CN101036748A - Quality control method of the Yixinshu Chinese traditional medicine for supplementing qi and for promoting blood circulation by removing blood stasis - Google Patents

Quality control method of the Yixinshu Chinese traditional medicine for supplementing qi and for promoting blood circulation by removing blood stasis Download PDF

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CN101036748A
CN101036748A CN 200710077725 CN200710077725A CN101036748A CN 101036748 A CN101036748 A CN 101036748A CN 200710077725 CN200710077725 CN 200710077725 CN 200710077725 A CN200710077725 A CN 200710077725A CN 101036748 A CN101036748 A CN 101036748A
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ginsenoside
ethyl acetate
chloroform
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CN101036748B (en
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张观福
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Guizhou Xinbang Pharmaceutical Co Ltd
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Abstract

The invention relates to a quality control method of Yixinshu traditional chinese medicine preparation for nourishing qi, restoring pulse, and activating blood circulation to dissipate blood stasis, belonging to medicine domain. The Yixinshu traditional chinese medicine preparation is composed of panax, astragalus root, radix salviae miltiorrhizae, lityturf root, chinese magnoliaving, chuanxiong rhizome and haw, with ability of nourishing qi, restoring pulse, activating blood circulation to dissipate blood stasis, nourishing yin and production of body fluid, applicable for the patients who suffer for deficiency of both vital energu and yin, heart-throb knotted pulse, chest oppression, chest pain, and angina pectoris of coronary heart disease. At present, on clinical usage, it is applied extensively in the treatment of angina pectoris, myocardial ischemia, various type of arrhythmias, atrial premature beat, chest pain, angina pectoris of coronary heart disease and so on. The said quality control method provides the criterion of detection, means of detection, technical method and so on for the associated production and detection mechanism, therefore the quality of Yixinshu traditional chinese medicine preparation can be better controlled to ensure the safety of the said preparation. The quality method can better guide the production to make the production process control more strict and reasonable, therefore the users could have an overall acquaintance with the product quality.

Description

The method of quality control of the YIXINSHU Chinese medicine preparation of a kind of Yiqi and vein recovery, blood circulation promoting and blood stasis dispelling
Technical field:
The present invention relates to the method for quality control of the YIXINSHU Chinese medicine preparation of a kind of Yiqi and vein recovery, blood circulation promoting and blood stasis dispelling, belong to technical field of medicaments.
Background technology:
The YIXINSHU Chinese medicine preparation is to form with seven flavor medicines such as Radix Ginseng, Radix Ophiopogonis, Fructus Schisandrae Chinensis, the Radix Astragali, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, Fructus Crataegis, has Yiqi and vein recovery, blood circulation promoting and blood stasis dispelling, the effect of YIN nourishing and the production of body fluid promoting, be used for deficiency of both QI and YIN, the cardiopalmus irregularly intermittent and regularly intermittent pulse does not uncomfortable in chestly relax, chest pain and angina pectoris are seen the person that has the above-mentioned symptom, are widely used in treatment angina pectoris, myocardial ischemia, various arrhythmia, artrial premature beat, chest pain and angina pectoris trouble etc. at present clinically.Many pharmacy workers have done number of research projects, as: the number of patent application that Xinbang Yuandong Pharmaceutical Co., Ltd., Guizhou proposes is " 200610050956.8 ", name is called the patent application of " a kind of Yiqi and vein recovery; YIXINSHU ejection preparation of blood circulation promoting and blood stasis dispelling and preparation method thereof ", the preparation method of YIXINSHU injection is provided, but pharmaceutical preparation must be on the basis that guarantees the constant product quality controllable safety, constantly more new development, in order better to control the quality of this Chinese medicine preparation, guarantee the safety of medication, better instruct and produce, make technology controlling and process rationally strict more, make consumer's energy full appreciation product quality, need research, control this Chinese medicine preparation method for quality, though Anhui Kechuang Chinese Medicine Research Institute Limited Liability Company is called the method for quality control that granule is provided in " particulate preparation method of YIXINSHU and Quality Control Technology " patent application at number of patent application for " 200510038859.2 " name, this method is the ginsenoside Re with Radix Ginseng, Rb1 is the content detection index, but, it is the quality of reactor product comprehensively at all, is not very reasonable with this quality that is used for controlling this Chinese medicine preparation only; If the index with other is controlled,, relatively be difficult to implement owing to do not have ready-made detection scheme, testing conditions etc.
