate methanol 50ml that adds, close plug claims to decide weight, puts in the water-bath heating and refluxing extraction 1.5 hours, gets final product.
2) after extraction is finished, reduce to minimum in order to make to disturb, differentiate the character of composition according to each, with the methanolic extract chloroform, n-butyl alcohol and ammonia solution have carried out further separating and extracting, and concrete grammar is as follows: get methanolic extract 25ml, put in the evaporating dish, evaporate to dryness, residue add water 25ml separates solution, and moves in the separatory funnel, adding the chloroform jolting extracts 2 times, each 15ml discards chloroform solution, and water liquid extracts 4 times with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, add ammonia solution 30ml washing, discard cleaning mixture, n-butyl alcohol liquid places evaporate to dryness in the water-bath, gets final product.
By measuring ginsenoside Rb in the last gained need testing solution
1Content, this separation method is verified that the result is as follows:
As can be seen from the above table, ginsenoside Rb before and after need testing solution separates with this method
1Content do not change, illustrate that this separation method is used for the effective ingredient good separating effect, be fit to test requirements document.
2) the middle developing solvent proportioning of above-mentioned discrimination method (2) is preferred: draw the need testing solution 10 μ l of preparation as stated above, the reference substance solution 5 μ l of ginsenoside Rb, Re, Rg and astragaloside, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water proportioning is that lower floor's solution that place below 10 ℃ (7: 7: 2), (10: 7: 2), (13: 7: 2), (15: 7: 2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, puts respectively under daylight and the ultra-violet lamp (365nm) and inspect.Observe the unfolded effect of test sample on each lamellae, the results are shown in following table:
| The developing solvent proportioning | 7∶7∶2 | 10∶7∶2 | 13∶7∶2 | 15∶5∶2 |
| Launch effect | Relatively poor | Difference | Good | Difference |
Developing solvent proportioning as can be seen from the above table is 13: 7: 2 o'clock, and it is best that need testing solution launches effect, and appearance hangover, speckle separate phenomenons such as bad.
3) the middle sample solution point sample amount of above-mentioned discrimination method (2) is preferred, get need testing solution 1 μ l, 5 μ l, 8 μ l, 10 μ l, reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, and lower floor's solution of placing below 10 ℃ with chloroform-methanol-water (13: 7: 2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear that hot blast blows to the speckle colour developing, puts respectively under daylight and the ultra-violet lamp (365nm) and inspect., the effect of observing test sample principal spot colour developing on the lamellae the results are shown in following table:
| The point sample amount | 1μl | 5μl | 8μl | 10μl |
| Color developing effect | Test sample is at corresponding reference substance position immaculate | Test sample is very shallow in corresponding reference substance position spot colors | Test sample is shallow in corresponding reference substance position spot colors | Test sample is good at corresponding reference substance position speckle color developing effect |
Test sample point sample amount is when 10 μ l as can be seen from the above table, and color developing effect is good on lamellae, is fit to test requirements document.
4) negative control test
Get the negative sample of scarce Radix Ginseng Rubra, the Radix Astragali, according to need testing solution preparation method in the above-mentioned discrimination method (2)
The preparation negative control solution launches the back and corresponding speckle do not occur on the reference substance solution correspondence position, illustrates that selected identification experiment specificity is strong.
3, the thin layer discrimination method of Herba Epimedii:
1) preparation of need testing solution: the preparation method of the test sample in the discrimination method 2, can contained active ingredient icariin in the pharmaceutical preparation more of the present invention be separated, carry out thin layer and differentiate, just no longer it has been discussed here.
2) selection of developing solvent:
Respectively with chloroform-methanol-water (13: 7: 2) and ethyl acetate-butanone-formic acid-water (10: 1: 1: 1) be developing solvent, draw and differentiate need testing solution and each 5 μ l of icariin reference substance solution in 2, put respectively on same silica gel g thin-layer plate, launch, take out, dry, spray, is put under the ultra-violet lamp (365nm) and is inspected 105C heating several minutes with the aluminum chloride test solution, under the more different developing solvents, the unfolded effect of test sample.
