CN1718206A

CN1718206A - Traditional Chinese medicine composition for treating deficiency disease and preparation method and quality standard thereof

Info

Publication number: CN1718206A
Application number: CN 200410069131
Authority: CN
Inventors: 吴少辉
Original assignee: Individual
Current assignee: Guangdong Shixin Medcine Co Ltd
Priority date: 2004-07-06
Filing date: 2004-07-06
Publication date: 2006-01-11
Anticipated expiration: 2024-07-06
Also published as: CN1323700C

Abstract

The invention discloses a traditional Chinese medicine composition for treating deficiency, and also discloses a preparation method and a quality standard of the composition. The traditional Chinese medicine composition mainly comprises semen cuscutae, herba epimedii, radix dipsaci, cynomorium songaricum, rhizoma cibotii, spina date seed, polygonum multiflorum, radix glycyrrhizae preparata, pericarpium citri reticulatae, deerhorn glue, prepared rehmannia root, tortoise-plastron glue, cherokee rose fruit, radix astragali preparata, Chinese yam and raspberry. The preparation method comprises pulverizing pericarpium Citri Tangerinae, rhizoma Dioscoreae, radix Glycyrrhizae Preparata, colla Cornus Cervi and colla Plastri Testudinis; decocting the rest materials, mixing decoctions, filtering, concentrating, refrigerating, standing, collecting supernatant, filtering, concentrating, drying, and pulverizing; mixing with the above four fine powders, grinding, adding adjuvants, and making into tablet or granule. The quality control method for preparing the composition into the medicament comprises identification and content measurement, wherein the identification method comprises a thin-layer chromatography test of polygonum multiflorum, liquorice and astragalus; the content determination method comprises HPLC method for determining herba Epimedii content. The invention is mainly used for treating consumptive disease, in particular to kidney-yang deficiency and kidney-qi deficiency.

Description

A kind of Chinese medicine composition for the treatment of deficiency of five viscera and preparation method thereof and quality standard

Invention field

The present invention relates to the preparation method and the quality standard of a kind of pharmaceutical composition and said composition, particularly a kind of Chinese medicine composition that is used for the treatment of deficiency of five viscera relates to the preparation method and the quality standard of said composition simultaneously.

Background technology

Deficiency of five viscera claims asthenia again.Due to multiple reason, with the internal organs loss, the negative and positive of qi and blood deficiency is the general name of the multiple chronic weak syndrome of main pathogenesis.

The deficiency of five viscera pathogenic factor is a lot of, and common reason has the natural endowment weakness, and body constitution is not strong; Bother excessively, undermine the five internal organs; Eating and drinking without temperance, impairing the spleen and stomach; Serious disease prolonged illness, lose in the conditioning etc.Deficient treatment is a basic principle with the tonification, and " element is asked a three body parts and nine pulse-taking sites opinion piece of writing " said: " deficiency syndrome should be treated by tonifying method." " element asks YIN YANG classification of natural phenomena a big opinion piece of writing " point out: " weakened configuration person, warming with drugs of thick nature; The insufficiency of essence person, tonifying with drugs of thick flavor ", in addition, the spleen being the foundation of acquired constitution is the source of water paddy, QI and bloodization life; The kidney being the origin of congenital constitution, and the residence nephroyin and nephroyang is this yuan of life, so invigorating spleen and kidney is significant in " deficiency of five viscera " treatment.

The present invention focuses on the Yuanyang with Semen Cuscutae, Herba Cynomorii, Herba Epimedii the kidney invigorating, with the Kidney-Yin of Radix Polygoni Multiflori, Colla cornus cervi, Colla Plastri Testudinis, Radix Rehmanniae Preparata the kidney invigorating; With Rhizoma Cibotii, the strong waist knee joint of Radix Dipsaci; Fructus Rosae Laevigatae, the astringent or styptic treatment for spontaneous sweating vital essence of Fructus Rubi; Radix Glycyrrhizae Preparata, Radix Astragali Preparata, the Rhizoma Dioscoreae tonification temper day after tomorrow; Assistant is with the Semen Ziziphi Spinosae mind tranquilizing and the heart calming.Full side is the merit of strengthening bone and muscle, replenishing QI and blood, kidney invigorating and YANG supporting altogether, for deficiency of five viscera show as physical weakness, soreness of the waist and knees, have a dizzy spell, deficiency of the kidney cold sperm, libido lower, urinate night more, forgetful insomniac, with more than obtain prompt effect.

Summary of the invention

One object of the present invention is to disclose a kind of Chinese medicine composition; Another object of the present invention is to disclose a kind of Chinese medicine composition and this Chinese medicine composition preparation method for the treatment of deficiency of five viscera; The 3rd purpose of the present invention is to disclose the method for quality control of this Chinese medicine composition.

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

The crude drug composition and the proportioning of pharmaceutical composition of the present invention are as follows:

Semen Cuscutae 120-140 weight portion Herba Epimedii 100-110 weight portion Radix Dipsaci 100-110 weight portion

Herba Cynomorii 120-140 weight portion Rhizoma Cibotii 150-170 weight portion Semen Ziziphi Spinosae 100-110 weight portion

Radix Polygoni Multiflori 150-170 weight portion Radix Glycyrrhizae Preparata 50-60 weight portion Pericarpium Citri Reticulatae 50-60 weight portion

Colla cornus cervi 20-30 weight portion Radix Rehmanniae Preparata 150-170 weight portion Colla Plastri Testudinis 30-40 weight portion

Fructus Rosae Laevigatae 120-140 weight portion Radix Astragali Preparata 100-110 weight portion Rhizoma Dioscoreae 100-110 weight portion

Fructus Rubi 210-230 weight portion

The above-mentioned raw materials optimum ratio is:

Semen Cuscutae (stir-fry) 128 weight portion Herba Epimedii (steaming) 106 weight portion Radix Dipsacis (steaming) 106 weight portions

Herba Cynomorii (steaming) 128 weight portion Rhizoma Cibotii (steaming) 160 weight portion Semen Ziziphi Spinosaes (stir-fry) 106 weight portions

Radix Polygoni Multiflori Preparata 160 weight portion Radix Glycyrrhizae Preparatas 53 weight portion Pericarpium Citri Reticulataes (steaming) 53 weight portions

Colla cornus cervi (stir-fry) 23 weight portion Radix Rehmanniae Preparata 160 weight portion Colla Plastri Testudiniss (stir-fry) 34 weight portions

Fructus Rosae Laevigatae (steaming) 128 weight portion Radix Astragali Preparatas 106 weight portion Rhizoma Dioscoreaes (stir-fry) 106 weight portions

Fructus Rubi (steaming) 213 weight portions

Preparation method is: get broken 10～75 microns of Pericarpium Citri Reticulatae, Rhizoma Dioscoreae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Carapax et Plastrum Testudinis rubber powder micropowder, and standby; All the other Semen Cuscutae etc. ten decoct with water secondary simply in the prescription, 2-3 hour for the first time, add 10-14 times of water gaging; 1-2 hour for the second time, add 8-12 times of water gaging; Collecting decoction filters, and concentrates, and cold preservation was left standstill 12-24 hour, gets supernatant and filters, and is concentrated into the thick paste shape, and 75 ℃ of dryings get dry extract, and are ground into fine powder, and are standby; Above-mentioned dried cream fine powder and Pericarpium Citri Reticulatae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis four flavor fine powders mix and grind, and add 10-20%PVK30 ethanol liquid and granulate 70-75 ℃ of drying; Add adjuvant, mixing, direct compression or make granule.