Summary of the invention
The objective of the invention is to: the method for quality control of the YIXINSHU Chinese medicine preparation of a kind of Yiqi and vein recovery, blood circulation promoting and blood stasis dispelling is provided, and this method provides means, technical method of the index that detects, detection or the like to relevant production, testing agency; So that better control the quality of this Chinese medicine preparation, guarantee the safety of medication, can better instruct production, make controlling of production process rationally strict more, make consumer's energy full appreciation product quality.
The present invention relates to ginseng crude drug or its extract; Radix Ophiopogonis medical material or its extract; schisandra chinensis medicinal material or its extract; Milkvetch Root or its extract; red rooted salvia or its extract; Rhizoma Chuanxiong medical material or its extract; the method of quality control of the Chinese medicine preparation that Fructus Crataegi medical material or its extract are made according to certain ratio prescription; mainly comprise discriminating; projects such as assay, it is with the Radix Ginseng control medicinal material; the ginsenoside Rg1; the ginsenoside Re; the ginsenoside Rh2; the panoxadiol; the panaxatriol; the ginsenoside Rb1; the Ginsenoside Rc; the ginsenoside Rb2; Radix Ginseng soap two Rd; the ginsenoside Ra 1; ginsenoside Rh1; the ginsenoside Rf; ginsenoside Rg2; the ginsenoside Rg3; Radix Ophiopogonis control medicinal material; ophiopogonin D; ruscogenin; diosgenin; ophiopogonin B; Ruscus aculeatus L. sapogenin; cupreol; glucose; the Fructus Schisandrae Chinensis control medicinal material; schisandrin; schisantherin B; deoxyschizandrin; schisandrin B; schisandrin C and schisantherin A; schisantherin B; Radix Astragali control medicinal material; acetyl astragaloside I; astragaloside I; astragaloside II; astragaloside III; astragaloside; different astragaloside I; different astragaloside II; astramembrannin; Cycloastragenol; soybean saponin I; formononetin; calycosin; kaempferol; rutin; Quercetin; Quercitroside; isorhamnetin; the rhamnocitrin aglycon; isoquercitrin; the cotton wool astragaloside; cotton wool astragaloside VI; cotton wool astragaloside II; the Radix Salviae Miltiorrhizae control medicinal material; Tanshinone I; tanshinone; Tanshinone II B; cryptotanshinone; salvianolic acid A; salvianolic acid B; salvianolic acid C; salvianolic acid D; salvianolic acid E; salvianolic acid G; salvianolic acid H; salvianolic acid I; salvianolic acid J; the red sour F of tetramethyl; different salvianolic acid C; rosmarinic acid; alkannic acid; Radix Salviae Miltiorrhizae quinone A; Radix Salviae Miltiorrhizae quinone B; Radix Salviae Miltiorrhizae quinone C; danshensu; danshensuan B; the Rhizoma Chuanxiong control medicinal material; ligustrazine; ferulic acid; adenine; adenosine; cnidium lactone; chuanxingol; fourth fork benzene peptide lactones; methyl phenylacetate; vanillin; the Fructus Crataegi control medicinal material; hyperin; vitexin; oleanolic acid; ursolic acid; Fumaric acid; succinic acid; stigmasterol; all or part of kind in the daucosterol is as the detection index of the quality control of this Chinese medicine preparation.
A kind of Yiqi and vein recovery of the present invention, the method of quality control of the YIXINSHU Chinese medicine preparation of blood circulation promoting and blood stasis dispelling is with the panoxadiol, the panaxatriol, the ginsenoside Rd, ginsenoside Rb3, the ginsenoside Rf, the ginsenoside Rg3, the ginsenoside Rg1, the ginsenoside Rb1, the ginsenoside Re, the Radix Ginseng control medicinal material, ophiopogonin D, ophiopogonin B, Radix Ophiopogonis control medicinal material, schisandrin, schisantherin B, deoxyschizandrin, schisandrin B, schisandrin C, and schisantherin A, schisantherin B, the Fructus Schisandrae Chinensis control medicinal material, astragaloside, kaempferol, rutin, Quercetin, Quercitroside, isorhamnetin, Radix Astragali control medicinal material, glucose, Tanshinone I, tanshinone, Tanshinone II B, salvianolic acid A, salvianolic acid B, salvianolic acid C, danshensu, danshensuan B, the Radix Salviae Miltiorrhizae control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, vanillin, the Rhizoma Chuanxiong control medicinal material, hyperin, vitexin, oleanolic acid, ursolic acid, Fumaric acid, all or part of kind in the Fructus Crataegi control medicinal material is as the discrimination method of this Chinese medicine preparation, the detection index of content assaying method.
