CN1994373A

CN1994373A - Formulation with basil, ginkgo leaf and notoginseng, preparation process and quality control method

Info

Publication number: CN1994373A
Application number: CNA2006101102332A
Authority: CN
Inventors: 叶湘武; 周黎亚
Original assignee: Guizhou Yibai Pharmaceutical Co Ltd
Current assignee: Guizhou Yibai Pharmaceutical Co Ltd
Priority date: 2006-12-27
Filing date: 2006-12-27
Publication date: 2007-07-11

Abstract

The invention relates to a method for producing honeysuckle flower notoginseng agent and relative quality control method, wherein it is mainly tablet, formed by ginkgo leaf extractive at 20-80 deals, veratriloside at 50-200 deals, notoginseng at 50-200 deals, Danshen at 50-200 deals, chuanxiong rhizome at 50-200 deals, frank incense at 25-100 deals, synthetic musk at 5-20 deals, and baras camphor at 12. 5-50 deals. Compared with present technique, the invention has high density, low cost and simple application. The inventon provides finding kinds and consumption. The inventive quality control method has high accuracy and high stability, to confirm clinic effect.

Description

A kind of gold silver notoginseng preparations and preparation method thereof and method of quality control

Technical field: the present invention relates to a kind of gold silver notoginseng preparations and preparation method thereof and method of quality control, belong to technical field of medicaments.

Background technology: the gold silver notoginseng preparations by Folium Ginkgo extract, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, Olibanum, artificial Moschus, Borneolum Syntheticum totally eight the flavor medicinal material extract make, have vital energy regualting and blood circulation-promoting, the effect of stasis-dispelling and pain-killing.For the thoracic obstruction due to the blood stasis impatency, uncomfortable in chest have a good therapeutic effect.Wherein " gold silver notoginseng capsule " rises GB internal medicine at national standard for traditional Chinese medicines terrestrial reference and feels concerned about in the fascicle on the books.Tablet is a common formulations, has steady quality, takes, carries, storage and convenient transportation, be suitable for mechanization production, cost is low, advantages such as protection against the tide and the loss of volatilization prevention composition, also be one of conventional dosage form of producing, and dosage form is comparatively single in the existing standard, can't satisfy more patients' needs; Simultaneously, regulation percolation speed not when in the existing preparation process percolation technology being investigated, and percolation speed is very important link in preparation of the present invention extracts, speed is crossed and can be caused the operating time long slowly, the effective ingredient impurity that obtains simultaneously is too much, excessive velocities can cause separates not exclusively, and the dried cream amount that obtains is very few; In addition, in existing preparation quality standard, to the assay of total flavonoids in the Folium Ginkgo extract adopt the methanol supersound process, the method that adds sour reflux prepares test sample, but extract through the method, impurity peaks is more, and repeatability is bad, is difficult for detecting and the control medicament contg; When Radix Notoginseng is carried out the thin layer discriminating, serve as that the Radix Notoginseng that contains in the medicine is differentiated in contrast with panoxadiol, panaxatriol, through test, the primary standard method is relatively poor, and speckled background disturbs greatly, is difficult for inspecting, and can not differentiate pseudo-ginseng in the preparation exactly; So existing preparation formulation and method of quality control can not satisfy numerous crowds' needs, can not effectively control the quality of this gold silver Radix Notoginseng oral formulations, thereby will influence the clinical efficacy of said preparation.

Summary of the invention:

The objective of the invention is to: a kind of gold silver Radix Notoginseng oral formulations is provided; Another object of the present invention is to provide the preparation method of gold silver Radix Notoginseng oral formulations; The 3rd purpose of the present invention also is to provide a kind of method of quality control of gold silver Radix Notoginseng oral formulations; This oral formulations comprises capsule, tablet.

The inventor finds in the research process of preparation process of the present invention, percolation speed is an important step that influences the quality of the pharmaceutical preparations of the present invention, and speed is crossed and can be caused the operating time long slowly, and the effective ingredient impurity that obtains simultaneously is too much, excessive velocities can cause separates not exclusively, and the dried cream amount that obtains is very few; So the inventor investigates the percolation speed in the percolation technology, optimized preparation technology, make extraction conditions more perfect, in addition owing to preparation acrid in the mouth of the present invention, hardship, the patient is difficult to take, so tablet of the present invention adopts film-coated technique, beautifies outward appearance, make the patient be easy to accept, conveniently take;

The inventor also furthers investigate the method for quality control of gold silver Radix Notoginseng oral formulations, in Folium Ginkgo extract in the content assaying method of total flavonoids, increase the link of chloroform decontamination in the preparation method of test sample, optimized the content assaying method of total flavonoids in the Folium Ginkgo extract; In addition, in the discrimination method of pseudo-ginseng, reference substance adopts ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1, and adopt the method for n-butyl alcohol supersound extraction to prepare need testing solution, improved discriminating to pseudo-ginseng, improve the quality control standard of gold silver Radix Notoginseng oral formulations, thereby guaranteed the clinical efficacy of said preparation.

Gold silver notoginseng preparations of the present invention is to constitute like this: calculate according to weight: it is prepared from by Folium Ginkgo extract 20-80, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 50-200, Radix Notoginseng 50-200, Radix Salviae Miltiorrhizae 50-200, Rhizoma Chuanxiong 50-200, Olibanum 25-100, artificial Moschus 5-20, Borneolum Syntheticum 12.5-50 and adjuvant.

Gold silver notoginseng preparations of the present invention is preparation like this: above eight flavor medical materials, get the Borneolum Syntheticum porphyrize, and frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong are ground into coarse powder, according to the percolation under Chinese Pharmacopoeia extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 12-48 hour, percolation speed is 5-7ml/min, collect percolate, reclaim ethanol, concentrating under reduced pressure is dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract and adjuvant, mixing is made different preparations according to conventional method again.

Gold silver Radix Notoginseng Tabellae of the present invention is preparation like this: above eight flavor medical materials, get the Borneolum Syntheticum porphyrize, and frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong are ground into coarse powder, according to the percolation under Chinese Pharmacopoeia extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 12-48 hour, percolation speed is 5-7ml/min, collect percolate, reclaim ethanol, concentrating under reduced pressure, be dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract and adjuvant, mixing is used the 70-95% alcohol granulation, drying, tabletting, coating, promptly.

Gold silver notoginseng capsule of the present invention is preparation like this: above eight flavor medical materials, get the Borneolum Syntheticum porphyrize, and frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong are ground into coarse powder, according to the percolation under Chinese Pharmacopoeia extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 12-48 hour, percolation speed is 5-7ml/min, collect percolate, reclaim ethanol, concentrating under reduced pressure, be dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract, add magnesium stearate, starch again, mixing incapsulates, promptly.

When the present invention made tablet, described adjuvant was total medicated powder amount 6-12% starch, 6-10% microcrystalline Cellulose and 0.5-1% magnesium stearate;

Be specially 9% starch, 8% microcrystalline Cellulose and 1% magnesium stearate;

Described adjuvant can also be total medicated powder amount 15-25% starch and 0.5-1% magnesium stearate;

Be specially 18% starch, 1% magnesium stearate.

Method of quality control of the present invention mainly comprise in character, discriminating, inspection and the assay project partly or entirely; Wherein differentiate the feature discriminating that comprises contained Folium Ginkgo extract, Radix Notoginseng, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Borneolum Syntheticum composition in the preparation; Assay is the assay to the contained total flavonoids of Folium Ginkgo extract in the preparation.

Discrimination method comprises the part or all of of following project:

(1) get tablet, capsule respectively, porphyrize adds methanol, supersound process, centrifugal, incline and get supernatant, medicinal residues are handled with method again, merge methanol extract liquid, evaporate to dryness, residue are dissolved in water and mixing, are added on the polyamide pillar of having handled well, the water eluting is collected water lotion, extracts with the ethyl acetate jolting, merge ethyl acetate liquid, water washing discards water liquid, ethyl acetate liquid evaporate to dryness, residue adds methanol makes dissolving, as need testing solution.Other gets the Folium Ginkgo control medicinal material, shines medical material solution in pairs with legal system.Test according to the Chinese Pharmacopoeia thin layer chromatography.Draw above-mentioned two kinds of solution, put respectively on same silica gel H lamellae, with toluene: ethyl acetate: acetone: methanol=1-10: 1-10: 1-10: 0.1-1 is developing solvent, launch, take out, dry up, after smoking with the acetic anhydride steam, 140-170 ℃ of heating put under the ultra-violet lamp (200-500nm) and inspected.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

(2) get tablet, capsule respectively, porphyrize adds an amount of moistening of water, adds water-saturated n-butanol, and supersound process filters, and filtrate adds the saturated water washing of n-butyl alcohol, gets the n-butanol extracting liquid evaporate to dryness, and residue adds methanol makes dissolving, as need testing solution.It is an amount of that other gets ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1 reference substance, adds methanol and make mixed solution, in contrast product solution; Get the Radix Notoginseng control medicinal material, press the compound method of need testing solution, make control medicinal material solution.Test according to the Chinese Pharmacopoeia thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same with silica gel g thin-layer plate on, with n-butyl alcohol: the upper solution of ethyl acetate: water=1-10: 1-10: 10-1 is developing solvent, launch, take out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 100-110 ℃.In the test sample chromatograph with the corresponding position of control medicinal material chromatograph on show the same color speckle.

(3) get tablet, capsule respectively, porphyrize adds ethanol, and jolting is extracted, and filters, filtrate evaporate to dryness, residue add sulfuric acid solution makes dissolving, filters, and filtrate is regulated pH value with strong ammonia solution, adds the chloroform jolting and extracts, combined chloroform liquid, evaporate to dryness, residue add chloroform makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, adds the chloroform dissolving, in contrast product solution.Test according to the Chinese Pharmacopoeia thin layer chromatography.Drawing above-mentioned need testing solution, reference substance solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene: methanol=10-1: 1-10, launches, and takes out, and dries, and spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color.