The method of quality control that this compositions is made medicament comprises discriminating and/or assay.

Discrimination method comprises a kind of and/or several in the following method:

A. get 10 in tablet of the present invention, remove coating, porphyrize, add methanol 40-60ml, supersound process 10-20 minute, filter, the filtrate evaporate to dryness, residue adds water 20-40ml makes dissolving, uses ethyl acetate 20-40ml at every turn, and jolting is extracted 2-4 time, merge ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Polygoni Multiflori control medicinal material 0.5g, adds ethanol 40-60ml reflux 1-1.5 hour, filters, and filtrate is concentrated into 3ml, in contrast medical material solution; Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 20 μ l, control medicinal material and reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent, to make into ribbon with the carboxymethylcellulose sodium solution, with 10-20: 2-4: 1-2 toluene-ethyl acetate-formic acid is placed and was treated that stratified upper solution was developing solvent in 20-40 minute, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of contrast mouthful chromatograph on, show the fluorescence streak of same color; Behind the ammonia cure, become redness under the streak daylight.

B. get the aqueous solution behind the A item ethyl acetate extraction, use water saturated n-butyl alcohol 20-40ml at every turn, extract 2-4 time, merge n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, add the 0.5-1g neutral alumina and mix thoroughly, drying is added in 100～120 orders, 2g is on the neutral alumina post of internal diameter 10mm, with 30-50% methanol 20-40ml eluting, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.3g adds water 30-40ml in addition, and reflux 1-1.5 hour, filter, the n-butyl alcohol that filtrate water is saturated shines 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, ethyl acetate-formic acid-glacial acetic acid-water with 15-20: 1-2: 1-2: 2-4 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃, puts respectively under sight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, on the corresponding position of control medicinal material chromatograph, daylight shows identical yellow principal spot down; Under the ultra-violet lamp, show identical yellow fluorescence principal spot.

C. get 10 in tablet of the present invention, remove coating, porphyrize, add methanol 30-50ml, reflux 1-1.5 hour, filter, filtrate evaporate to dryness, residue add water 30-40ml makes dissolving, uses ethyl acetate 20-40ml at every turn, extract 2-4 time, discard ethyl acetate liquid, water layer extracts 2-4 time with water saturated n-butyl alcohol 20-40ml at every turn, merge n-butanol extracting liquid, use 1% sodium hydroxide solution 20-40ml at every turn, wash 2-4 time, discard alkali wash water, each water 20-30ml washs 2-4 time, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, adding the 0.5-1g neutral alumina mixes thoroughly, drying is added in 100～120 orders, 2g, on the neutral alumina post of internal diameter 10mm, with 30-50% methanol 40-60ml eluting, collect eluent, evaporate to dryness, residue adds methanol 0.5ml makes dissolving, as need testing solution; Other gets the astragaloside 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 need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on the same silica gel g thin-layer plate of thick 0.5mm, with 10-15: 20-25: 10-15: 5-10 chloroform-ethyl acetate-methanol-water, at lower floor's solution of placing 10-20 hour below 10 ℃ is developing solvent, launches; Take out, dry, spray is with the 10-15% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105-110 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, daylight shows down identical sepia speckle, ultra-violet lamp shows identical orange-yellow fluorescence speckle down.

Content assaying method comprises following assay method:

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Water-acetonitrile-oxolane-glacial acetic acid with 750-760: 230-240: 10-15: 5-10 is a mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by the icariin peak should be not less than 3500;

The preparation of reference substance solution: take by weighing the icariin reference substance, add methanol and make the solution that 1ml contains 20 μ g, promptly;

The preparation of need testing solution: get 10 in tablet of the present invention, remove coating, it is fixed to claim, get the single taking dose, it is fixed to claim, puts in the tool plug conical flask, adding concentration is 50% ethanol 50ml, and close plug claims to decide weight, supersound process 1-1.5 hour, put coldly, claim to decide weight again, with concentration is that 50% ethanol is supplied the weight that subtracts mistake, shakes up, and filters, draw subsequent filtrate 25ml, put in the evaporating dish evaporate to dryness, residue adds water 5ml makes dissolving, is added in 13～80 orders of anticipating, 5g, internal diameter 1.5cm, on the polyamide column of dry column-packing, water 50-60ml eluting, discard eluent, continue, collect eluent with ethanol 80-100ml eluting, evaporate to dryness, residue adds dissolve with methanol and is transferred in the 5ml measuring bottle, adds methanol to scale, shakes up, filter, promptly;

Algoscopy: draw each 10 μ l of reference substance solution and need testing solution respectively, inject chromatograph of liquid, measure, promptly;

Drug combination preparation per unit preparation (being equivalent to conventional tablet) per unit preparation contains Herba Epimedii by icariin C ₃₃H ₄₀O ₁₅Meter must not be less than 0.05mg.

The present invention is mainly used in the treatment spleen fatiguing disease, and especially at insufficiency of kidney-YANG and syndrome of deficiency of kidney-QI, following experimental example further specifies the present invention.

Experimental example 1: the thin layer chromatography of Radix Polygoni Multiflori is differentiated comparative experiments

Get 10 in tablet of the present invention, remove coating, porphyrize adds methanol 50ml, supersound process 15 minutes, filter, filtrate evaporate to dryness, residue add water 30ml makes dissolving, adds the ethyl acetate jolting and extracts 2 times, each 30ml, merge ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Polygoni Multiflori control medicinal material 0.5g, adds ethanol 50ml reflux 1 hour, filters, and filtrate is concentrated into 3ml, in contrast medical material solution; Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 20 μ l, control medicinal material and reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent, to make into ribbon with the carboxymethylcellulose sodium solution, with 15: 2: 1 toluene-ethyl acetate-formic acid, place and treated that stratified upper solution was developing solvent in about 30 minutes, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of contrast mouthful chromatograph on, show the fluorescence streak of same color; Behind the ammonia cure, become redness under the streak daylight;

Other gets need testing solution, with reference to " " Radix Polygoni Multiflori " thin layer chromatography of Chinese pharmacopoeia version in 2000 discrimination method launches as the developing solvent secondary with benzene-ethanol, sprays with the phosphomolybdic acid test solution again, with stilbene glucoside category feature composition in the discriminating Radix Polygoni Multiflori, but negative control has interference.