The results are shown in following table:
| Developing solvent | Chloroform-methanol-water (13: 7: 2) | Ethyl acetate-butanone-formic acid-water (10: 1: 1: 1) |
| Launch effect | It is all bad that reference substance and test sample launch effect, inferior separating effect. | Reference substance and test sample launch effective, and the speckle colour developing is clear, and test sample principal spot free from admixture disturbs. |
As can be seen from the above table, select ethyl acetate-butanone-formic acid-water (10: 1: 1: 1) be developing solvent, launches effective, the free from admixture interference, it is clear to develop the color.
3) sample solution point sample amount preferred in the above-mentioned discrimination method 3 got need testing solution 1 μ l, 2 μ l, 3 μ l, 5 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, (10: 1: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, spray, is put under the ultra-violet lamp (365nm) and is inspected 105C heating several minutes with the aluminum chloride test solution, observe the effect of test sample principal spot colour developing on the lamellae, the results are shown in following table:
| The point sample amount | 1μl | 2μl | 3μl | 5μl |
| Color developing effect | Test sample is at corresponding reference substance position immaculate | Test sample is very shallow in corresponding reference substance position spot colors | Test sample is shallow in corresponding reference substance position spot colors | Test sample is good at corresponding reference substance position speckle color developing effect |
Test sample point sample amount is when 5 μ l as can be seen from the above table, and color developing effect is good on lamellae, is fit to test requirements document.
4) negative control test
Get the negative sample that lacks Herba Epimedii, prepare negative control solution, launch the back and corresponding speckle on the reference substance solution correspondence position, do not occur, illustrate selected according to need testing solution preparation method in the above-mentioned discrimination method 2
The identification experiment specificity of getting is strong.
4, the thin layer discrimination method of Fructus Lycii:
1) selection of different need testing solution preparation methoies:
Method one: get pharmaceutical preparation 5g of the present invention, add methanol 50m; , put in the water-bath reflux 1 hour, take out, put coldly, filter, filtrate evaporate to dryness, residue add water 20ml makes solution, extracts 2 times with the chloroform jolting, each 15ml, combined chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.
Method two: get pharmaceutical preparation 1g of the present invention, add water 70ml, heated and boiled 15 minutes is put coldly, filters, and filtrate is extracted with ethyl acetate 15ml jolting, and extracting solution is concentrated into about 2ml, as need testing solution.
Drawing each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with chloroform one ethyl acetate, one methanol (4: 2: 0.3), launches, and takes out, and dries, and puts under the ultra-violet lamp (365nm) and inspects.Compare the color developing effect of the need testing solution of two kinds of extracting method preparations, the results are shown in following table:
| Extracting method | Method one | Method two |
| Color developing effect | Color developing effect is good | It is unintelligible to develop the color, and interference is arranged. |
As can be seen from the above table, employing method one need testing solution color developing effect good, the Pass Test requirement.
2) developing solvent proportioning preferred in the above-mentioned discrimination method 4: draw the need testing solution 5 μ l of a preparation as stated above, the control medicinal material solution 5 μ l of Fructus Lycii, put respectively on same silica gel g thin-layer plate, with chloroform one ethyl acetate one methanol proportioning is that (2: 2: 0.3) (3: 2: 0.3) (4: 2: 0.3) (4: 3: 0.3) are developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.Observe the unfolded effect of test sample on each lamellae, the results are shown in following table:
| The developing solvent proportioning | 2∶2∶0.3 | 3∶2∶0.3 | 4∶2∶0.3 | 4∶3∶0.3 |
| Launch effect | Relatively poor | Difference | Good | Difference |
Developing solvent proportioning as can be seen from the above table is 4: 2: 0.3 o'clock, and it is best that need testing solution launches effect, and appearance hangover, speckle separate phenomenons such as bad.