(4) get tablet, capsule respectively, porphyrize is put in the evaporating dish, and loam cake glass surface ware heats in hot bath, gets the white crystals sublimate that adheres on the glass surface ware, makes dissolving with ethyl acetate, as need testing solution.Other gets the Borneolum Syntheticum reference substance, adds the ethyl acetate dissolving, in contrast product solution.According to the test of Chinese Pharmacopoeia thin layer chromatography, draw above-mentioned two kinds of solution, put respectively on same silica gel G plate, with petroleum ether (60～90 ℃): ethyl acetate=10-1: 1-10 is developing solvent, launches, and takes out, dry, spray is with phosphomolybdic acid ethanol solution, and it is clear to be heated to speckle colour developing at 100-110 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

Concrete discrimination method comprises the part or all of of following project:

(1) gets tablet respectively, capsule 1-3g, porphyrize adds methanol 10-40ml, supersound process 5-30 minute, centrifugal, incline and get supernatant, medicinal residues are handled 1-3 time with method again, merge methanol extract liquid, evaporate to dryness, residue adds water 10-30ml dissolving and mixing, is added in the polyamide pillar (60～80 orders, the internal diameter 1cm that have handled well, long 15cm, wet method dress post) on, water 100-300ml eluting is collected water lotion, extract 2-5 time (20-80ml) with the ethyl acetate jolting, merge ethyl acetate liquid, water washing 1-3 time, each 20-60ml, discard water liquid, ethyl acetate liquid evaporate to dryness, residue add methanol 0.5-2ml makes dissolving, as need testing solution.Other gets the Folium Ginkgo control medicinal material, shines medical material solution in pairs with legal system.Test according to the Chinese Pharmacopoeia thin layer chromatography.Draw each 2-20 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel H lamellae of adhesive preparation with the carboxymethylcellulose sodium solution that contains 4% sodium acetate, with toluene: ethyl acetate: acetone: methanol=1-10: 1-10: 1-10: 0.1-1 is developing solvent, launch, take out, dry up, smoke 10-30 minute with the acetic anhydride steam after, put 160 ℃ of heating 20-40 minute, put under the ultra-violet lamp (200-500nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

(2) get tablet, capsule 1-3g respectively, porphyrize, add an amount of moistening of water, add water-saturated n-butanol 20-80ml, supersound process 10-30 minute, filter, filtrate adds the saturated water washing of n-butyl alcohol that 2-5 doubly measures, get the n-butanol extracting liquid evaporate to dryness, residue adds methanol 0.5-2ml makes dissolving, as need testing solution.It is an amount of that other gets ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1 reference substance, adds methanol and make the mixed solution that every 1ml contains 1-5mg, in contrast product solution; Get Radix Notoginseng control medicinal material 1-3g, the compound method of pressing need testing solution is made control medicinal material solution.Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 5-20 μ l of above-mentioned two kinds of solution, put respectively in same with silica gel g thin-layer plate on, with n-butyl alcohol: the upper solution of ethyl acetate: water=1-10: 1-10: 10-1 is developing solvent, launch, take out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 100-110 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the same color speckle.

(3) get tablet, capsule 1-5g respectively, porphyrize adds ethanol 10-60ml, jolting was extracted 10-30 minute, filtered the filtrate evaporate to dryness, residue adds 5% sulfuric acid solution 10-30ml makes dissolving, filters, and filtrate is regulated pH value to 9～10 with strong ammonia solution, adding the chloroform jolting extracts 1-3 time, each 10-30ml, combined chloroform liquid, evaporate to dryness, residue adds chloroform 0.5-2ml makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, and chlorination is copied into the solution that every 1ml contains 0.5-2mg, in contrast product solution.Test according to the Chinese Pharmacopoeia thin layer chromatography.Draw above-mentioned need testing solution 5-20 μ l, reference substance solution 1-5 μ l, putting in the sodium carboxymethyl cellulose of same usefulness 0.5% sodium hydroxide solution preparation respectively is on the silica gel g thin-layer plate of adhesive, with toluene: methanol=10-1: 1-10 is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color.

(4) get tablet, capsule 1-3g respectively, porphyrize is put in the evaporating dish, and loam cake glass surface ware heated in hot bath 3～12 minutes, got the white crystals sublimate that adheres on the glass surface ware, and 0.5-2ml makes dissolving with ethyl acetate, as need testing solution.Other gets the Borneolum Syntheticum reference substance, adds ethyl acetate and makes the solution that every 1ml contains 0.1-1mg, in contrast product solution.Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 2-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel G plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃): ethyl acetate=10-1: 1-10 is developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 100-110 ℃.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color;

The content assaying method of total flavonoids is: according to high effective liquid chromatography for measuring.Chromatographic column is C18 or C4 or C8 post, and with methanol: 0.4% phosphoric acid=10-90: 90-10 is a mobile phase; The detection wavelength is 200-500nm; Number of theoretical plate calculates by the total flavonoids peak should be not less than 1800.It is an amount of to get Quercetin, kaempferol, isorhamnetin reference substance, accurately claims surely, adds dissolve with methanol and makes mixed solution, in contrast product solution; Get capsule, tablet under the content uniformity item, porphyrize is put in the tool plug conical flask, adds chloroform, supersound process filters, and discards chloroform solution, the accurate methanol that adds of medicinal residues, claim decide weight, supersound process is put coldly, and weight decided in title again, supply with methanol and to subtract weight loss, shake up, filter, precision is measured subsequent filtrate, add methanol and hydrochloric acid, reflux is put coldly, is transferred in the measuring bottle, add methanol and be diluted to scale, shake up, filter, promptly get need testing solution with microporous filter membrane; Accurate respectively reference substance solution and the need testing solution drawn injects hplc determination content.

In the said preparation, contain the Folium Ginkgo extract in the capsule, must not be less than and contain the Folium Ginkgo extract in 25.0mg/g, the tablet, must not be less than 20.0mg/g in total flavonoids in total flavonoids.

Concrete content assaying method is: according to high effective liquid chromatography for measuring.Chromatographic column is C18 or C4 or C8 post, and with methanol: 0.4% phosphoric acid=10-90: 90-10 is a mobile phase; The detection wavelength is 200-500nm; Number of theoretical plate calculates by the total flavonoids peak should be not less than 1800.It is an amount of that precision takes by weighing Quercetin, kaempferol, isorhamnetin reference substance, adds dissolve with methanol and make the mixed solution that every 1ml contains Quercetin 90-150 μ g, kaempferol 90-150 μ g, isorhamnetin 80-120 μ g, shakes up and promptly get reference substance solution; Get the capsule under the content uniformity item, tablet, porphyrize is got the about 2.0g of fine powder, put in the tool plug conical flask, add chloroform 10-30ml, supersound process 20-40 minute, filter, discard chloroform solution, the accurate methanol 10-30ml that adds of medicinal residues, claim to decide weight, supersound process 20-40 minute, put cold, weight decided in title again, supplies with methanol to subtract weight loss, shakes up, filter, precision is measured subsequent filtrate 5-20ml, adds methanol 5-20ml and 5% hydrochloric acid 1-10ml, reflux 20-50 minute, put cold, be transferred in the 50-100ml measuring bottle, add methanol and be diluted to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly get need testing solution; Accurate respectively reference substance solution and each 5-20 μ l of need testing solution of drawing injects chromatograph of liquid, measures content.

Method of quality control of the present invention comprises:

Character observed comprises:

For tablet: this product is a Film coated tablets, shows yellowish-brown to brown after removing coating; Gas fragrance, acrid in the mouth, hardship, little puckery;

For capsule: this product is a capsule, and content is the granule of yellowish-brown to brown; Gas fragrance, acrid in the mouth, hardship, little puckery; Described discrimination method is selected from one or more in the following method:

Official method inspection comprises:

Tablet of the present invention, capsule should meet Chinese Pharmacopoeia about the pertinent regulations under capsule, the tablet item.The total flavonoids that contains is carried out assay be may further comprise the steps:

Total flavonoids is according to high effective liquid chromatography for measuring.Chromatographic column is C18 or C4 or C8 post, and with methanol: 0.4% phosphoric acid=10-90: 90-10 is a mobile phase; The detection wavelength is 200-500nm; Number of theoretical plate calculates by the total flavonoids peak should be not less than 1800.It is an amount of to get Quercetin, kaempferol, isorhamnetin reference substance, accurately claims surely, adds dissolve with methanol and makes mixed solution, in contrast product solution; Get capsule, tablet under the content uniformity item, porphyrize is put in the tool plug conical flask, adds chloroform, supersound process filters, and discards chloroform solution, the accurate methanol that adds of medicinal residues, claim decide weight, supersound process is put coldly, and weight decided in title again, supply with methanol and to subtract weight loss, shake up, filter, precision is measured subsequent filtrate, add methanol and hydrochloric acid, reflux is put coldly, is transferred in the measuring bottle, add methanol and be diluted to scale, shake up, filter, promptly get need testing solution with microporous filter membrane; Accurate respectively reference substance solution and the need testing solution drawn injects hplc determination content.In the said preparation, contain the Folium Ginkgo extract in the capsule, must not be less than and contain the Folium Ginkgo extract in 25.0mg/g, the tablet, must not be less than 20.0mg/g in total flavonoids in total flavonoids.

The applicant finds after deliberation, adopts the quality of following method of quality control with this gold silver Radix Notoginseng of easier control oral formulations, is more conducive to guarantee the clinical efficacy of preparation.So described method of quality control also can comprise:

Character observed comprises:

(4) get tablet, capsule 1-3g respectively, porphyrize is put in the evaporating dish, and loam cake glass surface ware heated in hot bath 3～12 minutes, got the white crystals sublimate that adheres on the glass surface ware, and 0.5-2ml makes dissolving with ethyl acetate, as need testing solution.Other gets the Borneolum Syntheticum reference substance, adds ethyl acetate and makes the solution that every 1ml contains 0.1-1mg, in contrast product solution.Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 2-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel G plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃): ethyl acetate=10-1: 1-10 is developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 100-110 ℃.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color.

Official method inspection comprises:

Total flavonoids is according to high effective liquid chromatography for measuring.Chromatographic column is C18 or C4 or C8 post, and with methanol: 0.4% phosphoric acid=10-90: 90-10 is a mobile phase; The detection wavelength is 200-500nm; Number of theoretical plate calculates by the total flavonoids peak should be not less than 1800.It is an amount of that precision takes by weighing Quercetin, kaempferol, isorhamnetin reference substance, adds dissolve with methanol and make the mixed solution that every 1ml contains Quercetin 90-150 μ g, kaempferol 90-150 μ g, isorhamnetin 80-120 μ g, shakes up and promptly get reference substance solution; Get the capsule under the content uniformity item, tablet, porphyrize is got the about 2.0g of fine powder, put in the tool plug conical flask, add chloroform 10-30ml, supersound process 20-40 minute, filter, discard chloroform solution, the accurate methanol 10-30ml that adds of medicinal residues, claim to decide weight, supersound process 20-40 minute, put cold, weight decided in title again, supplies with methanol to subtract weight loss, shakes up, filter, precision is measured subsequent filtrate 5-20ml, adds methanol 5-20ml and 5% hydrochloric acid 1-10ml, reflux 20-50 minute, put cold, be transferred in the 50-100ml measuring bottle, add methanol and be diluted to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly get need testing solution; Accurate respectively reference substance solution and each 5-20 μ l of need testing solution of drawing injects chromatograph of liquid, measures content.In the said preparation, contain the Folium Ginkgo extract in the capsule, must not be less than and contain the Folium Ginkgo extract in 25.0mg/g, the tablet, must not be less than 20.0mg/g in total flavonoids in total flavonoids.

The invention provides the selection and the quality standard research of percolation technical study and adjuvant in the preparation method:

Experimental example 1 of the present invention: percolation technical study

Solvent for use, dip time, percolation speed and percolate collecting amount all are to influence the percolation process factors in the percolation technology, below are percolation technology is investigated experiment.

1, sample preparation: take by weighing medical material, according to technology of the present invention with Diluted Alcohol dipping 24-48 hour after, with the speed of 2--10ml/min percolation slowly, collect percolate respectively, concentrate.

2, serve as that the result is as follows with reference to the influence of reaction percolation speed to percolation technology with dried cream amount.

Percolation speed investigation table

Flow velocity (ml/min)	Collect percolate (ml)	Dried cream amount (g)
Flow velocity (ml/min)	Collect percolate (ml)	Dried cream amount (g)	2	2500	141
3	2500	134	2	2500	141
3	2500	134	4	2500	126
5	2500	119	4	2500	126
5	2500	119	6	2500	112
7	2500	103	6	2500	112
7	2500	103	8	2500	90
9	2500	76	8	2500	90
9	2500	76	10	2500	59

As seen from the above table: when flow velocity is that the impurity that too much contains of the 2-4ml/min amount of getting dry extract is more, when flow velocity is that the 8-10ml/minn amount of getting dry extract is very few, when flow velocity is that the 5-7ml/min amount of getting dry extract is the requirement that 112g meets preparation, be 5-7ml/min so we select the flow velocity of percolation.