Get tablet of the present invention, with reference to " the thin layer chromatography discrimination method under " Radix Polygoni Multiflori " item of Chinese pharmacopoeia version in 2000 gets the Radix Polygoni Multiflori thin layer and differentiates collection of illustrative plates.From thin layer chromatography as seen, in the test sample chromatograph, with Radix Polygoni Multiflori control medicinal material chromatograph relevant position on, streak is difficult to be observed, this may prepare relevantly with need testing solution, and the need testing solution viscosity is big, influence launches effect.

Experimental example 2: the thin layer chromatography of Radix Glycyrrhizae is differentiated comparative experiments

Get the aqueous solution after Radix Polygoni Multiflori thin layer in the experimental example 1 is differentiated an ethyl acetate extraction, with water saturated n-butanol extraction 2 times, 30ml at every turn, merge n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, add an amount of neutral alumina and mix thoroughly, drying is added in 100～120 orders, 2g is on the internal diameter 10mm neutral alumina post, with 40% methanol 30ml eluting, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.3g adds water 30ml in addition, and reflux 1 hour filters, and the n-butyl alcohol that filtrate water is saturated shines 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 15: 1: 1: 2 ethyl acetates-formic acid-glacial acetic acid-water was developing solvent, launched, and took out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, on the corresponding position of control medicinal material chromatograph, daylight shows identical yellow principal spot down; Under the ultra-violet lamp, show identical yellow fluorescence principal spot;

Radix Glycyrrhizae in the prescription is adopted the microscopical identification method, because among this product preparation technology, Radix Glycyrrhizae powder is broken into impalpable powder (10～75 μ m), the microscopic features difficulty is examined and seen, so adopt the thin layer discrimination method.

In addition, get 10 in this pharmaceutical composition tablet, with reference to " the thin layer chromatography discrimination method under Chinese pharmacopoeia version " Radix Glycyrrhizae " in 2000 item, with the ammonium glycyrrhizinate reference substance in contrast, experimental result test sample color vinegar with reference substance chromatograph relevant position on, speckle is unintelligible, inferior separating effect.

Experimental example 3: the thin layer chromatography of the Radix Astragali is differentiated comparative experiments

Get 10 in this pharmaceutical composition tablet, remove coating, porphyrize, add methanol 40ml, reflux 1 hour filters, filtrate evaporate to dryness, residue add water 30ml makes dissolving, uses ethyl acetate extraction 2 times, each 30ml discards ethyl acetate liquid, and water layer is with water saturated n-butanol extraction 2 times, each 30ml merges n-butanol extracting liquid, with 1% sodium hydroxide solution washing 2 times, each 30ml discards alkali wash water, washes with water 2 times, each 25ml discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, adds an amount of neutral alumina and mixes drying thoroughly, be added in 100～120 orders, 2g is on the internal diameter 10mm neutral alumina post, with 40% methanol 50ml eluting, collect eluent, evaporate to dryness, residue add methanol 0.5ml makes dissolving, as need testing solution; Other gets the astragaloside 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 need testing solution 10 μ l, reference substance solution 5 μ l put respectively on the same silica gel g thin-layer plate of thick 0.5mm, with 10: 20: 11: lower floor's solution that 5 chloroforms-ethyl acetate-methanol-water was placed 12 hours below 10 ℃ was developing solvent, launched; Take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, composing on the corresponding position with the reference substance bag, daylight shows identical sepia speckle down, and ultra-violet lamp shows identical orange-yellow fluorescence speckle down.

In addition, with reference to " the thin layer chromatography discrimination method under Chinese pharmacopoeia version " Radix Astragali " in 2000 item, with chloroform-methanol-water (13: 7: 2) as developing solvent, speckle can suitably separate than former method as a result, but speckle comparatively spreads relatively, particularly the hands bed board because thin layer collection of illustrative plates speckle is more, influences result of the test and observes.

Experimental example 4: the assay condition is selected test

This product prescription is made up of 16 flavor Chinese medicines, and wherein Herba Epimedii is a principal agent, and icariin is its main effective ingredient, so be elected to be the assay index.

The selection of extraction solvent amount: in the official method, the 0.2g crude drug adds 50% ethanol 20ml and extracts.Press recipe quantity and calculate, the every capsules of this product contains Herba Epimedii and is equivalent to crude drug 0.212g, except that the floating sheep leaves of pulse plants, also contains other Chinese crude drug in considering to write out a prescription, and may influence the extraction of icariin, is that 50ml is as extracting solvent so select 50% consumption of ethanol.

The selection of extracting method: pharmacopeia adopts 1 hour method of supersound process to extract.For investigating extracting method, get 2 parts of each 1g of same test sample, it is fixed to claim, respectively adds 50% ethanol 50ml, adopts supersound process respectively 1 hour and after reflux extracted in 1 hour, measures content Determination of Icariin by the assay condition of drafting, and the results are shown in Table 1.

Table 1:

Extracting method	Supersound process 1 hour	Reflux 1 hour
Extracting method	Supersound process 1 hour	Reflux 1 hour	Content (mg/ grain)	0.0875	0.0869

By The above results as can be known, the result of two kinds of methods is basic identical, selects 1 hour extracting method as assay of supersound process for use.

Need testing solution is removed the method for interference component: get the extracting solution after the supersound process, filter, get subsequent filtrate 25ml, water bath method, residue add dissolve with methanol and are settled to 5ml, improve the need testing solution content Determination of Icariin, but other interference component concentration improves relatively, after the filtration, directly get filtrate and inject chromatograph of liquid, influence separating effect.Because this product content Determination of Icariin is lower, Herba Epimedii contains flavonoid chemical constituents such as icariin, select for use to flavones ingredient absorption, separating effect preferably polyamide reduce the interference of need testing solution impurity as purifying pillar.

The selection of eluant: get 3 parts of each 1g of same test sample, it is fixed to claim,, measures by the content assaying method of drafting as eluant with 50% ethanol, 70% ethanol, each 100ml of 100% ethanol, the results are shown in Table 2.

Table 2:

Extract solvent	50% ethanol	70% ethanol	100% ethanol
Extract solvent	50% ethanol	70% ethanol	100% ethanol	Content (mg/ grain)	0.0769	0.0826	0.0860

The above results shows that ethanol is good than other solvent to the eluting power of icariin, and as eluant.

The consumption of eluant: get 2 parts of each 1g of same test sample, it is fixed to claim, by drafting the content assaying method operation, add ethanol 60ml, 80ml respectively and carry out eluting, and the 81～100ml eluent behind the collection 80ml ethanol elution, measure content Determination of Icariin behind the evaporate to dryness, result of the test such as table 3:

Table 3:

Eluant	60ml	80ml	81～100ml
Eluant	60ml	80ml	81～100ml	Content (mg/ grain)	0.0876	0.0811	0

The above results shows, and is that the icariin eluting is complete with 60ml ethanol, considers that every batch sample content Determination of Icariin has difference, for guaranteeing the eluting of tested composition, and the usefulness of the determining eluant 80ml that measures one's own ability.