3) sample solution point sample amount preferred in the above-mentioned discrimination method 4, get need testing solution 1 μ l, 2 μ l, 3 μ l, 5 μ l, control medicinal material solution 5 μ l put respectively on same silica gel g thin-layer plate, are that (2: 2: 0.3) (3: 2: 0.3) (4: 2: 0.3) (4: 3: 0.3) are developing solvent with chloroform one ethyl acetate one methanol proportioning, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, observe the effect of test sample principal spot colour developing on the lamellae, the results are shown in following table:
| The point sample amount | 1μl | 2μl | 3μl | 5μl |
| Color developing effect | Test sample is at corresponding reference substance position immaculate | Test sample is very shallow in corresponding reference substance position spot colors | Test sample is shallow in corresponding reference substance position spot colors | Test sample is good at corresponding reference substance position speckle color developing effect |
Test sample point sample amount is when 5 μ l as can be seen from the above table, and color developing effect is good on lamellae, is fit to test requirements document.
4) negative control test
Get the negative sample that lacks Fructus Lycii, prepare negative control solution, launch the back and on control medicinal material solution correspondence position, corresponding speckle do not occur, illustrate that selected identification experiment specificity is strong according to above-mentioned need testing solution preparation method.
Experimental example 8 assay screening experiment
Adopt high-efficient liquid phase technique to measure ginsenoside Rb in the pharmaceutical preparation of the present invention
1Content, make drug quality detection means of the present invention more complete.The preparation need testing solution still adopts the preparation method preparation of need testing solution in the discrimination method 2.
1, the selection of mobile phase: be mobile phase with acetonitrile-water (29: 71) and acetonitrile-0.05% phosphoric acid solution (99: 400) respectively, carry out the test sample assay at molten night, by comparing among the general figure of high-efficient liquid phase color the separating effect at each peak, determine preferred mobile phase, the result is as follows:
| Mobile phase reagent is selected | Acetonitrile: water (29: 71) | Methanol-0.05mol/L phosphoric acid solution (99: 400) |
| Each peak separating effect in the chromatogram | With other peak good separating effect, noiseless. | With other peak inferior separating effect, disturb big. |
As can be seen from the above table, acetonitrile: water (29: 71) is each peak good separating effect of mobile phase.
2, proportion of mobile phase is preferred:
Respectively with acetonitrile: the water proportioning is that (14: 80), (15: 85), (29: 71), (16: 85) are mobile phase, carry out the test sample assay at molten night, by comparing among the general figure of high-efficient liquid phase color the separating effect at each peak, determine preferred mobile phase, the result is as follows:
| Proportion of mobile phase | 15∶60 | 29∶71 | 40∶80 | 46∶90 |
| Each peak separating effect in the chromatogram | Interference is arranged | Good separating effect | Interference is arranged | Interference is arranged |
As can be seen from the above table, proportion of mobile phase is selected 29: 71 for well.
3, the methodological study of content assaying method
To the detection method of content that medicine of the present invention adopted, carried out related side's science of law from aspects such as linear relationship, stability, precision, repeatability, the response rate and investigated, concrete outcome is as follows:
(1) linear relationship is investigated accurate reference substance solution (0.6952mg/ml) 0.5,1,2,3, the 4ml of drawing, put respectively in the 5ml measuring bottle, respectively add methanol and be diluted to scale, shake up the accurate respectively 20 μ l of absorption, inject chromatograph of liquid, measure peak area, the results are shown in following table, and the drawing standard curve, show ginsenoside Rb
1Linear between 1.3904ug-11.1232ug, its regression equation is:
Area＝100044.64*Amt+7466.13(r＝0.9999)
(2) the same need testing solution 10 μ l of the accurate absorption of stability test respectively at preparing the back 0,2,4,8,24 hour, measure in accordance with the law, and the result shows that it is basicly stable in 24 hours, the results are shown in following table
(3) the accurate need testing solution 10 μ l that draw of precision test repeat sample introduction 5 times, try to achieve relative standard deviation＜2%, the results are shown in following table
(4) 5 parts in same sample is got in the repeatability test, measures respectively, tries to achieve relative standard deviation＜2%, the results are shown in following table
(5) the recovery test precision takes by weighing the accurate respectively again ginsenoside Rb1 of the adding reference substance solution 10ml of same batch sample 1.0g of known content, the accurate methanol 40ml that adds, preparation method operation by above need testing solution, measure its content, and calculate its response rate, measurement result sees the following form:
From above result of the test as can be seen, its linear relationship of the content assaying method that medicine of the present invention adopted, stability, precision, repeatability etc. are all good, can effectively control drug quality of the present invention.