Experimental example 2 of the present invention: the screening study of additive of tablet

When the present invention is tablet,, select different auxiliary material for use, design several prescriptions and investigate according to the character of material, with the compressibility of improving material, increase the flowability of material, phenomenon such as prevent that sticking, pine in the tabletting process from splitting.

1, drug powder preparation: take by weighing Folium Ginkgo extract 40g, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 100g, Radix Notoginseng 100g, Radix Salviae Miltiorrhizae 100g, Rhizoma Chuanxiong 100g, Olibanum 50g, artificial Moschus 10g, Borneolum Syntheticum 25g, technology is: get the Borneolum Syntheticum porphyrize, frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong are ground into coarse powder, according to the percolation under Chinese Pharmacopoeia extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 24 hours, percolation speed is 6ml/min, collect the about 2500ml of percolate, reclaim ethanol, concentrating under reduced pressure is dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract, mixing, promptly.

2, adjuvant: with pregelatinized Starch, starch, lactose, mannitol, sorbitol, dextrin, microcrystalline Cellulose, sucrose single variety or different proportion mixed diluent; Be mixed into disintegrating agent with starch, carboxymethyl starch sodium, low-substituted hydroxypropyl cellulose, cross-linking sodium carboxymethyl cellulose single variety or different proportion;

3, with the outward appearance of tablet, disintegration, hardness as index, investigate the influence of adjuvant to the tablet molding.Owing to contain the Borneolum Syntheticum medical material in the medicine, for guaranteeing a constituent content, be difficult for adopting the method for heating to granulate, the powder behind the thing mixing of therefore getting it filled carries out the direct compression test;

Investigation is the result show, with pregelatinized Starch, starch, microcrystalline Cellulose is diluent and disintegrating agent, the compression molding effect is better, the outward appearance of tablet, disintegration, hardness all meet the Chinese Pharmacopoeia pertinent regulations, because starch property is stable and low price, consider production cost, first-selected starch and microcrystalline Cellulose are as main adjuvant; For making this product tablet forming technique further perfect, make tablet forming technique more easy to operate, controlled, the flowability of this product is investigated.

4, be lubricant with magnesium stearate, micropowder silica gel, Pulvis Talci; The results are shown in following table;

The adjuvant screening study

	Drug powder	Starch	Microcrystalline Cellulose	Magnesium stearate	Micropowder silica gel	Pulvis Talci	Tablet appearance	Hardness (kg)	Disintegration
	Drug powder	Starch	Microcrystalline Cellulose	Magnesium stearate	Micropowder silica gel	Pulvis Talci	Tablet appearance	Hardness (kg)	Disintegration	Prescription 1	83g	9g	8g	1g		-	Smooth	4.5	14min
Prescription 2	83g	9g	8g	-	0.2g	-	Smooth	4.7	13min	Prescription 1	83g	9g	8g	1g		-	Smooth	4.5	14min
Prescription 2	83g	9g	8g	-	0.2g	-	Smooth	4.7	13min	Prescription 3	83g	9g	8g	-	-	1g	The pine sheet	3.2	22min

The result shows, system of selection 1,2 preparation samples, and the outward appearance of tablet, hardness, disintegration all can meet the requirements, but the micropowder silica gel price is more expensive, is not suitable for big production, uses extensive inadequately, so select magnesium stearate as lubricant, the concrete consumption of adjuvant investigated to determine its scope.

The selection 1 of supplementary product consumption

	Drug powder	Starch	Microcrystalline Cellulose	Magnesium stearate	Tablet appearance	Disintegration (branch)	Hardness (kg)
	Drug powder	Starch	Microcrystalline Cellulose	Magnesium stearate	Tablet appearance	Disintegration (branch)	Hardness (kg)	Prescription 1	90	5	5	0.5	Coarse	44	3.0
Prescription 2	90	5	5	1	Coarse	37	3.6	Prescription 1	90	5	5	0.5	Coarse	44	3.0
Prescription 2	90	5	5	1	Coarse	37	3.6	Prescription 3	85	10	5	0.5	Smooth	20	3.1
Prescription 4	85	8	7	1	Smooth	18	4.0	Prescription 3	85	10	5	0.5	Smooth	20	3.1
Prescription 4	85	8	7	1	Smooth	18	4.0	Prescription 5	83	9	8	0.5	Smooth	14	4.5
Prescription 6	80	12	8	1	Smooth	17	4.2	Prescription 5	83	9	8	0.5	Smooth	14	4.5
Prescription 6	80	12	8	1	Smooth	17	4.2	Prescription 7	75	15	10	0.5	Slight sliver	21	4.7
Prescription 8	75	13	12	1	The pine sheet	20	4.0	Prescription 7	75	15	10	0.5	Slight sliver	21	4.7
Prescription 8	75	13	12	1	The pine sheet	20	4.0	Prescription 9	70	16	14	1	The pine sheet	46	4.5

By integrated survey, select drug powder and starch 6-12%, microcrystalline Cellulose 6-10% mixing, the outward appearance of gained tablet, disintegration, hardness are all better, and optimum adjuvant is: starch 9%, microcrystalline Cellulose 8%.To use the 70-95% alcohol granulation behind adjuvant and the drug powder mixing, drying adds the 0.5-1% magnesium stearate again, mixing, and tabletting, coating, promptly.

The selection 2 of supplementary product consumption

	Drug powder	Starch	Magnesium stearate	Tablet appearance	Disintegration (branch)	Hardness (kg)
	Drug powder	Starch	Magnesium stearate	Tablet appearance	Disintegration (branch)	Hardness (kg)	Prescription 1	95	5	1	Coarse	54	3.0
Prescription 2	90	10	1	Coarse	47	3.6	Prescription 1	95	5	1	Coarse	54	3.0

Prescription 3	85	15	1	Smooth	22	4.3
Prescription 3	85	15	1	Smooth	22	4.3	Prescription 4	82	18	1	Smooth	18	4.7
Prescription 5	80	20	1	Smooth	20	4.2	Prescription 4	82	18	1	Smooth	18	4.7
Prescription 5	80	20	1	Smooth	20	4.2	Prescription 6	75	25	1	Smooth	24	3.4
Prescription 7	70	30	1	The pine sheet	30	3.8	Prescription 6	75	25	1	Smooth	24	3.4

Test shows, selects drug powder and starch 15-25% mixing, and the outward appearance of gained tablet, disintegration, hardness are all better, and optimum adjuvant is: starch 18%.To use the 70-95% alcohol granulation behind adjuvant and the drug powder mixing, drying adds the 0.5-1% magnesium stearate again, mixing, and tabletting, coating, promptly.

Experimental example 3 of the present invention: total flavonoids content assaying method research

1, need testing solution preparation method research:

Need testing solution preparation method one: get tablet, capsule fine powder, the accurate title, decide, the accurate methanol that adds, supersound process filters, and precision is got subsequent filtrate, add methanol, add 4% sulfuric acid solution again, put in the flask, reflux is put coldly, is transferred in the measuring bottle, add methanol and be diluted to scale, shake up, filter, promptly.

Need testing solution preparation method two: get tablet, capsule fine powder, the accurate title, decide, and puts in the tool plug conical flask, adds chloroform, supersound process filters, and discards chloroform solution, the accurate methanol that adds of medicinal residues, claim decide weight, supersound process is put coldly, and weight decided in title again, supply with methanol and to subtract weight loss, shake up, filter, precision is measured subsequent filtrate, add methanol and 5% hydrochloric acid, reflux is put coldly, is transferred in the measuring bottle, add methanol and be diluted to scale, shake up, microporous filter membrane filters, promptly.

Need testing solution preparation method three: get tablet, capsule fine powder, the accurate title, decide, and puts in the tool plug conical flask, adds diethyl ether, supersound process filters, and discards ether solution, the accurate methanol that adds of medicinal residues, supersound process filters, precision is measured subsequent filtrate, adds methanol and 5% hydrochloric acid, reflux, put coldly, be transferred in the measuring bottle, add methanol and be diluted to scale, shake up, microporous filter membrane filters, promptly.

Sample	Method 1 (mg/g)	Method 2 (mg/g)	Method 3 (mg/g)
Sample	Method 1 (mg/g)	Method 2 (mg/g)	Method 3 (mg/g)	1	48.7	53.6	50.3
2	50.0	55.0	52.1	1	48.7	53.6	50.3
2	50.0	55.0	52.1	3	52.3	56.3	53.5

According to result of the test as can be known, adopt method two to prepare need testing solution, remove impurity earlier with the chloroform ultrasonic processing method, Folium Ginkgo extract extracts more complete, and extraction effect is good, and sample main peak and impurity peaks separating effect are better, are easy to detect.Employing method one is extracted, and impurity peaks is more, and repeatability is bad, is difficult for detecting and control this product content.

2, reference substance solution is selected research:

Reference substance solution preparation method one: it is an amount of that precision takes by weighing the plain reference substance of Quercetin, adds dissolve with methanol, shakes up, promptly.

Reference substance solution preparation method two: it is an amount of that precision takes by weighing Quercetin, kaempferol, isorhamnetin reference substance, adds dissolve with methanol and make mixed solution, shakes up, promptly.

The selection result of reference substance solution shows: adopt method two promptly to adopt Quercetin reference substance, kaempferol reference substance and isorhamnetin reference substance mixed solution in contrast, the peak position of explanation Quercetin, kaempferol and isorhamnetin that more can be definite is easy to detect.

3, the selection of mobile phase:

Mobile phase 1 is mobile phase with the mixed solution of methanol and acetic acid different proportion.

Mobile phase 2 is mobile phase with the mixed solution of acetonitrile and acetic acid different proportion.

Mobile phase 3 is mobile phase with the mixed solution of methanol, 0.4% phosphoric acid different proportion.

Mobile phase 4 is mobile phase with the mixed solution of methanol, acetonitrile and water different proportion.

Result: with methanol: 0.4% phosphoric acid=10-90: 90-10 is a mobile phase; The negative sample chromatogram is at corresponding Quercetin, kaempferol, non-false positive peak, isorhamnetin position, Quercetin, kaempferol, isorhamnetin and close impurity peaks separate fully (separating degree＞1.5), and promptly Quercetin, kaempferol, isorhamnetin separate with other components fully under this condition.Optimal flow is mutually: methanol: 0.4% phosphoric acid=45: 55.

4, repeated experiment:

Get tablet or capsule, by 6 parts of test liquids of preparation method preparation of test liquid under the method for quality control assay item of the present invention, sample introduction is measured peak area, and result of calculation is listed following table in, and the total flavonoids average content is 16.5mg/g, and RSD is 1.9%.

Replica test

The sample introduction number of times	1	2	3	4	5	6	Meansigma methods	RSD(％)
The sample introduction number of times	1	2	3	4	5	6	Meansigma methods	RSD(％)	Sample size (g)	2.0036	2.0006	2.0069	2.0072	1.9998	2.0207	55.0	1.9
Content (mg/g)	55.7	56.3	53.7	55.0	55.7	54.0			Sample size (g)	2.0036	2.0006	2.0069	2.0072	1.9998	2.0207

According to the result as can be known, this method repeatability is good.