Measure the selection of wavelength: get excessive sheep flower bud glycosides reference substance solution, in the interscan of 200～320nm wave-length coverage, experimental result must have absorption maximum at 270nm wavelength place.

The selection of mobile phase: the mobile phase that pharmacopeia is recorded under " Herba Epimedii " assay item is acetonitrile-water (30: 70), through test, test sample is because the component content complexity, tested component fails effectively to separate with impurity, find that with the different proportionings of water acetonitrile-water (23: 77) is all better to the separation of icariin than other proportioning by changing acetonitrile, but still it is undesirable, selected for use afterwards flavone compound separation selectivity oxolane preferably, and add a certain amount of glacial acetic acid, make faintly acid compound separation effect better, through adjusting different proportion, test of many times, determined water-acetonitrile-oxolane-glacial acetic acid at last (755: 230: 10: 5) be best proportioning, behind the tested peak and do not have Interference Peaks substantially, can reach baseline separation.The methanol-water with different proportion, methanol-glacial acetic acid-water, methanol-0.2mol/L NaH have also been attempted in this test ₂PO ₄Make mobile phase, but separating effect is all not good enough, therefore selected water-acetonitrile-oxolane-glacial acetic acid for use (755: 230: 10: 5) be the optimal flow phase of " Herba Epimedii " assay.

Experimental example 5: sample size determination test

Get it filled three batches in compositions tablet is measured by content assaying method in the technical scheme, with content Determination of Icariin in the external standard method calculation sample.The results are shown in Table 4.

Table 4:

Lot number	1	2	On average (mg/ sheet)
Lot number	1	2	On average (mg/ sheet)	020301 020302 020303	0.0720 0.0843 0.0884	0.0751 0.0888 0.0915	0.074 0.086 0.090

Because the place of production and the difference in season, the quantity of the contained blade of crude drug are difficult to control, carry out an acceptance inspection by standard test, crude drug content acceptable ranges is bigger, so according to above experimental result, be to guarantee product quality, just decide this product and contain icariin and must not be less than the 0.05mg/ unit formulation.

Experimental example 6: assay test

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With 755: 230: 10: 5 water-acetonitrile-oxolane-glacial acetic acid was a mobile phase; The detection wavelength is 270nm; Theory is pulled number should be not less than 3500 by the calculating of icariin peak;

The preparation of need testing solution: get 10 in tablet of the present invention, remove coating, it is fixed to claim, get about 2 amount, it is fixed to claim, puts in the tool plug conical flask, adding concentration is 50% ethanol 50ml, and close plug claims to decide weight, supersound process 1 hour is put coldly, claims to decide weight again, with concentration is that 50% ethanol is supplied the weight that subtracts mistake, shakes up, and filters, draw subsequent filtrate 25ml, put in the evaporating dish evaporate to dryness, residue adds water 5ml makes dissolving, is added in 13～80 orders of anticipating, 5g, internal diameter 1.5cm, on the polyamide column of dry column-packing, water 50ml eluting, discard eluent, continue, collect eluent with ethanol 80ml eluting, evaporate to dryness, residue adds dissolve with methanol and is transferred in the 5ml measuring bottle, adds methanol to scale, shakes up, filter, promptly;

Every in tablet of the present invention contains Herba Epimedii by icariin C ₃₃H ₄₀O ₁₅Meter must not be less than 0.05mg;

Measure and the test of medical material assay through blank assay, precision test, replica test, stability test, application of sample recovery test, sample size, prove that above-mentioned assay test method can improve the control drug quality.

Experimental example 7: clinical drug trial

With reference to " syndrome of deficiency of kidney-YANG " standard of carrying the whole nation the 3rd traditional Chinese medical science combination of Chinese and Western medicine deficiency syndrome meeting formulation of record in national high traditional Chinese medical science universities and colleges' teaching materials " Chinese Internal Medicine " spleen fatiguing diseases " syndrome of deficiency of kidney-YANG " and the Ministry of Public Health " the clinical research guideline of new Chinese medicine treatment syndrome of deficiency of kidney-YANG ".30 routine patients, male 14 examples, women 16 examples, the oldest 68 years old, minimum 40 years old.Primary symptom: soreness of waist and knee joint, aversion to cold and cold limbs, hyposexuality, body of the tongue is fat big, and tongue is white, deep pulse.Inferior disease: lassitude, nocturia, big loose stool.Take tablet of the present invention, each 4,2 times on the one, 4 weeks were 1 course of treatment.

Table 4: mild symptoms weight classification

Symptom	Gently (+)	In (++)	Heavy (+++)
Symptom	Gently (+)	In (++)	Heavy (+++)	Soreness of waist and knee joint sexual disorder lassitude nocturia	Idol has the outbreak libido to reduce the lassitude nocturia 1-2 time	Even sexual lethargy nocturia 3-4 time that require of outbreak repeatedly	Continue outbreak, be difficult for alleviating sexual impotence or infertility lethargy, bradykinesia nocturia frequency, number of times is a lot

Curative effect judging standard

1, clinical recovery: deficiency of kidney-QI or insufficiency of kidney-YANG symptom disappear.

2, produce effects: deficiency of kidney-QI or insufficiency of kidney-YANG symptom obviously improve more than 2 grades (by +++become+): or indivedual symptom changes at 1 grade, and other symptoms all disappear.

3, effective: deficiency of kidney-QI or deficiency of kidney-YANG syndrome improve more than 1 grade, or indivedual symptom be significantly improved (by ++ become+).

4, invalid: deficiency of kidney-QI or insufficiency of kidney-YANG symptom do not have improvement.

Result of the test:

1, total effects: clinical recovery 8 examples (accounting for 26.67%), produce effects 14 examples (accounting for 46.67%), row is imitated 7 examples (accounting for 23.33%), invalid 1 example (accounting for 3.33%).

2, symptom curative effect

Soreness of waist and knee joint effective percentage 96.67% (29/30)

Sexual disorder effective percentage 50% (6/12)

Lassitude effective percentage 71.43% (20/28)

Nocturia effective percentage 72% (18/25)

This drug combination preparation treatment deficiency of five viscera syndrome of deficiency of kidney-QI and syndrome of deficiency of kidney-YANG, effective percentage is remarkable, and determined curative effect is safe in utilization.