Following embodiment all can realize the described effect of above-mentioned experimental example
Embodiment 1
Radix Ginseng Rubra 108g Radix Astragali 108g Cornu Cervi Pantotrichum 36g
Radix Polygoni Multiflori Preparata 60g Fructus Lycii 36g Cordyceps 20g
Herba Epimedii (processing) 72g Rhizoma Polygonati 36g Radix Salviae Miltiorrhizae 60g
Bee pollen 24g Radix Glycyrrhizae 28g Lac regis apis (lyophilized powder) 12g
Except that bee pollen, Lac regis apis lyophilized powder, Radix Ginseng Rubra, Cornu Cervi Pantotrichum, Cordyceps are ground into fine powder, seven flavors such as all the other Radixs Astragali, add 10 times of water gagings and decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into the clear paste that relative density is 1.20-1.25 (60 ℃), and drying under reduced pressure becomes dry extract, is ground into fine powder, sieve with fine powder mixings such as above-mentioned bee pollen, Lac regis apis lyophilized powder and Radix Ginseng Rubra, incapsulate, make 1000, promptly.
Differentiate:
(1) gets this product, put microscopically and observe; Calcium oxalate cluster crystal diameter 20-68 μ m, the sharp point of corner angle.Unossified osseous tissue light gray or closely colourless, edge and surface are all irregular, have irregular block-like protrusions thing, the linear marking that mays be seen indistinctly therebetween, mycelia is elongated, and is colourless, not branch or branch, intensive intersection is agglomerating or fragment into joint.
(2) get ginsenoside Rb, Re, Rg and astragaloside reference substance, add methanol and make the mixed solution that every 1ml contains 1mg, in contrast product solution.The need testing solution preparation: get the content under this product content uniformity item, mixing is got about 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, puts in the water-bath heating and refluxing extraction 1.5 hours, take out, put coldly, claim to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured filtrate 25ml, puts in the evaporating dish evaporate to dryness, residue adds water 25ml separates solution, and move in the separatory funnel, add the chloroform jolting and extract 2 times, each 15ml, discard chloroform solution, water liquid extracts 4 times with water saturated n-butyl alcohol jolting, and each 20ml merges n-butyl alcohol liquid, add ammonia solution 30ml washing, discard cleaning mixture, n-butyl alcohol liquid places evaporate to dryness in the water-bath, and residue adds quantity of methyl alcohol makes dissolving.And quantitatively be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly.
Test according to thin layer chromatography, draw need testing solution 10 μ l, above-mentioned reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water (13: 7: 2) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing, puts respectively under daylight and the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle or the fluorescence speckle of same color.
(3) get the icariin reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.
The preparation of need testing solution is got the content under this product content uniformity item, mixing, get about 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, put in the water-bath heating and refluxing extraction 1.5 hours, and took out, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured filtrate 25ml, puts in the evaporating dish, evaporate to dryness, residue add water 25ml separates solution, and moves in the separatory funnel, adding the chloroform jolting extracts 2 times, each 15ml discards chloroform solution, and water liquid extracts 4 times with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, add ammonia solution 30ml washing, discard cleaning mixture, n-butyl alcohol liquid places evaporate to dryness in the water-bath, and residue adds quantity of methyl alcohol makes dissolving.And quantitatively be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly.Test according to thin layer chromatography, draw each 5 μ l of need testing solution and above-mentioned reference substance solution, put respectively on same silica gel g thin-layer plate, (10: 1: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, spray, is put under the ultra-violet lamp (365nm) and is inspected 105C heating several minutes with the aluminum chloride test solution.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 content 5g, add methanol 50m; , put in the water-bath reflux 1 hour, take out, put coldly, filter, filtrate evaporate to dryness, residue add water 20ml makes solution, extracts 2 times with the chloroform jolting, each 15ml, combined chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Fructus Lycii control medicinal material 1g, decoct with water 15 minutes, filter, filtrate is shone medical material solution in pairs with legal system, test according to thin layer chromatography, drawing each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with chloroform one ethyl acetate, one methanol (4: 2: 0.3), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
Assay:
According to high effective liquid chromatography for measuring, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-water (29: 71) is a mobile phase; The detection wavelength is 203nm; Column temperature 40C.Number of theoretical plate is by ginsenoside Rb
1The peak calculates should be not less than 2500.