5, stability experiment:

Get tablet or capsule, prepare test liquid, the stability of this need testing solution is investigated, measured once respectively at 0,2,4,6,8 hour by the preparation method of test liquid under the method for quality control assay item of the present invention.The results are shown in following table.

The stability test of preparation test sample

Time (hour)	0	2	4	6	8
Time (hour)	0	2	4	6	8	The Quercetin peak area	934718	913677	901450	922929	906010
Meansigma methods	915757					The Quercetin peak area	934718	913677	901450	922929	906010
Meansigma methods	915757					RSD(％)	1.5
The kaempferol peak area	912631	893605	890870	913447	890250	RSD(％)	1.5
The kaempferol peak area	912631	893605	890870	913447	890250	Meansigma methods	900161
RSD(％)	1.3					Meansigma methods	900161
RSD(％)	1.3					The isorhamnetin peak area	196524	199739	200570	195232	198652
Meansigma methods	198143					The isorhamnetin peak area	196524	199739	200570	195232	198652
Meansigma methods	198143					RSD(％)	1.1

As seen from the above table: sample measurement result in 8 hours is basicly stable.The result meets the requirements.

6, response rate experiment:

Adopt the application of sample absorption method, precision takes by weighing 6 parts in sample measuring content (containing Quercetin 9.957mg/g, kaempferol 9.690mg/g, isorhamnetin 2.08mg/g), add Quercetin reference substance, kaempferol reference substance and isorhamnetin reference substance respectively, by method operation under the method for quality control assay item of the present invention, calculate recovery rate.

Recovery test

Sample	1	2	3	4	5	6
Sample	1	2	3	4	5	6	Sample volume (g)	1.0962	0.9569	1.0928	0.9407	0.9665	0.9581
Sample Quercetin amount (mg)	10.6103	9.2620	10.5774	9.1052	9.3549	9.2736	Sample volume (g)	1.0962	0.9569	1.0928	0.9407	0.9665	0.9581
Sample Quercetin amount (mg)	10.6103	9.2620	10.5774	9.1052	9.3549	9.2736	Reference substance addition (mg)	10.79	11.01	10.85	11.05	10.88	11.05
Actual measurement content (mg)	21.3922	20.4739	21.2889	20.1805	20.3708	20.2224	Reference substance addition (mg)	10.79	11.01	10.85	11.05	10.88	11.05
Actual measurement content (mg)	21.3922	20.4739	21.2889	20.1805	20.3708	20.2224	The response rate (%)	99.92	101.83	98.72	100.23	101.25	99.08
Average same yield (%)	100.17						The response rate (%)	99.92	101.83	98.72	100.23	101.25	99.08
Average same yield (%)	100.17						RSD％	1.2
Kaempferol amount (mg) in the sample	10.3262	9.0140	10.2941	8.8614	9.1044	9.0253	RSD％	1.2
Kaempferol amount (mg) in the sample	10.3262	9.0140	10.2941	8.8614	9.1044	9.0253	Reference substance addition (mg)	11.14	11.15	11.50	11.36	11.23	11.55
Actual measurement content (mg)	21.5710	20.4149	22.0130	20.6220	20.4987	20.4293	Reference substance addition (mg)	11.14	11.15	11.50	11.36	11.23	11.55
Actual measurement content (mg)	21.5710	20.4149	22.0130	20.6220	20.4987	20.4293	The response rate (%)	100.94	102.25	101.90	103.53	101.46	98.74
Average recovery rate (%)	101.47						The response rate (%)	100.94	102.25	101.90	103.53	101.46	98.74
Average recovery rate (%)	101.47						RSD％	1.6
Isorhamnetin amount (mg) in the sample	2.2166	1.9349	2.2097	1.9021	1.9543	1.9373	RSD％	1.6
Isorhamnetin amount (mg) in the sample	2.2166	1.9349	2.2097	1.9021	1.9543	1.9373	Reference substance addition (mg)	2.72	2.72	2.72	2.72	2.72	2.72
Actual measurement content (mg)	4.8933	4.6532	4.8927	4.5230	4.5403	4.6446	Reference substance addition (mg)	2.72	2.72	2.72	2.72	2.72	2.72
Actual measurement content (mg)	4.8933	4.6532	4.8927	4.5230	4.5403	4.6446	The response rate (%)	98.41	99.94	98.64	96.36	95.07	99.53
Average same yield (%)	97.99						The response rate (%)	98.41	99.94	98.64	96.36	95.07	99.53
Average same yield (%)	97.99						RSD％	1.9

Experimental example 4 of the present invention: Folium Ginkgo extract thin layer Study on Identification

Differentiate Folium Ginkgo extract in the preparation with the Folium Ginkgo control medicinal material

Need testing solution preparation method one: get tablet or capsule, porphyrize adds methanol, supersound process, centrifugal, incline and get supernatant, medicinal residues are handled with method again, merge methanol extract liquid, evaporate to dryness, residue are dissolved in water and mixing, are added on the polyamide pillar of having handled well, the water eluting is collected water lotion, extracts with the ethyl acetate jolting, merge ethyl acetate liquid, water washing discards water liquid, ethyl acetate liquid evaporate to dryness, residue adds methanol makes dissolving, lacks the negative test liquid of Folium Ginkgo extract with the method preparation.

Need testing solution preparation method two: get tablet or capsule, porphyrize adds acetone, reflux is put coldly, filters, filtrate boils off acetone, puts coldly, adds 15% dissolve with ethanol, be added on the polyamide column, use 5% ethanol elution, collect water lotion, extract twice with the ethyl acetate jolting, merge extractive liquid,, evaporate to dryness, residue adds acetone makes dissolving, lacks the negative test liquid of Folium Ginkgo extract with the method preparation.

Developing solvent is selected: respectively with the mixed solution of toluene, ethyl acetate, acetone, methanol different proportion; The mixed solution of acetonitrile, ethyl acetate, water different proportion; The mixed solution of chloroform, methanol, acetone different proportion is developing solvent.

The result: employing method one preparation need testing solution, with toluene: ethyl acetate: acetone: methanol=1-10: 1-10: 1-10: 0.1-1 is developing solvent, and its separating degree is good, and the speckle colour developing is clear, and separating degree is good, and negative control is noiseless, the method favorable reproducibility.Best developing solvent is: toluene: ethyl acetate: acetone: methanol=5: 2.5: 2.5: 0.3.

Experimental example 5 of the present invention: ginsenoside Rg1, arasaponin R1 and ginsenoside Rb1's thin layer Study on Identification

With ginsenoside Rg1, arasaponin R1, ginsenoside Rb1's reference substance, the Radix Notoginseng control medicinal material is differentiated pseudo-ginseng in the preparation

Need testing solution preparation method one: get tablet or capsule, porphyrize adds 50% alcoholic solution of 8% hydrochloric acid, reflux filters, and filtrate is extracted 2 times with petroleum ether (60-90 ℃), merge petroleum ether liquid, add anhydrous sodium sulfate dehydration, filter, filtrate concentrates, be added on the neutral alumina post of having handled well, use methanol-eluted fractions, the eluent evaporate to dryness, residue adds methanol makes dissolving, lacks the negative test liquid of Radix Notoginseng with the method preparation.

Need testing solution preparation method two: get tablet or capsule, porphyrize adds an amount of moistening of water, adds water-saturated n-butanol liquid, supersound process filters, and filtrate adds the saturated water washing of n-butyl alcohol, get the n-butanol extracting liquid evaporate to dryness, residue adds methanol makes dissolving, lacks the negative test liquid of Radix Notoginseng with the method preparation.

Need testing solution preparation method three: get tablet or capsule, porphyrize adds an amount of moistening of water, adds water-saturated n-butanol liquid, reflux is put coldly, filters, and filtrate adds the saturated water washing of n-butyl alcohol, get the n-butanol extracting liquid evaporate to dryness, residue adds methanol makes dissolving, lacks the negative test liquid of Radix Notoginseng with the method preparation.

The selection of reference substance solution: get panoxadiol, panaxatriol's reference substance respectively, add dissolve with methanol; Get ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1 reference substance, add dissolve with methanol and make mixed solution; Product solution in contrast.

Developing solvent is selected: respectively with the mixed solution of cyclohexane extraction, acetone different proportion; The mixed solution of n-butyl alcohol, ethyl acetate, water different proportion; The mixed solution of chloroform, methanol, water different proportion is developing solvent.

Result: adopt method two to prepare need testing solution, with ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1 product in contrast, with n-butyl alcohol: ethyl acetate: water=1-10: 1-10: 10-1 is developing solvent, its separating degree is good, the speckle colour developing is clear, negative control is noiseless, the method favorable reproducibility.Best developing solvent is: n-butyl alcohol: ethyl acetate: water=4: 1: 5.

Experimental example 6 of the present invention: tetrahydropalmatine thin layer Study on Identification

Differentiate Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) medical material in the preparation with the tetrahydropalmatine reference substance

Need testing solution preparation method one: get tablet or capsule, porphyrize adds ethanol, jolting is extracted, and filters the filtrate evaporate to dryness, residue adds 5% sulfuric acid solution makes dissolving, filter, filtrate is regulated pH value with strong ammonia solution, adds the chloroform jolting and extracts 2 times, combined chloroform liquid, evaporate to dryness, residue add chloroform makes dissolving, lacks the negative test liquid of Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) with the method preparation.

Need testing solution preparation method two: get tablet or capsule, porphyrize adds methanol, supersound extraction filters the filtrate evaporate to dryness, residue adds water makes dissolving, filter, filtrate is regulated pH value with strong ammonia solution, adds diethyl ether to extract 3 times, merge ether solution, evaporate to dryness, residue add methanol makes dissolving, lacks the negative test liquid of Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) with the method preparation.

Developing solvent is selected: respectively with the mixed solution of toluene, ethyl acetate different proportion; The mixed solution of toluene, methanol different proportion; The mixed solution of chloroform, acetonitrile, water different proportion is developing solvent.

The result: employing method one preparation need testing solution is developing solvent with toluene: methanol=10-1: 1-10, and its separating degree is good, and the speckle colour developing is clear, and negative control is noiseless, the method favorable reproducibility.Best developing solvent is: toluene: methanol=10: 1.

Experimental example 7 of the present invention: Borneolum Syntheticum thin layer Study on Identification

Differentiate Borneolum Syntheticum medical material in the preparation with the Borneolum Syntheticum reference substance

Need testing solution preparation method one: get tablet or capsule, porphyrize is put in the evaporating dish, loam cake glass surface ware heats in hot bath, gets the white crystals sublimate that adheres on the glass surface ware, make dissolving with ethyl acetate, lack the negative test liquid of Borneolum Syntheticum with the method preparation.

Need testing solution preparation method two: get tablet or capsule, porphyrize is put in the evaporating dish, loam cake glass surface ware, and the white crystals sublimate that adheres on the glass surface ware is got in straight fire heating, makes dissolving with petroleum ether, lacks the negative test liquid of Borneolum Syntheticum with the method preparation.

Developing solvent is selected: respectively with the mixed solution of petroleum ether, formic acid different proportion; The mixed solution of ethyl acetate, toluene different proportion; The mixed solution of petroleum ether, ethyl acetate different proportion is developing solvent.