The method of quality control of the YIXINSHU Chinese medicine preparation of a kind of Yiqi and vein recovery of the present invention, blood circulation promoting and blood stasis dispelling, for authentication technique, adopt all or part of method as quality control in the following method:
Discrimination method for Radix Ginseng: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Radix Ginseng control medicinal material, the panoxadiol, the panaxatriol, the ginsenoside Rd, the ginsenoside Rb1, the ginsenoside Rf, the ginsenoside Rg3, the ginsenoside Rg1, ginsenoside Rb3, all or part of kind product in contrast among the ginsenoside Re, sample pre-treatments comprises direct sample or with the method for refining reconcentration behind ethanol or methanol or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be chloroform, acetone, formic acid, water, methanol, dichloromethane, ethyl acetate, glacial acetic acid, in the n-butyl alcohol one or more are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with 2-30% sulphuric acid ethanol, or spray is with the method for solution such as 1-10% triketohydrindene hydrate ethanol colour developing;
Discrimination method for Radix Ophiopogonis: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with control medicinal material Radix Ophiopogonis, ophiopogonin D, ruscogenin, diosgenin, ophiopogonin B, Ruscus aculeatus L. sapogenin, cupreol, all or part of kind product in contrast in the glucose, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be ethyl acetate, methanol, water, normal hexane, chloroform, acetone, n-butyl alcohol, diethylamine, pyridine, toluene, formic acid, cyclohexane extraction, benzene, glacial acetic acid, one or more reagent in the petroleum ether are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with ethanol solution of sulfuric acid, concentrated sulfuric acid aqueous solution, the anisaldehyde sulfuric acid solution, 10% sulfuric acid solution, the method of solution such as 5% ferric chloride alcoholic solution colour developing;
Discrimination method for Fructus Schisandrae Chinensis: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Fructus Schisandrae Chinensis control medicinal material, schisandrin, schisantherin B, deoxyschizandrin, schisandrin B, schisandrin C, and schisantherin A, all or part of kind product in contrast in the schisantherin B, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with the chromotropic acid sulfuric acid solution, the anisaldehyde sulfuric acid solution, iodine vapor, the method of 10% phosphomolybdic acid ethanol solution solution colour developing;
Discrimination method for the Radix Astragali: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with Radix Astragali control medicinal material, astragaloside, kaempferol, rutin, Quercetin, Quercitroside, isorhamnetin, all or part of kind product in contrast in the glucose, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be ethyl acetate, methanol, water, normal hexane, chloroform, acetone, n-butyl alcohol, diethylamine, pyridine, toluene, formic acid, cyclohexane extraction, benzene, glacial acetic acid, one or more reagent in the petroleum ether are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with ethanol solution of sulfuric acid, concentrated sulfuric acid solution, the anisaldehyde sulfuric acid solution, 10% sulfuric acid solution, the method of solution such as 5% ferric chloride alcoholic solution colour developing;
Discrimination method for Radix Salviae Miltiorrhizae: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Radix Salviae Miltiorrhizae control medicinal material, Tanshinone I, tanshinone, Tanshinone II B, salvianolic acid A, salvianolic acid B, salvianolic acid C, danshensu, all or part of kind product in contrast in the danshensuan B, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with the chromotropic acid sulfuric acid solution, the anisaldehyde sulfuric acid solution, iodine vapor, the method of 10% phosphomolybdic acid ethanol solution solution colour developing;
Discrimination method for Rhizoma Chuanxiong: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with the chromotropic acid sulfuric acid solution, the anisaldehyde sulfuric acid solution, iodine vapor, the method of 10% phosphomolybdic acid ethanol solution solution colour developing;
Discrimination method for Fructus Crataegi: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Fructus Crataegi control medicinal material, hyperin, vitexin, oleanolic acid, ursolic acid, all or part of kind product in contrast in the Fumaric acid, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with 1～10% ferric chloride alcoholic solution, the chromotropic acid sulfuric acid solution, the anisaldehyde sulfuric acid solution, iodine vapor, the method of 10% phosphomolybdic acid ethanol solution solution colour developing.