The preparation of reference substance solution, precision take by weighing ginsenoside Rb
1Reference substance 7.5mg puts in the 25ml measuring bottle, adds methanol and makes solution, and be diluted to scale, shakes up, and promptly gets (to contain ginsenoside Rb among every 1ml
10.3mg).
The preparation of need testing solution is got the content under this product content uniformity item, mixing, get about 1.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, put in the water-bath heating and refluxing extraction 1.5 hours, and took out, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured filtrate 25ml, puts in the evaporating dish, evaporate to dryness, residue add water 25ml separates solution, and moves in the separatory funnel, adding the chloroform jolting extracts 2 times, each 15ml discards chloroform solution, and water liquid extracts 4 times with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, add ammonia solution 30ml washing, discard cleaning mixture, n-butyl alcohol liquid places evaporate to dryness in the water-bath, and residue adds quantity of methyl alcohol makes dissolving.And quantitatively be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly.
Algoscopy, accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, measure, promptly.Every of this product contains ginsenoside Rb
1(C
54H
92O
23), must not be less than 0.40mg.
Function cures mainly: QI invigorating replenishing essence, reinforcing the kidney and supporting YANG.Be applicable to deficiency of vital energy damage of essence, the spiritlessness and weakness that insufficiency of kidney-YANG causes, insomnia is dizzy,, soreness of the waist and knees, aversion to cold and cold limbs, inappetence, diseases such as shortness of breath and palpitation.
Usage and dosage: oral, one time 4,3 times on the one.
Attention: should not take during the deficiency of YIN, fever, the insufficiency of kidney-YANG.
Specification: every dress 0.3g
Embodiment 2 capsules
Radix Ginseng 80g Placenta Hominis 100g
Radix Polygoni Multiflori Preparata 90g Fructus Lycii 50g Cordyceps 20g
Herba Epimedii (processing) 90g Rhizoma Polygonati 60g Radix Notoginseng 30g
Bee pollen 50g Radix Glycyrrhizae 40g Lac regis apis (lyophilized powder) 8g;
More than 12 the flavor, except that bee pollen, Lac regis apis lyophilized powder, Radix Ginseng Rubra, Cornu Cervi Pantotrichum, Cordyceps are ground into fine powder, seven flavors such as all the other Radixs Astragali add 10 times of water gagings and decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into the clear paste that relative density is 1.20-1.25 (60 ℃), and drying under reduced pressure becomes dry extract, be ground into fine powder, sieve with fine powder mixings such as above-mentioned bee pollen, Lac regis apis lyophilized powder and Radix Ginseng Rubra, incapsulate, promptly.
Embodiment 3 tablets
Radix Ginseng Rubra 75g Radix Astragali 130g Cornu Cervi Pantotrichum 55g
Radix Polygoni Multiflori Preparata 75g Fructus Lycii 60g Cordyceps 13g
Herba Epimedii (processing) 95g Rhizoma Polygonati 60g Radix Salviae Miltiorrhizae 90g
Bee pollen 60g Radix Glycyrrhizae 12g Lac regis apis (lyophilized powder) 8g
More than 12 the flavor, except that bee pollen, Lac regis apis lyophilized powder, Radix Ginseng Rubra, Cornu Cervi Pantotrichum, Cordyceps are ground into fine powder, seven flavors such as all the other Radixs Astragali add 10 times of water gagings and decoct secondary, each 2 hours, collecting decoction filters, and filtrate is concentrated into the clear paste that relative density is 1.20-1.25 (60 ℃), or add appropriate amount of auxiliary materials, with fine powder mixings such as above-mentioned bee pollen, Lac regis apis lyophilized powder and Radix Ginseng Rubra, drying, make granule, tabletting, or sugar coating or film-coat, promptly.