The result: employing method one preparation need testing solution, with petroleum ether (60-90 ℃): ethyl acetate=10-1: 1-10 is developing solvent, and its separating degree is good, and the speckle colour developing is clear, and negative control is noiseless, the method favorable reproducibility.Best developing solvent is: petroleum ether (60-90 ℃): ethyl acetate=8: 2.

Compared with prior art, percolation speed in the percolation technology that the present invention is clear and definite, the process for refining parameter makes extraction process more perfect; The present invention takes into full account the preparation tablets factor by adjuvant is selected, the adjuvant that choose stable in properties, compressibility is strong, adhesion is strong, is easy to obtain, and preparation hardness is suitable, all satisfactory preparation of disintegrate, outward appearance; At preparation acrid in the mouth of the present invention, hardship, the shortcoming that the patient is difficult to take, tablet of the present invention adopts film-coated technique, beautifies outward appearance, makes the patient be easy to accept, and conveniently takes; Method of quality control precision height provided by the invention in addition, favorable reproducibility, measurement result is accurate, has improved the quality control standard of gold silver Radix Notoginseng oral formulations, can control product quality effectively, thereby guarantee its clinical efficacy.

The specific embodiment:

Further specify the present invention by the following examples, but not as limitation of the present invention.

Embodiments of the invention 1:

Folium Ginkgo extract 40g, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 100g, Radix Notoginseng 100g, Radix Salviae Miltiorrhizae 100g, Rhizoma Chuanxiong 100g, Olibanum 50g, artificial Moschus 10g, Borneolum Syntheticum 25g.

Get the Borneolum Syntheticum porphyrize, frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong is ground into coarse powder, according to the percolation (2000 editions appendix IO of Chinese Pharmacopoeia) under extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 24 hours, percolation speed is 6ml/min, collect the about 2500ml of percolate, reclaim ethanol, concentrating under reduced pressure is dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract, getting the medicated powder amount is 237g, adds starch 25g, microcrystalline Cellulose 22g, mixing, use 80% alcohol granulation, drying adds magnesium stearate 3g again, mixing, tabletting, coating promptly gets the gold silver Radix Notoginseng Tabellae.

Embodiments of the invention 2:

Get the Borneolum Syntheticum porphyrize, frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong are ground into coarse powder, according to the percolation under Chinese Pharmacopoeia extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 24 hours, percolation speed is 6ml/min, collect the about 2500ml of percolate, reclaim ethanol, concentrating under reduced pressure is dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract, getting the medicated powder amount is 239g, adds starch 53g, mixing, use 80% alcohol granulation, drying adds magnesium stearate 3g again, mixing, tabletting, coating promptly gets the gold silver Radix Notoginseng Tabellae.

Embodiments of the invention 3:

Folium Ginkgo extract 20g, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 50g, Radix Notoginseng 50g, Radix Salviae Miltiorrhizae 50g, Rhizoma Chuanxiong 50g, Olibanum 25g, artificial Moschus 5g, Borneolum Syntheticum 12.5g.

Get the Borneolum Syntheticum porphyrize, frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong is ground into coarse powder, according to the percolation under Chinese Pharmacopoeia extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 24 hours, percolation speed is 6ml/min, collect the about 1250ml of percolate, reclaim ethanol, concentrating under reduced pressure is dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract gets the medicated powder amount and is about 118g, adds starch 8.5g, microcrystalline Cellulose 13.5g, mixing, use 80% alcohol granulation, drying adds magnesium stearate 1.4g again, mixing, tabletting, coating promptly gets the gold silver Radix Notoginseng Tabellae.

Embodiments of the invention 4:

Folium Ginkgo extract 80g, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 200g, Radix Notoginseng 200g, Radix Salviae Miltiorrhizae 200g, Rhizoma Chuanxiong 200g, Olibanum 100g, artificial Moschus 20g, Borneolum Syntheticum 50g.

Get the Borneolum Syntheticum porphyrize, frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong is ground into coarse powder, according to the percolation under Chinese Pharmacopoeia extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 24 hours, percolation speed is 6ml/min, collect the about 5000ml of percolate, reclaim ethanol, concentrating under reduced pressure is dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract, getting the medicated powder amount is 475g, adds starch 68g, microcrystalline Cellulose 35g, mixing, use 80% alcohol granulation, drying adds magnesium stearate 4.8g again, mixing, tabletting, coating promptly gets the gold silver Radix Notoginseng Tabellae.

Embodiments of the invention 5:

Folium Ginkgo extract 30g, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 80g, Radix Notoginseng 80g, Radix Salviae Miltiorrhizae 80g, Rhizoma Chuanxiong 80g, Olibanum 40g, artificial Moschus 8g, Borneolum Syntheticum 20g.

Get the Borneolum Syntheticum porphyrize, frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong are ground into coarse powder, according to the percolation under Chinese Pharmacopoeia extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 24 hours, percolation speed is 6ml/min, collect the about 2000ml of percolate, reclaim ethanol, concentrating under reduced pressure is dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract, getting the medicated powder amount is 200g, adds starch 30g, mixing, use 80% alcohol granulation, drying adds magnesium stearate 2g again, mixing, tabletting, coating promptly gets the gold silver Radix Notoginseng Tabellae.

Embodiments of the invention 6:

Folium Ginkgo extract 60g, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 150g, Radix Notoginseng 150g, Radix Salviae Miltiorrhizae 150g, Rhizoma Chuanxiong 150g, Olibanum 70g, artificial Moschus 15g, Borneolum Syntheticum 40g.

Get the Borneolum Syntheticum porphyrize, frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong are ground into coarse powder, according to the percolation under Chinese Pharmacopoeia extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 24 hours, percolation speed is 6ml/min, collect the about 4000ml of percolate, reclaim ethanol, concentrating under reduced pressure is dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract, getting the medicated powder amount is 380g, adds starch 95g, mixing, use 80% alcohol granulation, drying adds magnesium stearate 2g again, mixing, tabletting, coating promptly gets the gold silver Radix Notoginseng Tabellae.

Embodiments of the invention 7:

Folium Ginkgo extract 20g, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 200g, Radix Notoginseng 200g, Radix Salviae Miltiorrhizae 200g, Rhizoma Chuanxiong 200g, Olibanum 25g, artificial Moschus 20g, Borneolum Syntheticum 50g.

Get the Borneolum Syntheticum porphyrize, frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong are ground into coarse powder, according to the percolation (2000 editions one appendix I O of Chinese Pharmacopoeia) under extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 24 hours, percolation speed is 6ml/min, collect the about 2500ml of percolate, reclaim ethanol, concentrating under reduced pressure, be dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract, add magnesium stearate, starch again, mixing incapsulates, and promptly gets the gold silver notoginseng capsule.

Embodiments of the invention 8: the method for quality control of gold silver notoginseng preparations comprises:

Character: for tablet, this product is a Film coated tablets, removes to show yellowish-brown behind the coating to brown; Gas fragrance, acrid in the mouth, hardship, little puckery;

Differentiate: (1) gets 6 in tablet, and porphyrize adds methanol 20ml, supersound process 15 minutes, centrifugal, incline and get supernatant, medicinal residues are handled 2 times with method again, merge methanol extract liquid, evaporate to dryness, residue adds water 15ml dissolving and mixing, is added in the polyamide pillar (60～80 orders, the internal diameter 1cm that have handled well, long 15cm, wet method dress post) on, water 150ml eluting, collect water lotion, extract 3 (40ml, 30ml with the ethyl acetate jolting, 30ml), merge ethyl acetate liquid, water washing 2 times, each 30ml, discard water liquid, ethyl acetate liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Folium Ginkgo control medicinal material 1.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005).Draw each 8 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel H lamellae of adhesive preparation with the carboxymethylcellulose sodium solution that contains 4% sodium acetate, with toluene-ethyl acetate-acetone-methanol (5: 2.5: 2.5: 0.3) be developing solvent, launch, take out, dry up, smoke 15 minutes with the acetic anhydride steam after, put 160 ℃ of heating 30 minutes, 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.

(2) get 6 in tablet, porphyrize adds an amount of moistening of water, adds water-saturated n-butanol 40ml, and supersound process 15 minutes filters, and filtrate adds the saturated water washing of n-butyl alcohol of 3 times of amounts, gets the n-butanol extracting liquid evaporate to dryness, and residue adds methanol 1ml makes dissolving, as need testing solution.It is an amount of that other gets ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1 reference substance, adds methanol and make the mixed solution that every 1ml contains 2.5mg, in contrast product solution; Get Radix Notoginseng control medicinal material 1.0g, the compound method of pressing need testing solution is made control medicinal material solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same with silica gel g thin-layer plate on, with n-butyl alcohol-ethyl acetate-water (4: 1: 5) upper solution is developing solvent, launch, take out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃.In the test sample chromatograph with the corresponding position of reference substance chromatograph on show the same color speckle.

(3) get 12 in tablet, porphyrize adds ethanol 40ml, jolting was extracted 20 minutes, filtered the filtrate evaporate to dryness, residue adds 5% sulfuric acid solution 15ml makes dissolving, filters, and filtrate is regulated pH value to 9～10 with strong ammonia solution, adding the chloroform jolting extracts 2 times, each 15ml, combined chloroform liquid, evaporate to dryness, residue adds chloroform 1ml makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, and chlorination is copied into the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005).Draw above-mentioned need testing solution 10 μ l, reference substance solution 3 μ l, putting in the sodium carboxymethyl cellulose of same usefulness 0.5% sodium hydroxide solution preparation respectively is on the silica gel g thin-layer plate of adhesive, is developing solvent with toluene-methanol (10: 1), launch, take out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

(4) get 8 in tablet, porphyrize is put in the evaporating dish, and loam cake glass surface ware heated in hot bath 5～10 minutes, got the white crystals sublimate that adheres on the glass surface ware, and 1ml makes dissolving with ethyl acetate, as need testing solution.Other gets the Borneolum Syntheticum reference substance, adds ethyl acetate and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 4 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel G plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃)-ethyl acetate (8: 2) is developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

Check: should meet Chinese Pharmacopoeia about the pertinent regulations under the tablet item.

Assay: schisandrin is according to high effective liquid chromatography for measuring.With the octadecylsilane chemically bonded silica is filler; Methanol: 0.4% phosphoric acid=45: 55 is mobile phase, and the detection wavelength is 370nm.Theoretical cam curve should be not less than 1800 by the cholic acid peak.It is an amount of that precision takes by weighing Quercetin, kaempferide, isorhamnetin reference substance, adds methanol and make the mixed solution that every 1ml contains Quercetin 120 μ g, kaempferide 120 μ g, isorhamnetin 100 μ g, shakes up, and promptly gets reference substance solution; Get 20 in tablet, claim to decide weight, porphyrize, get 2.0g, put in the tool plug conical flask, add chloroform 20ml, supersound process (power 250W, frequency 80KHz) 30 minutes filters, discard chloroform solution, the accurate methanol 20ml that adds of medicinal residues claims to decide weight, supersound process (power 250W, frequency 80KHz) 30 minutes is put cold, weight decided in title again, supplies with methanol to subtract weight loss, shakes up, filter, precision is measured subsequent filtrate 10ml, adds methanol 10ml and 25% hydrochloric acid 5ml, reflux 30 minutes is put coldly, is transferred in the 50ml measuring bottle, add methanol and be diluted to scale, shake up, filter, promptly get need testing solution with 0.45 μ m microporous filter membrane; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure content.Contain the Folium Ginkgo extract in the tablet in total flavonoids, must not be less than 20.0mg/g.