Specific embodiments of the invention are as follows

Embodiment 1The preparation tablet

Semen Cuscutae (stir-fry) 128g Herba Epimedii (steaming) 106g Radix Dipsaci (steaming) 106g

Herba Cynomorii (steaming) 128g Rhizoma Cibotii (steaming) 160g Semen Ziziphi Spinosae (stir-fry) 106g

Radix Polygoni Multiflori Preparata 160g Radix Glycyrrhizae Preparata 53g Pericarpium Citri Reticulatae (steaming) 53g

Colla cornus cervi (stir-fry) 23g Radix Rehmanniae Preparata 160g Colla Plastri Testudinis (stir-fry) 34g

Fructus Rosae Laevigatae (steaming) 128g Radix Astragali Preparata 106g Rhizoma Dioscoreae (stir-fry) 106g

Fructus Rubi (steaming) 213g

Get 75 microns of Pericarpium Citri Reticulataes, Rhizoma Dioscoreae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis micronizing, standby; All the other Semen Cuscutae etc. ten decoct with water secondary simply in the prescription, 2 hours for the first time, add 12 times of water gagings; 1 hour for the second time, add 10 times of water gagings; Collecting decoction filters, and concentrates, and cold preservation was left standstill 16 hours, gets supernatant and filters, and is concentrated into the thick paste shape, and 75 ℃ of dryings get dry extract, and are ground into fine powder, and are standby; Above-mentioned dried cream fine powder and Pericarpium Citri Reticulatae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis four flavor fine powders mix and grind, and add 10%PVK30 ethanol liquid and granulate 75 ℃ of dryings, granulate; Dry granular adds carboxymethyl starch sodium 14g again, and is above-mentioned by the medicated powder mixing, and add 50%7 alcohol and granulate, 75 ℃ of dryings, granulate adds carboxymethyl starch sodium 13g, silica 1 0g and magnesium stearate 5g, and mixing is pressed special-shaped tablets, wraps pink film-coat, promptly.

Embodiment 2The preparation tablet

Semen Cuscutae (stir-fry) 120g Herba Epimedii (steaming) 100g Radix Dipsaci (steaming) 100g

Herba Cynomorii (steaming) 120g Rhizoma Cibotii (steaming) 150g Semen Ziziphi Spinosae (stir-fry) 100g

Radix Polygoni Multiflori Preparata 150g Radix Glycyrrhizae Preparata 50g Pericarpium Citri Reticulatae (steaming) 50g

Colla cornus cervi (stir-fry) 20g Radix Rehmanniae Preparata 150g Colla Plastri Testudinis (stir-fry) 30g

Fructus Rosae Laevigatae (steaming) 120g Radix Astragali Preparata 100g Rhizoma Dioscoreae (stir-fry) 100g

Fructus Rubi (steaming) 210g

Get 20 microns of Pericarpium Citri Reticulataes, Rhizoma Dioscoreae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Carapax et Plastrum Testudinis rubber powder micronizing, standby; All the other Semen Cuscutae etc. ten decoct with water secondary simply in the prescription, 2 hours for the first time, add 11 times of water gagings; 1 hour for the second time, add 8 times of water gagings; Collecting decoction filters, and concentrates, and cold preservation was left standstill 15 hours, gets supernatant and filters, and is concentrated into the thick paste shape, and 75 ℃ of dryings get dry extract, and are ground into fine powder, and are standby; Above-mentioned dried cream fine powder and Pericarpium Citri Reticulatae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis four flavor fine powders mix and grind, and add 10%PVK30 ethanol liquid and granulate 70 ℃ of dryings, granulate; Dry granular adds carboxymethyl starch sodium 10g again, and is above-mentioned by the medicated powder mixing, and add 40% alcohol and granulate, 70 ℃ of dryings, granulate adds carboxymethyl starch sodium 10g, silicon dioxide 8g and magnesium stearate 4g, and mixing, tabletting are promptly.

Embodiment 3The preparation tablet

Semen Cuscutae (stir-fry) 140g Herba Epimedii (steaming) 110g Radix Dipsaci (steaming) 110g

Herba Cynomorii (steaming) 140g Rhizoma Cibotii (steaming) 170g Semen Ziziphi Spinosae (stir-fry) 110g

Radix Polygoni Multiflori Preparata 170g Radix Glycyrrhizae Preparata 60g Pericarpium Citri Reticulatae (steaming) 60g

Colla cornus cervi (stir-fry) 30g Radix Rehmanniae Preparata 170g Colla Plastri Testudinis (stir-fry) 40g

Fructus Rosae Laevigatae (steaming) 140g Radix Astragali Preparata 110g Rhizoma Dioscoreae (stir-fry) 110g

Fructus Rubi (steaming) 230g

Get 40 microns of Pericarpium Citri Reticulataes, Rhizoma Dioscoreae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Carapax et Plastrum Testudinis rubber powder micronizing, standby; All the other Semen Cuscutae etc. ten decoct with water secondary simply in the prescription, 2.5 hours for the first time, add 12 times of water gagings; 1.5 hours for the second time, add 10 times of water gagings; Collecting decoction filters, and concentrates, and cold preservation was left standstill 20 hours, gets supernatant and filters, and is concentrated into the thick paste shape, and 75 ℃ of dryings get dry extract, and are ground into fine powder, and are standby; Above-mentioned dried cream fine powder and Pericarpium Citri Reticulatae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis four flavor fine powders mix and grind, and add 15%PVK30 ethanol liquid and granulate 75 ℃ of dryings, granulate; Dry granular adds carboxymethyl starch sodium 12g again, and is above-mentioned by the medicated powder mixing, adds 50% alcohol granulation, 75 ℃ of dryings, and granulate adds carboxymethyl starch sodium 12g, silica 1 0g and magnesium stearate 6g, mixing, direct compression.

Embodiment 4The preparation tablet

Semen Cuscutae (stir-fry) 120g Herba Epimedii (steaming) 110g Radix Dipsaci (steaming) 100g

Herba Cynomorii (steaming) 140g Rhizoma Cibotii (steaming) 150g Semen Ziziphi Spinosae (stir-fry) 110g

Radix Polygoni Multiflori Preparata 150g Radix Glycyrrhizae Preparata 60g Pericarpium Citri Reticulatae (steaming) 50g

Colla cornus cervi (stir-fry) 30g Radix Rehmanniae Preparata 150g Colla Plastri Testudinis (stir-fry) 40g

Fructus Rosae Laevigatae (steaming) 120g Radix Astragali Preparata 110g Rhizoma Dioscoreae (stir-fry) 100g

Fructus Rubi (steaming) 230g

Get 60 microns of Pericarpium Citri Reticulataes, Rhizoma Dioscoreae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Carapax et Plastrum Testudinis rubber powder micronizing, standby; All the other Semen Cuscutae etc. ten decoct with water secondary simply in the prescription, 3 hours for the first time, add 13 times of water gagings; 2 hours for the second time, add 12 times of water gagings; Collecting decoction filters, and concentrates, and cold preservation was left standstill 4 hours, gets supernatant and filters, and is concentrated into the thick paste shape, and 75 ℃ of dryings get dry extract, and are ground into fine powder, and are standby; Above-mentioned dried cream fine powder and Pericarpium Citri Reticulatae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis four flavor fine powders mix and grind, and add 20%PVK30 ethanol liquid, 75 ℃ of dryings, granulate; Dry granular adds carboxymethyl starch sodium 15g again, and is above-mentioned by the medicated powder mixing, adds 60% alcohol granulation, 75 ℃ of dryings, and granulate adds carboxymethyl starch sodium 15g, silica 1 2g and magnesium stearate 8g, mixing, direct compression.