Embodiment 4 drop pills
Radix Ginseng Rubra 85g Radix Astragali 160g Cornu Cervi Pantotrichum 58g
Radix Polygoni Multiflori Preparata 85g Fructus Lycii 65g Cordyceps 14g
Herba Epimedii (processing) 100g Rhizoma Polygonati 60g Radix Salviae Miltiorrhizae 85g
Bee pollen 65g Radix Glycyrrhizae 15g Lac regis apis (lyophilized powder) 7g
More than 12 the flavor, except that bee pollen, Lac regis apis lyophilized powder, Radix Ginseng Rubra, Cornu Cervi Pantotrichum, Cordyceps are ground into fine powder, seven flavors such as all the other Radixs Astragali add 10 times of water gagings and decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into the thick paste that relative density is 1.20-1.25, after mixing thoroughly with fine powders such as bee pollen, Lac regis apis lyophilized powder and Radix Ginseng Rubra, add in the fused Polyethylene Glycol substrate, splash in the condensed fluid, drop is most, promptly.
Embodiment 5 granules
Radix Ginseng Rubra 75g Radix Astragali 130g Cornu Cervi Pantotrichum 55g
Radix Polygoni Multiflori Preparata 75g Fructus Lycii 60g Cordyceps 13g
Herba Epimedii (processing) 95g Rhizoma Polygonati 60g Radix Salviae Miltiorrhizae 90g
Bee pollen 60g Radix Glycyrrhizae 12g Lac regis apis (lyophilized powder) 8g
More than 12 the flavor, except that bee pollen, Lac regis apis lyophilized powder, Radix Ginseng Rubra, Cornu Cervi Pantotrichum, Cordyceps are ground into fine powder, seven flavors such as all the other Radixs Astragali, add 10 times of water gagings and decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into the clear paste that relative density is 1.20-1.25 (60 ℃), adds an amount of sucrose and dextrin, drying, granulate, promptly.
Embodiment 6 effervescent tablets
Radix Ginseng Rubra 85g Radix Astragali 160g Cornu Cervi Pantotrichum 58g
Radix Polygoni Multiflori Preparata 85g Fructus Lycii 65g Cordyceps 14g
Herba Epimedii (processing) 100g Rhizoma Polygonati 60g Radix Salviae Miltiorrhizae 85g
Bee pollen 65g Radix Glycyrrhizae 15g Lac regis apis (lyophilized powder) 7g
More than 12 the flavor, except that bee pollen, Lac regis apis lyophilized powder, Radix Ginseng Rubra, Cornu Cervi Pantotrichum, Cordyceps are ground into fine powder, seven flavors such as all the other Radixs Astragali add 10 times of water gagings and decoct secondary, each 2 hours, collecting decoction filters, and filtrate is concentrated into the clear paste that relative density is 1.20-1.25 (60 ℃), drying under reduced pressure becomes dry extract, be ground into fine powder, with fine powder mixings such as above-mentioned bee pollen, Lac regis apis lyophilized powder and Radix Ginseng Rubra, after the Polyethylene Glycol fusion, add sodium bicarbonate. stir. cooling is pulverized, and crosses 80 mesh sieves.In addition citric acid, sweetener are crossed 80 mesh sieves,, granulate with medicated powder, Polyethylene Glycol wrappage fine powder mixing, drying,, compressed tablet, promptly.
Embodiment 7 granules
Radix Ginseng Rubra 80g Radix Astragali 150g Cornu Cervi Pantotrichum 55g
Radix Polygoni Multiflori Preparata 85g Fructus Lycii 65g Cordyceps 14g
Herba Epimedii (processing) 95g Rhizoma Polygonati 60g Radix Salviae Miltiorrhizae 85g
Bee pollen 65g Radix Glycyrrhizae 15g Lac regis apis (lyophilized powder) 7g
More than 12 the flavor, except that bee pollen, Lac regis apis lyophilized powder, Radix Ginseng Rubra, Cornu Cervi Pantotrichum, Cordyceps are ground into fine powder, seven flavors such as all the other Radixs Astragali, add 10 times of water gagings and decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into the clear paste that relative density is 1.20-1.25 (60 ℃), adds Sugarless type adjuvants such as an amount of steviosin and dextrin, drying, granulate, promptly.