Embodiments of the invention 9: the method for quality control of gold silver notoginseng capsule agent comprises:

Character: for capsule, its content is the granule of yellowish-brown to brown; Gas fragrance, acrid in the mouth, hardship, little puckery;

Differentiate: (1) gets capsule 1g, and porphyrize adds methanol 10ml, supersound process 5 minutes, centrifugal, incline and get supernatant, medicinal residues are handled with method again, merge methanol extract liquid, evaporate to dryness, residue adds water 10ml dissolving and mixing, is added in the polyamide pillar (60～80 orders, the internal diameter 1cm that have handled well, long 15cm, wet method dress post) on, water 100ml eluting is collected water lotion, extract 2 (30ml with the ethyl acetate jolting, 20ml), merge ethyl acetate liquid, use the 20ml water washing, discard water liquid, ethyl acetate liquid evaporate to dryness, residue add methanol 0.5ml makes dissolving, as need testing solution.Other gets Folium Ginkgo control medicinal material 1.5g, shines medical material solution in pairs with legal system.Test according to the Chinese Pharmacopoeia thin layer chromatography.Draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H lamellae, with toluene: ethyl acetate: acetone: methanol=1: 10: 1: 1 is developing solvent, launch, take out, dry up, after smoking 10 minutes with the acetic anhydride steam, put 160 ℃ of heating 20 minutes, put under the ultra-violet lamp (200nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

(2) get capsule 1g, porphyrize adds an amount of moistening of water, adds water-saturated n-butanol 20ml, supersound process 10 minutes filters, and filtrate adds the saturated water washing of n-butyl alcohol of 2 times of amounts, get the n-butanol extracting liquid evaporate to dryness, residue adds methanol 0.5ml makes dissolving, as need testing solution.It is an amount of that other gets ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1 reference substance, adds methanol and make the mixed solution that every 1ml contains 1mg, in contrast product solution; Get Radix Notoginseng control medicinal material 1.0g, the compound method of pressing need testing solution is made control medicinal material solution.Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same with silica gel g thin-layer plate on, with n-butyl alcohol: ethyl acetate: the upper solution of water=1: 10: 1 is developing solvent, launch, take out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 100 ℃.In the test sample chromatograph with the corresponding position of reference substance chromatograph on show the same color speckle.

(3) get capsule 1g, porphyrize adds ethanol 10ml, jolting was extracted 10 minutes, filter, filtrate evaporate to dryness, residue add 5% sulfuric acid solution 10ml makes dissolving, filter, filtrate is regulated pH value to 9～10 with strong ammonia solution, adds the jolting of 10ml chloroform and extracts the extracting solution evaporate to dryness, residue adds chloroform 0.5ml makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, and chlorination is copied into the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to the Chinese Pharmacopoeia thin layer chromatography.Draw above-mentioned need testing solution 5 μ l, reference substance solution 1 μ l, put respectively on same silica gel g thin-layer plate, with toluene: methanol=1: 10 is developing solvent, launches, and takes out, and dries, and spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

(4) get capsule 1g, porphyrize is put in the evaporating dish, and loam cake glass surface ware heated in hot bath 3～10 minutes, got the white crystals sublimate that adheres on the glass surface ware, and 0.5ml makes dissolving with ethyl acetate, as need testing solution.Other gets the Borneolum Syntheticum reference substance, adds ethyl acetate and makes the solution that every 1ml contains 0.1mg, in contrast product solution.Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel G plate, with petroleum ether (60～90 ℃): ethyl acetate=1: 10 is developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 100 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

Check: should meet Chinese Pharmacopoeia about the pertinent regulations under the capsule item.

Assay: schisandrin is according to high effective liquid chromatography for measuring.With the octadecylsilane chemically bonded silica is filler; Methanol: 0.4% phosphoric acid=10: 90 is mobile phase, and the detection wavelength is 200nm.Theoretical cam curve should be not less than 1800 by the cholic acid peak.It is an amount of that precision takes by weighing Quercetin, kaempferide, isorhamnetin reference substance, adds methanol and make the mixed solution that every 1ml contains Quercetin 90 μ g, kaempferide 90 μ g, isorhamnetin 80 μ g, shakes up, and promptly gets reference substance solution; Get 20 of capsules, claim to decide weight, porphyrize, get 2.0g, put in the tool plug conical flask, add chloroform 10ml, supersound process (power 250W, frequency 80KHz) 20 minutes filters, discard chloroform solution, the accurate methanol 10ml that adds of medicinal residues claims to decide weight, supersound process (power 250W, frequency 80KHz) 20 minutes is put cold, weight decided in title again, supplies with methanol to subtract weight loss, shakes up, filter, precision is measured subsequent filtrate 5ml, adds methanol 5ml and 25% hydrochloric acid 1ml, reflux 20 minutes is put coldly, is transferred in the 50ml measuring bottle, add methanol and be diluted to scale, shake up, filter, promptly get need testing solution with 0.45 μ m microporous filter membrane; Accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing inject chromatograph of liquid, measure content.Contain the Folium Ginkgo extract in the capsule in total flavonoids, must not be less than 25.0mg/g.

Embodiments of the invention 10: the method for quality control of gold silver notoginseng preparations of the present invention can comprise:

For tablet, this product is a Film coated tablets, removes to show yellowish-brown behind the coating to brown; Gas fragrance, acrid in the mouth, hardship, little puckery;

For capsule, its content is the granule of yellowish-brown to brown; Gas fragrance, acrid in the mouth, hardship, little puckery;

Differentiate: (1) gets tablet or capsule 3g, and porphyrize adds methanol 40ml, supersound process 15 minutes, centrifugal, incline and get supernatant, medicinal residues are handled 3 times with method again, merge methanol extract liquid, evaporate to dryness, residue adds water 30ml dissolving and mixing, is added in the polyamide pillar (60～80 orders, the internal diameter 1cm that have handled well, long 15cm, wet method dress post) on, water 300ml eluting, collect water lotion, extract 5 (80ml, 60ml with the ethyl acetate jolting, 40ml, 30ml, 30ml), merge ethyl acetate liquid, water washing 3 times, each 60ml, discard water liquid, ethyl acetate liquid evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.Other gets Folium Ginkgo control medicinal material 1.5g, shines medical material solution in pairs with legal system.Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 20 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H lamellae, with toluene: ethyl acetate: acetone: methanol=10: 1: 10: 0.1 is developing solvent, launches, and takes out, dry up, after smoking 30 minutes with the acetic anhydride steam, put 160 ℃ of heating 40 minutes, put under the ultra-violet lamp (500nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

(2) get tablet or capsule 3g, porphyrize adds an amount of moistening of water, adds water-saturated n-butanol 80ml, supersound process 30 minutes filters, and filtrate adds the saturated water washing of n-butyl alcohol of 5 times of amounts, get the n-butanol extracting liquid evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution.It is an amount of that other gets ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1 reference substance, adds methanol and make the mixed solution that every 1ml contains 5mg, in contrast product solution; Get Radix Notoginseng control medicinal material 1.0g, the compound method of pressing need testing solution is made control medicinal material solution.Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 20 μ l of above-mentioned two kinds of solution, put respectively in same with silica gel g thin-layer plate on, with n-butyl alcohol: ethyl acetate: the upper solution of water=10: 1: 10 is developing solvent, launch, take out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 110 ℃.In the test sample chromatograph with the corresponding position of reference substance chromatograph on show the same color speckle.

(3) get tablet or capsule 5g, porphyrize adds ethanol 60ml, jolting was extracted 30 minutes, filtered the filtrate evaporate to dryness, residue adds 5% sulfuric acid solution 30ml makes dissolving, filters, and filtrate is regulated pH value to 9～10 with strong ammonia solution, adding the chloroform jolting extracts 3 times, each 30ml, combined chloroform liquid, evaporate to dryness, residue adds chloroform 2ml makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, and chlorination is copied into the solution that every 1ml contains 2mg, in contrast product solution.According to Chinese Pharmacopoeia thin layer chromatography test, draw above-mentioned need testing solution 20 μ l, reference substance solution 5 μ l, put respectively on same silica gel g thin-layer plate, with toluene: methanol=10: 1 be developing solvent, launches, and takes out, and dries, and sprays with rare bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

(4) get tablet or capsule 3g, porphyrize is put in the evaporating dish, and loam cake glass surface ware heated in hot bath 5～12 minutes, got the white crystals sublimate that adheres on the glass surface ware, and 2ml makes dissolving with ethyl acetate, as need testing solution.Other gets the Borneolum Syntheticum reference substance, adds ethyl acetate and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel G plate, with petroleum ether (60～90 ℃): ethyl acetate=10: 1 is developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 110 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

Embodiments of the invention 11: the method for quality control of gold silver notoginseng preparations of the present invention can comprise:

Differentiate: (1) gets tablet or capsule 2g, and porphyrize adds methanol 20ml, supersound process 20 minutes, centrifugal, incline and get supernatant, medicinal residues are handled with method again, merge methanol extract liquid, evaporate to dryness, residue adds water 25ml dissolving and mixing, is added in the polyamide pillar (60～80 orders, the internal diameter 1cm that have handled well, long 15cm, wet method dress post) on, water 250ml eluting, collect water lotion, extract 4 (60ml, 50ml with the ethyl acetate jolting, 30ml, 20ml), merge ethyl acetate liquid, use the 50ml water washing, discard water liquid, ethyl acetate liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Folium Ginkgo control medicinal material 1.5g, shines medical material solution in pairs with legal system.Test according to the Chinese Pharmacopoeia thin layer chromatography.Draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H lamellae, with toluene: ethyl acetate: acetone: methanol=6: 3: 8: 0.6 is developing solvent, launch, take out, dry up, smoke 10 minutes with the acetic anhydride steam after, put 160 ℃ of heating 20 minutes, put under the ultra-violet lamp (400nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.

(2) get capsule 3g, porphyrize adds an amount of moistening of water, adds water-saturated n-butanol 60ml, and supersound process 20 minutes filters, and filtrate adds the saturated water washing of n-butyl alcohol of 4 times of amounts, gets the n-butanol extracting liquid evaporate to dryness, and residue adds methanol 1ml makes dissolving, as need testing solution.It is an amount of that other gets ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1 reference substance, adds methanol and make the mixed solution that every 1ml contains 4mg, in contrast product solution; Get Radix Notoginseng control medicinal material 1.0g, the compound method of pressing need testing solution is made control medicinal material solution.Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 15 μ l of above-mentioned two kinds of solution, put respectively in same with silica gel g thin-layer plate on, with n-butyl alcohol: ethyl acetate: the upper solution of water=8: 3: 7 is developing solvent, launch, take out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃.In the test sample chromatograph with the corresponding position of reference substance chromatograph on show the same color speckle.