Embodiment 5The preparation granule

Colla cornus cervi (stir-fry) 23g Radix Rehmanniae Preparata 160g plate glue (stir-fry) 34g

Fructus Rubi (steaming) 213g

Get 75 microns of Pericarpium Citri Reticulataes, Rhizoma Dioscoreae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis micronizing, standby; All the other Semen Cuscutae etc. ten decoct with water secondary simply in the prescription, 2 hours for the first time, add 12 times of water gagings; 1 hour for the second time, add 10 times of water gagings; Collecting decoction filters, and concentrates, and cold preservation was left standstill 16 hours, gets supernatant and filters, and is concentrated into the thick paste shape, and 75 ℃ of dryings get dry extract, and are ground into fine powder, and are standby; Above-mentioned dried cream fine powder and Pericarpium Citri Reticulatae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis four flavor fine powders add cane sugar powder 500g again, and dextrin 72g mixes and grinds, and add 10%PVK30 ethanol liquid and granulate, 75 ℃ of dryings, granulate is promptly.

Embodiment 6Preparation granule system

Semen Cuscutae (stir-fry) 140g Herba Epimedii (steaming) 100g Radix Dipsaci (steaming) 110g

Herba Cynomorii (steaming) 120g Rhizoma Cibotii (steaming) 170g Semen Ziziphi Spinosae (stir-fry) 100g

Radix Polygoni Multiflori Preparata 170g Radix Glycyrrhizae Preparata 50g Pericarpium Citri Reticulatae (steaming) 60g

Colla cornus cervi (stir-fry) 20g Radix Rehmanniae Preparata 170g Colla Plastri Testudinis (stir-fry) 30g

Fructus Rosae Laevigatae (steaming) 140g Radix Astragali Preparata 100g Rhizoma Dioscoreae (stir-fry) 110g

Fructus Rubi (steaming) 210g

Get 20 microns of Pericarpium Citri Reticulataes, Rhizoma Dioscoreae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Carapax et Plastrum Testudinis rubber powder micronizing, standby; All the other Semen Cuscutae etc. ten decoct with water secondary simply in the prescription, 2 hours for the first time, add 11 times of water gagings; 1 hour for the second time, add 8 times of water gagings; Collecting decoction filters, and concentrates, and cold preservation was left standstill 15 hours, gets supernatant and filters, and is concentrated into the thick paste shape, and 75 ℃ of dryings get dry extract, and are ground into fine powder, and are standby; Above-mentioned dried cream fine powder and Pericarpium Citri Reticulatae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis four flavor fine powders add cane sugar powder 500g again, and dextrin 38g mixes and grinds, and add 10%PVK30 ethanol liquid and granulate, 70 ℃ of dryings, granulate is promptly.

Embodiment 7The preparation granule

Semen Cuscutae (stir-fry) 130g Herba Epimedii (steaming) 105g Radix Dipsaci (steaming) 105g

Herba Cynomorii (steaming) 130g Rhizoma Cibotii (steaming) 160g Semen Ziziphi Spinosae (stir-fry) 105g

Radix Polygoni Multiflori Preparata 160g Radix Glycyrrhizae Preparata 55g Pericarpium Citri Reticulatae (steaming) 55g

Colla cornus cervi (stir-fry) 25g Radix Rehmanniae Preparata 160g Colla Plastri Testudinis (stir-fry) 35g

Fructus Rosae Laevigatae (steaming) 130g Radix Astragali Preparata 105g Rhizoma Dioscoreae (stir-fry) 105g

Fructus Rubi (steaming) 220g

Get 40 microns of Pericarpium Citri Reticulataes, Rhizoma Dioscoreae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Carapax et Plastrum Testudinis rubber powder micronizing, standby; All the other Semen Cuscutae etc. ten decoct with water secondary simply in the prescription, 2.5 hours for the first time, add 12 times of water gagings; 1.5 hours for the second time, add 10 times of water gagings; Collecting decoction filters, and concentrates, and cold preservation was left standstill 20 hours, gets supernatant and filters, and is concentrated into the thick paste shape, and 75 ℃ of dryings get dry extract, and are ground into fine powder, and are standby; Above-mentioned dried cream fine powder and Pericarpium Citri Reticulatae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis four flavor fine powders add cane sugar powder 500g again, and dextrin 35g mixes and grinds, and add 15%PVK30 ethanol liquid and granulate, 75 ℃ of dryings, granulate is promptly.

Embodiment 8The preparation granule

Fructus Rosae Laevigatae (steaming) 140g Radix Astragali Preparata 110g medicine (stir-fry) 110g

Fructus Rubi (steaming) 230g

Get 60 microns of Pericarpium Citri Reticulataes, Rhizoma Dioscoreae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Carapax et Plastrum Testudinis rubber powder micronizing, standby; All the other Semen Cuscutae etc. ten decoct with water secondary simply in the prescription, 3 hours for the first time, add 13 times of water gagings; 2 hours for the second time, add 12 times of water gagings; Collecting decoction filters, and concentrates, and cold preservation was left standstill 4 hours, gets supernatant and filters, and is concentrated into the thick paste shape, and 75 ℃ of dryings get dry extract, and are ground into fine powder, and are standby; Above-mentioned dried cream fine powder and Pericarpium Citri Reticulatae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis four flavor fine powders add cane sugar powder 470g again, and dextrin 29g mixes and grinds, and adds 20%PVK30 ethanol liquid, 75 ℃ of dryings, and granulate is promptly.

Embodiment 9The assay test

Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With 755: 230: 10: 5 water-acetonitrile-oxolane-glacial acetic acid was a mobile phase; The detection wavelength is 270nm; Theory is pulled number should be not less than 3500 by the calculating of icariin peak;

The preparation of need testing solution: get 10 in tablet of the present invention, remove coating, the accurate title, decide, get about 2 amount, it is fixed to claim, puts in the tool plug conical flask, adding concentration is 50% ethanol 50ml, and close plug claims to decide weight, supersound process 1 hour is put coldly, claims to decide weight again, with concentration is that 50% ethanol is supplied the weight that subtracts mistake, shakes up, and filters, draw subsequent filtrate 25ml, put in the evaporating dish evaporate to dryness, residue adds water 5ml makes dissolving, is added in 13～80 orders of anticipating, 5g, internal diameter 1.5cm, on the polyamide column of dry column-packing, water 50ml eluting, discard eluent, continue, collect eluent with ethanol 80ml eluting, evaporate to dryness, residue adds dissolve with methanol and is transferred in the 5ml measuring bottle, adds methanol to scale, shakes up, filter, promptly;

Embodiment 10The preparation tablet

Fructus Rubi (steaming) 230g

Get the above-mentioned raw materials medicine and make tablet, every heavy 0.5g, the deficiency of five viscera patient is oral, each 2-4 sheet, every day 2 times.