Embodiment 8 capsules
Radix Ginseng Rubra 73g Radix Astragali 140g Cornu Cervi Pantotrichum 58g
Radix Polygoni Multiflori Preparata 75g Fructus Lycii 60g Cordyceps 13g
Herba Epimedii (processing) 75g Rhizoma Polygonati 60g Radix Salviae Miltiorrhizae 98g
Bee pollen 50g Radix Glycyrrhizae 15g Lac regis apis (lyophilized powder) 8g
More than 12 the flavor, except that bee pollen, Lac regis apis lyophilized powder, Radix Ginseng Rubra, Cornu Cervi Pantotrichum, Cordyceps are ground into fine powder, seven flavors such as all the other Radixs Astragali add 10 times of water gagings and decoct secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into the clear paste that relative density is 1.20-1.25 (60 ℃), and drying under reduced pressure becomes dry extract, be ground into fine powder, sieve with fine powder mixings such as above-mentioned bee pollen, Lac regis apis lyophilized powder and Radix Ginseng Rubra, incapsulate, promptly.
Claims (2)
1. pharmaceutical composition for the treatment of insufficiency of kidney-YANG is characterized in that the crude drug of this pharmaceutical composition consists of:
The Radix Ginseng Rubra 75 weight portion Radixs Astragali 130 weight portion Cornu Cervi Pantotrichums 55 weight portions
Radix Polygoni Multiflori Preparata 75 weight portion Fructus Lycii 60 weight portion Cordyceps 13 weight portions
Herba Epimedii Preparata 95 weight portion Rhizoma Polygonatis 60 weight portion Radix Salviae Miltiorrhizaes 90 weight portions
Bee pollen 60 weight portion Radix Glycyrrhizaes 12 weight portion Lac regis apis lyophilized powders 8 weight portions.
2. pharmaceutical composition for the treatment of insufficiency of kidney-YANG is characterized in that the crude drug of this pharmaceutical composition consists of:
The Radix Ginseng Rubra 85 weight portion Radixs Astragali 160 weight portion Cornu Cervi Pantotrichums 58 weight portions
Radix Polygoni Multiflori Preparata 85 weight portion Fructus Lycii 65 weight portion Cordyceps 14 weight portions
Herba Epimedii Preparata 100 weight portion Rhizoma Polygonatis 60 weight portion Radix Salviae Miltiorrhizaes 85 weight portions
Bee pollen 65 weight portion Radix Glycyrrhizaes 15 weight portion Lac regis apis lyophilized powders 7 weight portions.
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| CN102613554B (en) * | 2012-03-29 | 2013-06-26 | 常熟市新港农产品产销有限公司 | Total nutrient multifunctional compound health care product |
| CN104165962B (en) * | 2013-05-15 | 2016-03-16 | 广州白云山中一药业有限公司 | The quality determining method of WEINAIAN sheet |
| CN105455082A (en) * | 2015-12-15 | 2016-04-06 | 北京农科亿健蜂产品研究院 | Preparation method of three-treasure tablet |
| CN108226331B (en) * | 2017-12-26 | 2020-09-22 | 贵州益佰制药股份有限公司 | Detection method of anti-tumor injection preparation |
| CN112697949B (en) * | 2020-12-09 | 2022-05-27 | 浙江金城阜通制药有限公司 | Thin-layer identification method for Baoyuan decoction, similar formula extract and preparation thereof |
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| CN1074831A (en) * | 1993-01-08 | 1993-08-04 | 赵绵生 | Antisenile medicine and preparation method thereof |
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Effective date of registration: 20070907 Address after: No. 8, Zhenxing Road, Zhongguancun science and Technology Park, Beijing, Changping District Applicant after: Beijing Asia-East Bio-Pharmaceutical Co., Ltd. Address before: Beijing City, Chaoyang District Wangjing silver international room 130#303 Applicant before: Ma Zhongan Co-applicant before: Zhao Kaijun |
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