(3) get capsule 4g, porphyrize adds ethanol 50ml, jolting was extracted 25 minutes, filtered the filtrate evaporate to dryness, residue adds 5% sulfuric acid solution 25ml makes dissolving, filter, filtrate is regulated pH value to 9～10 with strong ammonia solution, adds the chloroform jolting and extracts 2 times, each 25ml, combined chloroform liquid evaporate to dryness, residue add chloroform 1.5ml makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, and chlorination is copied into the solution that every 1ml contains 1.5mg, in contrast product solution.Test according to the Chinese Pharmacopoeia thin layer chromatography.Draw above-mentioned need testing solution 15 μ l, reference substance solution 4 μ l, put respectively on same silica gel g thin-layer plate, with toluene: methanol=5: 4 is developing solvent, launches, and takes out, and dries, and spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

Assay: schisandrin is according to high effective liquid chromatography for measuring.With the octadecylsilane chemically bonded silica is filler; Methanol: 0.4% phosphoric acid=35: 65 is mobile phase, and the detection wavelength is 500nm.Theoretical cam curve should be not less than 1800 by the cholic acid peak.It is an amount of that precision takes by weighing Quercetin, kaempferide, isorhamnetin reference substance, adds methanol and make the mixed solution that every 1ml contains Quercetin 150 μ g, kaempferide 150 μ g, isorhamnetin 120 μ g, shakes up, and promptly gets reference substance solution; Get tablet or capsule, claim to decide weight, porphyrize, get 2.0g, put in the tool plug conical flask, add chloroform 30ml, supersound process (power 250W, frequency 80KHz) 40 minutes filters, discard chloroform solution, the accurate methanol 30ml that adds of medicinal residues claims to decide weight, supersound process (power 250W, frequency 80KHz) 40 minutes is put cold, weight decided in title again, supplies with methanol to subtract weight loss, shakes up, filter, precision is measured subsequent filtrate 20ml, adds methanol 20ml and 25% hydrochloric acid 10ml, reflux 50 minutes is put coldly, is transferred in the 100ml measuring bottle, add methanol and be diluted to scale, shake up, filter, promptly get need testing solution with 0.45 μ m microporous filter membrane; Accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing inject chromatograph of liquid, measure content.In the said preparation, contain the Folium Ginkgo extract in the capsule, must not be less than 25.0mg/g in total flavonoids; Contain the Folium Ginkgo extract in the tablet in total flavonoids, must not be less than 20.0mg/g.

Embodiments of the invention 12: the method for quality control of gold silver notoginseng preparations of the present invention can comprise:

Differentiate: get tablet or capsule 2g, porphyrize is put in the evaporating dish, and loam cake glass surface ware heated in hot bath 5～9 minutes, got the white crystals sublimate that adheres on the glass surface ware, and 1ml makes dissolving with ethyl acetate, as need testing solution.Other gets the Borneolum Syntheticum reference substance, adds ethyl acetate and makes the solution that every 1ml contains 0.6mg, in contrast product solution.According to the test of Chinese Pharmacopoeia thin layer chromatography, draw each 7 μ l of above-mentioned two kinds of solution, put respectively on same silica gel G plate, with petroleum ether (60～90 ℃): ethyl acetate=7: 3 is developing solvent, launches, and takes out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

Check: should meet Chinese Pharmacopoeia about the pertinent regulations under tablet, the capsule item.

Assay: schisandrin is according to high effective liquid chromatography for measuring.With the octadecylsilane chemically bonded silica is filler; Methanol: 0.4% phosphoric acid=90: 10 is mobile phase, and the detection wavelength is 400nm.Theoretical cam curve should be not less than 1800 by the cholic acid peak.It is an amount of that precision takes by weighing Quercetin, kaempferide, isorhamnetin reference substance, adds methanol and make the mixed solution that every 1ml contains Quercetin 130 μ g, kaempferide 130 μ g, isorhamnetin 100 μ g, shakes up, and promptly gets reference substance solution; Get tablet or capsule, claim to decide weight, porphyrize, get 2.0g, put in the tool plug conical flask, add chloroform 20ml, supersound process (power 250W, frequency 80KHz) 40 minutes filters, discard chloroform solution, the accurate methanol 20ml that adds of medicinal residues claims to decide weight, supersound process (power 250W, frequency 80KHz) 30 minutes is put cold, weight decided in title again, supplies with methanol to subtract weight loss, shakes up, filter, precision is measured subsequent filtrate 15ml, adds methanol 15ml and 25% hydrochloric acid 8ml, reflux 40 minutes is put coldly, is transferred in the 50ml measuring bottle, add methanol and be diluted to scale, shake up, filter, promptly get need testing solution with 0.45 μ m microporous filter membrane; Accurate respectively reference substance solution and each 15 μ l of need testing solution of drawing inject chromatograph of liquid, measure content.In the said preparation, contain the Folium Ginkgo extract in the capsule, must not be less than 25.0mg/g in total flavonoids; Contain the Folium Ginkgo extract in the tablet in total flavonoids, must not be less than 20.0mg/g.

Claims

1. gold silver notoginseng preparations, it is characterized in that: calculate according to weight: it is prepared into capsule or tablet by Folium Ginkgo extract 20-80, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 50-200, Radix Notoginseng 50-200, Radix Salviae Miltiorrhizae 50-200, Rhizoma Chuanxiong 50-200, Olibanum 25-100, artificial Moschus 5-20, Borneolum Syntheticum 12.5-50 and adjuvant.

2. according to the described gold silver notoginseng preparations of claim 1, it is characterized in that: described adjuvant is total medicated powder amount 6-12% starch, 6-10% microcrystalline Cellulose and 0.5-1% magnesium stearate when being prepared into tablet.

3. according to the described gold silver notoginseng preparations of claim 2, it is characterized in that: be specially 9% starch, 8% microcrystalline Cellulose and 1% magnesium stearate.

4. according to the described gold silver notoginseng preparations of claim 1, it is characterized in that: described adjuvant is total medicated powder amount 15-25% starch, 0.5-1% magnesium stearate when being prepared into tablet.

5. according to the described gold silver notoginseng preparations of claim 4, it is characterized in that: be specially 18% starch, 1% magnesium stearate.

6. as the preparation method of gold silver notoginseng preparations as described among the claim 1-5 any, it is characterized in that: gold silver notoginseng preparations of the present invention is preparation like this: above eight flavor medical materials, get the Borneolum Syntheticum porphyrize, and frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong are ground into coarse powder, according to the percolation under Chinese Pharmacopoeia extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 12-48 hour, percolation speed is 5-7ml/min, collect percolate, reclaim ethanol, concentrating under reduced pressure is dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract and adjuvant, mixing is made different preparations according to conventional method again.

7. according to the preparation method of any described gold silver notoginseng preparations among the claim 1-6, it is characterized in that: tablet prepares like this: above eight flavor medical materials, get the Borneolum Syntheticum porphyrize, and frankincense powder is broken into fine powder; Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Notoginseng, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong are ground into coarse powder, according to the percolation under Chinese Pharmacopoeia extractum and the fluid extract item, make solvent with Diluted Alcohol, flood and carry out percolation after 12-48 hour, percolation speed is 5-7ml/min, collect percolate, reclaim ethanol, concentrating under reduced pressure, be dried to dried cream, be ground into fine powder, add above-mentioned fine powder and artificial Moschus, Folium Ginkgo extract and adjuvant, mixing is used the 70-95% alcohol granulation, drying, tabletting, coating, promptly.

8. the method for quality control of a gold silver notoginseng preparations, described preparation comprises capsule and tablet, it is characterized in that: described method of quality control mainly comprise in character, discriminating, inspection and the assay project partly or entirely; Wherein differentiate the feature discriminating that comprises contained Folium Ginkgo extract, Radix Notoginseng, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Borneolum Syntheticum composition in the preparation; Assay is the assay to the contained total flavonoids of Folium Ginkgo extract in the preparation.

9. according to the method for quality control of the described gold silver notoginseng preparations of claim 8, it is characterized in that: discrimination method comprises the part or all of of following project:

(1) get tablet, capsule respectively, porphyrize adds methanol, supersound process, centrifugal, incline and get supernatant, medicinal residues are handled with method again, merge methanol extract liquid, evaporate to dryness, residue are dissolved in water and mixing, are added on the polyamide pillar of having handled well, the water eluting is collected water lotion, extracts with the ethyl acetate jolting, merge ethyl acetate liquid, water washing discards water liquid, ethyl acetate liquid evaporate to dryness, residue adds methanol makes dissolving, as need testing solution; Other gets the Folium Ginkgo control medicinal material, shines medical material solution in pairs with legal system; Test according to the Chinese Pharmacopoeia thin layer chromatography; Draw above-mentioned two kinds of solution, put respectively on same silica gel H lamellae, with toluene: ethyl acetate: acetone: methanol=1-10: 1-10: 1-10: 0.1-1 is developing solvent, launch, take out, dry up, after smoking with the acetic anhydride steam, 140-170 ℃ of heating put under the ultra-violet lamp (200-500nm) and inspected; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

(2) get tablet, capsule respectively, porphyrize adds an amount of moistening of water, adds water-saturated n-butanol, and supersound process filters, and filtrate adds the saturated water washing of n-butyl alcohol, gets the n-butanol extracting liquid evaporate to dryness, and residue adds methanol makes dissolving, as need testing solution; It is an amount of that other gets ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1 reference substance, adds methanol and make mixed solution, in contrast product solution; Get the Radix Notoginseng control medicinal material, press the compound method of need testing solution, make control medicinal material solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw above-mentioned two kinds of solution, put respectively in same with silica gel g thin-layer plate on, with n-butyl alcohol: the upper solution of ethyl acetate: water=1-10: 1-10: 10-1 is developing solvent, launch, take out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 100-110 ℃; In the test sample chromatograph with the corresponding position of control medicinal material chromatograph on show the same color speckle;

(3) get tablet, capsule respectively, porphyrize adds ethanol, and jolting is extracted, and filters, filtrate evaporate to dryness, residue add sulfuric acid solution makes dissolving, filters, and filtrate is regulated pH value with strong ammonia solution, adds the chloroform jolting and extracts, combined chloroform liquid, evaporate to dryness, residue add chloroform makes dissolving, as need testing solution; Other gets the tetrahydropalmatine reference substance, adds the chloroform dissolving, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography; Drawing above-mentioned need testing solution, reference substance solution, put respectively on same silica gel g thin-layer plate, is developing solvent with toluene: methanol=10-1: 1-10, launches, and takes out, and dries, and spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4) get tablet, capsule respectively, porphyrize is put in the evaporating dish, and loam cake glass surface ware heats in hot bath, gets the white crystals sublimate that adheres on the glass surface ware, makes dissolving with ethyl acetate, as need testing solution; Other gets the Borneolum Syntheticum reference substance, adds the ethyl acetate dissolving, in contrast product solution; According to the test of Chinese Pharmacopoeia thin layer chromatography, draw above-mentioned two kinds of solution, put respectively on same silica gel G plate, with petroleum ether (60～90 ℃): ethyl acetate=10-1: 1-10 is developing solvent, launches, and takes out, dry, spray is with phosphomolybdic acid ethanol solution, and it is clear to be heated to speckle colour developing at 100-110 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

10. according to the method for quality control of claim 8 or 9 described gold silver notoginseng preparations, it is characterized in that: discrimination method comprises the part or all of of following project:

(1) gets tablet respectively, capsule 1-3g, porphyrize adds methanol 10-40ml, supersound process 5-30 minute, centrifugal, incline and get supernatant, medicinal residues are handled 1-3 time with method again, merge methanol extract liquid, evaporate to dryness, residue adds water 10-30ml dissolving and mixing, is added in the polyamide pillar (60～80 orders, the internal diameter 1cm that have handled well, long 15cm, wet method dress post) on, water 100-300ml eluting is collected water lotion, extract 2-5 time (20-80ml) with the ethyl acetate jolting, merge ethyl acetate liquid, water washing 1-3 time, each 20-60ml, discard water liquid, ethyl acetate liquid evaporate to dryness, residue add methanol 0.5-2ml makes dissolving, as need testing solution; Other gets the Folium Ginkgo control medicinal material, shines medical material solution in pairs with legal system; Test according to the Chinese Pharmacopoeia thin layer chromatography; Draw each 2-20 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel H lamellae of adhesive preparation with the carboxymethylcellulose sodium solution that contains 4% sodium acetate, with toluene: ethyl acetate: acetone: methanol=1-10: 1-10: 1-10: 0.1-1 is developing solvent, launch, take out, dry up, smoke 10-30 minute with the acetic anhydride steam after, put 160 ℃ of heating 20-40 minute, put under the ultra-violet lamp (200-500nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

(2) get tablet, capsule 1-3g respectively, porphyrize, add an amount of moistening of water, add water-saturated n-butanol 20-80ml, supersound process 10-30 minute, filter, filtrate adds the saturated water washing of n-butyl alcohol that 2-5 doubly measures, get the n-butanol extracting liquid evaporate to dryness, residue adds methanol 0.5-2ml makes dissolving, as need testing solution; It is an amount of that other gets ginsenoside Rg1, ginsenoside Rb1 and arasaponin R1 reference substance, adds methanol and make the mixed solution that every 1ml contains 1-5mg, in contrast product solution; Get Radix Notoginseng control medicinal material 1-3g, the compound method of pressing need testing solution is made control medicinal material solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 5-20 μ l of above-mentioned two kinds of solution, put respectively in same with silica gel g thin-layer plate on, with n-butyl alcohol: the upper solution of ethyl acetate: water=1-10: 1-10: 10-1 is developing solvent, launch, take out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 100-110 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the same color speckle;

(3) get tablet, capsule 1-5g respectively, porphyrize adds ethanol 10-60ml, jolting was extracted 10-30 minute, filtered the filtrate evaporate to dryness, residue adds 5% sulfuric acid solution 10-30ml makes dissolving, filters, and filtrate is regulated pH value to 9～10 with strong ammonia solution, adding the chloroform jolting extracts 1-3 time, each 10-30ml, combined chloroform liquid, evaporate to dryness, residue adds chloroform 0.5-2ml makes dissolving, as need testing solution; Other gets the tetrahydropalmatine reference substance, and chlorination is copied into the solution that every 1ml contains 0.5-2mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography; Draw above-mentioned need testing solution 5-20 μ l, reference substance solution 1-5 μ l, putting in the sodium carboxymethyl cellulose of same usefulness 0.5% sodium hydroxide solution preparation respectively is on the silica gel g thin-layer plate of adhesive, with toluene: methanol=10-1: 1-10 is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4) get tablet, capsule 1-3g respectively, porphyrize is put in the evaporating dish, and loam cake glass surface ware heated in hot bath 3～12 minutes, got the white crystals sublimate that adheres on the glass surface ware, and 0.5-2ml makes dissolving with ethyl acetate, as need testing solution; Other gets the Borneolum Syntheticum reference substance, adds ethyl acetate and makes the solution that every 1ml contains 0.1-1mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 2-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel G plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃): ethyl acetate=10-1: 1-10 is developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 100-110 ℃; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color.

11. the method for quality control according to the described gold silver notoginseng preparations of claim 8 is characterized in that: the content assaying method of total flavonoids is: according to high effective liquid chromatography for measuring; Chromatographic column is C18 or C4 or C8 post, and with methanol: 0.4% phosphoric acid=10-90: 90-10 is a mobile phase; The detection wavelength is 200-500nm; Number of theoretical plate calculates by the total flavonoids peak should be not less than 1800; It is an amount of to get Quercetin, kaempferol, isorhamnetin reference substance, accurately claims surely, adds dissolve with methanol and makes mixed solution, in contrast product solution; Get capsule, tablet under the content uniformity item, porphyrize is put in the tool plug conical flask, adds chloroform, supersound process filters, and discards chloroform solution, the accurate methanol that adds of medicinal residues, claim decide weight, supersound process is put coldly, and weight decided in title again, supply with methanol and to subtract weight loss, shake up, filter, precision is measured subsequent filtrate, add methanol and hydrochloric acid, reflux is put coldly, is transferred in the measuring bottle, add methanol and be diluted to scale, shake up, filter, promptly get need testing solution with microporous filter membrane; Accurate respectively reference substance solution and the need testing solution drawn injects hplc determination content;

12. the method for quality control according to claim 8 or 11 described gold silver notoginseng preparations is characterized in that: concrete content assaying method is: according to high effective liquid chromatography for measuring; Chromatographic column is C18 or C4 or C8 post, and with methanol: 0.4% phosphoric acid=10-90: 90-10 is a mobile phase; The detection wavelength is 200-500nm; Number of theoretical plate calculates by the total flavonoids peak should be not less than 1800; It is an amount of that precision takes by weighing Quercetin, kaempferol, isorhamnetin reference substance, adds dissolve with methanol and make the mixed solution that every 1ml contains Quercetin 90-150 μ g, kaempferol 90-150 μ g, isorhamnetin 80-120 μ g, shakes up and promptly get reference substance solution; Get the capsule under the content uniformity item, tablet, porphyrize is got the about 2.0g of fine powder, put in the tool plug conical flask, add chloroform 10-30ml, supersound process 20-40 minute, filter, discard chloroform solution, the accurate methanol 10-30ml that adds of medicinal residues, claim to decide weight, supersound process 20-40 minute, put cold, weight decided in title again, supplies with methanol to subtract weight loss, shakes up, filter, precision is measured subsequent filtrate 5-20ml, adds methanol 5-20ml and 5% hydrochloric acid 1-10ml, reflux 20-50 minute, put cold, be transferred in the 50-100ml measuring bottle, add methanol and be diluted to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly get need testing solution; Accurate respectively reference substance solution and each 5-20 μ l of need testing solution of drawing injects chromatograph of liquid, measures content;

13. the method for quality control according to the described gold silver notoginseng preparations of claim 8 is characterized in that: method of quality control of the present invention comprises:

Character observed comprises:

For tablet, character is: this product is a Film coated tablets, removes to show yellowish-brown behind the coating to brown; Gas fragrance, acrid in the mouth, hardship, little puckery;

For capsule, character is: this product is a capsule, and content is the granule of yellowish-brown to brown; Gas fragrance, acrid in the mouth, hardship, little puckery;

Described discrimination method is selected from one or more in the following method:

(4) get tablet, capsule respectively, porphyrize is put in the evaporating dish, and loam cake glass surface ware heats in hot bath, gets the white crystals sublimate that adheres on the glass surface ware, makes dissolving with ethyl acetate, as need testing solution; Other gets the Borneolum Syntheticum reference substance, adds the ethyl acetate dissolving, in contrast product solution; According to the test of Chinese Pharmacopoeia thin layer chromatography, draw above-mentioned two kinds of solution, put respectively on same silica gel G plate, with petroleum ether (60～90 ℃): ethyl acetate=10-1: 1-10 is developing solvent, launches, and takes out, dry, spray is with phosphomolybdic acid ethanol solution, and it is clear to be heated to speckle colour developing at 100-110 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

Official method inspection comprises:

Tablet of the present invention, capsule should meet Chinese Pharmacopoeia about the pertinent regulations under capsule, the tablet item; The total flavonoids that contains is carried out assay be may further comprise the steps:

Total flavonoids is according to high effective liquid chromatography for measuring; Chromatographic column is C18 or C4 or C8 post, and with methanol: 0.4% phosphoric acid=10-90: 90-10 is a mobile phase; The detection wavelength is 200-500nm; Number of theoretical plate calculates by the total flavonoids peak should be not less than 1800; It is an amount of to get Quercetin, kaempferol, isorhamnetin reference substance, accurately claims surely, adds dissolve with methanol and makes mixed solution, in contrast product solution; Get capsule, tablet under the content uniformity item, porphyrize is put in the tool plug conical flask, adds chloroform, supersound process filters, and discards chloroform solution, the accurate methanol that adds of medicinal residues, claim decide weight, supersound process is put coldly, and weight decided in title again, supply with methanol and to subtract weight loss, shake up, filter, precision is measured subsequent filtrate, add methanol and hydrochloric acid, reflux is put coldly, is transferred in the measuring bottle, add methanol and be diluted to scale, shake up, filter, promptly get need testing solution with microporous filter membrane; Accurate respectively reference substance solution and the need testing solution drawn injects hplc determination content; In the said preparation, contain the Folium Ginkgo extract in the capsule, must not be less than and contain the Folium Ginkgo extract in 25.0mg/g, the tablet, must not be less than 20.0mg/g in total flavonoids in total flavonoids.

14. the method for quality control according to claim 8 or 13 described gold silver notoginseng preparations is characterized in that: described method of quality control comprises:

Character observed comprises:

(4) get tablet, capsule 1-3g respectively, porphyrize is put in the evaporating dish, and loam cake glass surface ware heated in hot bath 3～12 minutes, got the white crystals sublimate that adheres on the glass surface ware, and 0.5-2ml makes dissolving with ethyl acetate, as need testing solution; Other gets the Borneolum Syntheticum reference substance, adds ethyl acetate and makes the solution that every 1ml contains 0.1-1mg, in contrast product solution; Test according to the Chinese Pharmacopoeia thin layer chromatography, draw each 2-10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel G plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃): ethyl acetate=10-1: 1-10 is developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 100-110 ℃; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color;

Official method inspection comprises:

Total flavonoids is according to high effective liquid chromatography for measuring; Chromatographic column is C18 or C4 or C8 post, and with methanol: 0.4% phosphoric acid=10-90: 90-10 is a mobile phase; The detection wavelength is 200-500nm; Number of theoretical plate calculates by the total flavonoids peak should be not less than 1800; It is an amount of that precision takes by weighing Quercetin, kaempferol, isorhamnetin reference substance, adds dissolve with methanol and make the mixed solution that every 1ml contains Quercetin 90-150 μ g, kaempferol 90-150 μ g, isorhamnetin 80-120 μ g, shakes up and promptly get reference substance solution; Get the capsule under the content uniformity item, tablet, porphyrize is got the about 2.0g of fine powder, put in the tool plug conical flask, add chloroform 10-30ml, supersound process 20-40 minute, filter, discard chloroform solution, the accurate methanol 10-30ml that adds of medicinal residues, claim to decide weight, supersound process 20-40 minute, put cold, weight decided in title again, supplies with methanol to subtract weight loss, shakes up, filter, precision is measured subsequent filtrate 5-20ml, adds methanol 5-20ml and 5% hydrochloric acid 1-10ml, reflux 20-50 minute, put cold, be transferred in the 50-100ml measuring bottle, add methanol and be diluted to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly get need testing solution; Accurate respectively reference substance solution and each 5-20 μ l of need testing solution of drawing injects chromatograph of liquid, measures content; In the said preparation, contain the Folium Ginkgo extract in the capsule, must not be less than and contain the Folium Ginkgo extract in 25.0mg/g, the tablet, must not be less than 20.0mg/g in total flavonoids in total flavonoids.