Embodiment 11The preparation granule

Fructus Rubi (steaming) 210g

Get the above-mentioned raw materials medicine and make granule, every bag heavy 2g, the deficiency of five viscera patient is oral, each 1-2 bag, every day 2 times.

Claims

1, a kind of Chinese medicine composition is characterized in that this pharmaceutical composition is made up of following crude drug:

Semen Cuscutae 120-140 weight portion Herba Epimedii 100-110 weight portion

Radix Dipsaci 100-110 weight portion Herba Cynomorii 120-140 weight portion

Rhizoma Cibotii 50-170 weight portion Semen Ziziphi Spinosae 100-110 weight portion

Radix Polygoni Multiflori 150-170 weight portion Radix Glycyrrhizae Preparata 50-60 weight portion

Pericarpium Citri Reticulatae 50-60 weight portion Colla cornus cervi 20-30 weight portion

Radix Rehmanniae Preparata 150-170 weight portion Colla Plastri Testudinis 30-40 weight portion

Fructus Rosae Laevigatae 120-140 weight portion Radix Astragali Preparata 100-110 weight portion

Rhizoma Dioscoreae 100-110 weight portion Fructus Rubi 210-230 weight portion.

2, the described pharmaceutical composition of claim 1 is characterized in that this pharmaceutical composition is made up of following crude drug:

Semen Cuscutae (parched) 128 weight portions steam Herba Epimedii 106 weight portions

Steam Radix Dipsaci 106 weight portions and steam Herba Cynomorii 128 weight portions

Steam Rhizoma Cibotii 160 weight portion Semen Ziziphi Spinosae (parched)s 106 weight portions

Radix Polygoni Multiflori Preparata 160 weight portion Radix Glycyrrhizae Preparatas 53 weight portions

Steam Pericarpium Citri Reticulatae 53 weight portions and fry Colla cornus cervi 23 weight portions

Radix Rehmanniae Preparata 160 weight portions are fried Colla Plastri Testudinis 34 weight portions

Steam Fructus Rosae Laevigatae 128 weight portion Radix Astragali Preparatas 106 weight portions

Rhizoma dioscoreae (parched) 106 weight portions steam Fructus Rubi 213 weight portions.

3, claim 1 or 2 described preparation of drug combination methods is characterized in that this method comprises the steps:

Get broken 10～75 microns of Pericarpium Citri Reticulatae, Rhizoma Dioscoreae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Carapax et Plastrum Testudinis rubber powder micropowder, standby; All the other Semen Cuscutae etc. ten decoct with water secondary simply in the prescription, 2-3 hour for the first time, add 10-14 times of water gaging; 1-2 hour for the second time, add 8-12 times of water gaging; Collecting decoction filters, and concentrates, and cold preservation was left standstill 12-24 hour, gets supernatant and filters, and is concentrated into the thick paste shape, and 75 ℃ of dryings get dry extract, and are ground into fine powder, and are standby; Above-mentioned dried cream fine powder and Pericarpium Citri Reticulatae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis four flavor fine powders mix and grind, and add 10-20%PVK30 ethanol liquid and granulate, and 70-75 ℃ of drying adds adjuvant, mixing, direct compression or make granule.

4, preparation of drug combination method as claimed in claim 3 is characterized in that this method may further comprise the steps:

Get 75 microns of Pericarpium Citri Reticulataes, Rhizoma Dioscoreae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Carapax et Plastrum Testudinis rubber powder micronizing, standby; All the other Semen Cuscutae etc. ten decoct with water secondary simply in the prescription, 2 hours for the first time, add 12 times of water gagings; 1 hour for the second time, add 10 times of water gagings; Collecting decoction filters, and concentrates, and cold preservation was left standstill 16 hours, gets supernatant and filters, and is concentrated into the thick paste shape, and 75 ℃ of dryings get dry extract, and are ground into fine powder, and are standby; Above-mentioned dried cream fine powder and Pericarpium Citri Reticulatae, Radix Glycyrrhizae Preparata, Colla cornus cervi, Colla Plastri Testudinis four flavor fine powders mix and grind, and add 10%PVK30 ethanol liquid and granulate, and 75 ℃ of dryings add adjuvant, mixing, direct compression or make granule.

5, the method for quality control of pharmaceutical composition as claimed in claim 1 or 2 is characterized in that discrimination method in this method comprises one or more in the following discriminating:

A. get 10 in this pharmaceutical composition tablet, remove coating, porphyrize, add methanol 40-60ml, supersound process 10-20 minute, filter, the filtrate evaporate to dryness, residue adds water 20-40ml makes dissolving, uses ethyl acetate 20-40ml at every turn, and jolting is extracted 2-4 time, merge ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Polygoni Multiflori control medicinal material 0.5g, adds ethanol 40-60ml reflux 1-1.5 hour, filters, and filtrate is concentrated into 3ml, in contrast medical material solution; Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 20 μ l, control medicinal material and reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent, to make into ribbon with the carboxymethylcellulose sodium solution, with 10-20: 2-4: 1-2 toluene-ethyl acetate-formic acid is placed and was treated that stratified upper solution was developing solvent in 20-40 minute, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of contrast mouthful chromatograph on, show the fluorescence streak of same color; Behind the ammonia cure, become redness under the streak daylight;

B. get the aqueous solution behind the A item ethyl acetate extraction, use water saturated n-butyl alcohol 20-40ml at every turn, extract 2-4 time, merge n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, add the 0.5-1g neutral alumina and mix thoroughly, drying is added in 100～120 orders, 2g is on the neutral alumina post of internal diameter 10mm, with 30-50% methanol 20-40ml eluting, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.3g adds water 30-40ml in addition, and reflux 1-1.5 hour, filter, the n-butyl alcohol that filtrate water is saturated shines 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, ethyl acetate-formic acid-glacial acetic acid-water with 15-20: 1-2: 1-2: 2-4 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, on the corresponding position of control medicinal material chromatograph, daylight shows identical yellow principal spot down; Under the ultra-violet lamp, show identical yellow fluorescence principal spot;

C. get 10 in this pharmaceutical composition tablet, remove coating, porphyrize, add methanol 30-50ml, reflux 1-.5 hour, filter, filtrate evaporate to dryness, residue add water 30-40ml makes dissolving, uses ethyl acetate 20-40ml at every turn, extract 2-4 time, discard ethyl acetate liquid, water layer extracts 2-4 time with water saturated n-butyl alcohol 20-40ml at every turn, merge n-butanol extracting liquid, use 1% sodium hydroxide solution 20-40ml at every turn, wash 2-4 time, discard alkali wash water, each water 20-30ml washs 2-4 time, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, adding the 0.5-1g neutral alumina mixes thoroughly, drying is added in 100～120 orders, 2g, on the neutral alumina post of internal diameter 10mm, with 30-50% methanol 40-60ml eluting, collect eluent, evaporate to dryness, residue adds methanol 0.5ml makes dissolving, as need testing solution; Other gets the astragaloside 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 need testing solution 10 μ l, reference substance solution 5 μ l, put respectively on the same silica gel g thin-layer plate of thick 0.5mm, with 10-15: 20-25: 10-15: 5-10 chloroform-ethyl acetate-methanol-water, at lower floor's solution of placing 10-20 hour below 10 ℃ is developing solvent, launches; Take out, dry, spray is with the 10-15% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105-110 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, daylight shows down identical sepia speckle, ultra-violet lamp shows identical orange-yellow fluorescence speckle down.

6, require the discrimination method of 5 described pharmaceutical compositions as profit, it is characterized in that this discrimination method comprises one or more in the following discriminating:

A. get 10 in this pharmaceutical composition tablet, remove coating, porphyrize, add methanol 50ml, supersound process 15 minutes filters, the filtrate evaporate to dryness, residue adds water 30ml makes dissolving, adds the ethyl acetate jolting and extracts 2 times, each 30ml, merge ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Polygoni Multiflori control medicinal material 0.5g, adds ethanol 50ml reflux 1 hour, filters, and filtrate is concentrated into 3ml, in contrast medical material solution; Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 20 μ l, control medicinal material and reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent, to make into ribbon with the carboxymethylcellulose sodium solution, with 15: 2: 1 toluene-ethyl acetate-formic acid, place and treated that stratified upper solution was developing solvent in about 30 minutes, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of contrast mouthful chromatograph on, show the fluorescence streak of same color; Behind the ammonia cure, become redness under the streak daylight;

B. get the aqueous solution behind the A item ethyl acetate extraction, with water saturated n-butanol extraction 2 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, add an amount of neutral oxidation instruction aluminum and mix thoroughly, drying is added in 100～120 orders, 2g is on the internal diameter 10mm neutral alumina post, with 40% methanol 30ml eluting, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Extracting liquorice contrast medicine letter 0.3g adds water 30ml in addition, and reflux 1 hour filters, and the n-butyl alcohol that filtrate water is saturated shines 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 15: 1: 1: 2 ethyl acetates-formic acid-glacial acetic acid-water was developing solvent, launched, and took out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 100 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, on the corresponding position of control medicinal material chromatograph, daylight shows identical yellow principal spot down; Under the ultra-violet lamp, show identical yellow fluorescence principal spot;

C. get 10 in this pharmaceutical composition tablet, remove coating, porphyrize, add methanol 40ml, reflux 1 hour filters, filtrate evaporate to dryness, residue add water 30ml makes dissolving, uses ethyl acetate extraction 2 times, each 30ml discards ethyl acetate liquid, and water layer is with water saturated n-butanol extraction 2 times, each 30ml merges n-butanol extracting liquid, with 1% sodium hydroxide solution washing 2 times, each 30ml discards alkali wash water, washes with water 2 times, each 25ml discards water liquid, and n-butyl alcohol liquid steams, residue adds methanol 1ml makes dissolving, adds an amount of neutral alumina and mixes drying thoroughly, be added in 100～120 orders, 2g is on the internal diameter 10mm neutral alumina post, with 40% methanol 50ml eluting, collect eluent, evaporate to dryness, residue add methanol 0.5ml makes dissolving, as need testing solution; Other gets the astragaloside 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 need testing solution 10 μ l, reference substance solution 5 μ l put respectively on the same silica gel g thin-layer plate of thick 0.5mm, with 10: 20: 11: lower floor's solution that 5 chloroforms-ethyl acetate-methanol-water was placed 12 hours below 10 ℃ was developing solvent, launched; Take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, composing on the corresponding position with the reference substance bag, showing identical sepia speckle under the sight, ultra-violet lamp shows identical orange-yellow fluorescence speckle down.

7, require the method for quality control of 1 or 2 described pharmaceutical compositions as profit, it is characterized in that the assay in this method comprises following assay method:

Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Water-acetonitrile-oxolane-glacial acetic acid with 750-760: 230-240: 10-15: 5-10 is a mobile phase; The detection wavelength is 270nm; Theory is pulled number should be not less than 3500 by the calculating of icariin peak;

The preparation of need testing solution: get 10 in this pharmaceutical composition tablet, remove coating, it is fixed to claim, get the single taking dose, it is fixed to claim, puts in the tool plug conical flask, adding concentration is 50% ethanol 50ml, and close plug claims to decide weight, supersound process 1-1.5 hour, put coldly, claim to decide weight again, with concentration is that 50% ethanol is supplied the weight that subtracts mistake, shakes up, and filters, draw subsequent filtrate 25ml, put in the evaporating dish evaporate to dryness, residue adds water 5ml makes dissolving, is added in 13～80 orders of anticipating, 5g, internal diameter 1.5cm, on the polyamide column of dry column-packing, water 50-60ml eluting, discard eluent, continue, collect eluent with ethanol 80-100ml eluting, evaporate to dryness, residue adds dissolve with methanol and is transferred in the 5ml measuring bottle, adds methanol to scale, shakes up, filter, promptly;

This drug combination preparation per unit preparation contains Herba Epimedii by icariin C ₃₃H ₄₀O ₁₅Meter must not be less than 0.05mg.

8, require 7 described method of quality control as profit, it is characterized in that the assay in this method comprises following assay method:

The preparation of need testing solution: get 10 in this pharmaceutical composition tablet, remove coating, it is fixed to claim, get about 2 amount, it is fixed to claim, puts in the tool plug conical flask, adding concentration is 50% ethanol 50ml, and close plug claims to decide weight, supersound process 1 hour is put coldly, claims to decide weight again, with concentration is that 50% ethanol is supplied the weight that subtracts mistake, shakes up, and filters, draw subsequent filtrate 25ml, put in the evaporating dish evaporate to dryness, residue adds water 5ml makes dissolving, is added in 13～80 orders of anticipating, 5g, internal diameter 1.5cm, on the polyamide column of dry column-packing, water 50ml eluting, discard eluent, continue, collect eluent with ethanol 80ml eluting, evaporate to dryness, residue adds dissolve with methanol and is transferred in the 5ml measuring bottle, adds methanol to scale, shakes up, filter, promptly;

9, the application of pharmaceutical composition as claimed in claim 1 or 2 in the medicine of preparation treatment deficiency of five viscera.

10, the application of pharmaceutical composition as claimed in claim 1 or 2 in the medicine of preparation treatment syndrome of deficiency of kidney-YANG or syndrome of deficiency of kidney-QI.