The method of quality control of the YIXINSHU Chinese medicine preparation of a kind of Yiqi and vein recovery of the present invention, blood circulation promoting and blood stasis dispelling, for authentication technique, can also adopt all or part of method as quality control in the following method:
Discrimination method for Radix Ginseng: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with acetonitrile, water, methanol, one or more kind solvents in the phosphoric acid are mobile phase under the proper ratio condition of routine, with the Radix Ginseng control medicinal material, the ginsenoside Rg1, the ginsenoside Re, the ginsenoside Rh2, the panoxadiol, the panaxatriol, the ginsenoside Rb1, the Ginsenoside Rc, the ginsenoside Rb2, the ginsenoside Rd, the ginsenoside Ra 1, ginsenoside Rh1, the ginsenoside Rf, ginsenoside Rg2, all or part of kind product in contrast among the ginsenoside Rg3 detect wavelength in 200～600nm scope;
Discrimination method for Radix Ophiopogonis: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with the second eyeball, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with control medicinal material Radix Ophiopogonis, ophiopogonin D, ruscogenin, diosgenin, ophiopogonin B, Ruscus aculeatus L. sapogenin, cupreol, all or part of kind product in contrast in the glucose detect wavelength in 200～600nm scope;
Discrimination method for Fructus Schisandrae Chinensis: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate vinegar or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, acetonitrile, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the suitable ratio condition of routine, with the Fructus Schisandrae Chinensis control medicinal material, schisandrin, schisantherin B, deoxyschizandrin, schisandrin B, plain in the Fructus Schisandrae Chinensis, and schisantherin A, all or part of kind product in contrast in the schisantherin B detect wavelength in 200～600nm scope;
Discrimination method for the Radix Astragali: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with acetonitrile, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with Radix Astragali control medicinal material, astragaloside, kaempferol, Quercetin, Quercitroside, isorhamnetin, all or part of kind product in contrast in the glucose detect wavelength in 200～600nm scope;
Discrimination method for Radix Salviae Miltiorrhizae: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with acetonitrile, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with the Radix Salviae Miltiorrhizae control medicinal material, Tanshinone I, tanshinone, Tanshinone II B, salvianolic acid A, salvianolic acid B, salvianolic acid C, danshensu, all or part of kind product in contrast in the danshensuan B detect wavelength in 200～600nm scope;
Discrimination method for Rhizoma Chuanxiong: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with acetonitrile, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin detect wavelength in 200～600nm scope;
Discrimination method for Fructus Crataegi: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with acetonitrile, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with the Fructus Crataegi control medicinal material, hyperin, vitexin, oleanolic acid, ursolic acid, all or part of kind product in contrast in the Fumaric acid detect wavelength in 200～600nm scope.
The method of quality control of the YIXINSHU Chinese medicine preparation of a kind of Yiqi and vein recovery of the present invention, blood circulation promoting and blood stasis dispelling, for authentication technique, the method for preferably selecting for use is: adopt all or part of method as quality control in the following method:
Discriminating for Radix Ginseng: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is 0.5～20 μ l, with the ginsenoside Rb1, Re, all or part of kind product in contrast among the Rg1, sample pre-treatments is with chloroform-ether mixed solvent extraction according to a certain percentage impurity, use ethanol then, methanol, ethyl acetate, a kind of or their any mixed solvents in the water extract back reconcentration method, the reuse n-butyl alcohol, the purified method of water extraction, developing solvent is a chloroform, methanol, water is formulated according to conventional ratio, and the condition of inspecting is the method for spray to inspect under the ultraviolet of 2～30% sulphuric acid ethanol colour developing back;
Discriminating for Radix Ophiopogonis: adopt thin layer chromatography, use silica gel G to be lamellae, the point sample amount is 0.5～20 μ l, with control medicinal material Radix Ophiopogonis product in contrast, sample pre-treatments is with methanol, ethanol, ethyl acetate, ether, acetone, chloroform, dichloromethane, petroleum ether, n-butyl alcohol, a kind of or their any mixed solvents in the water extract back reconcentration method, developing solvent is a chloroform, acetone is formulated according to conventional ratio, and the condition of inspecting is the method liquid of spray to inspect under the ultraviolet of 2～30% sulphuric acid ethanol colour developing back, concentrated sulfuric acid aqueous solution, the anisaldehyde sulfuric acid solution, 10% sulfuric acid solution, the method of 5% ferric chloride alcoholic solution solution colour developing;
Discriminating for Fructus Schisandrae Chinensis: adopt thin layer chromatography, use silica gel G F 254Lamellae, the point sample amount is an a certain volume between 0.5～20 μ l, with Fructus Schisandrae Chinensis control medicinal material, deoxyschizandrin product in contrast, sample pre-treatments is that a kind of or their any mixed solvents in chloroform, dichloromethane, ethyl acetate, acetone, Ethyl formate, n-butyl alcohol, benzene, toluene, methanol, ethanol, ether, the petroleum ether extract back reconcentration method, developing solvent is the upper strata liquid of petroleum ether, Ethyl formate, formic acid, and the condition of inspecting is that 254nm inspects under the ultra-violet lamp.
Discriminating for the Radix Astragali: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is an a certain volume between 0.5 μ l～30 μ l, with Radix Astragali control medicinal material, astragaloside is product in contrast, sample pre-treatments is a chloroform, dichloromethane, ethyl acetate, acetone, Ethyl formate, n-butyl alcohol, benzene, toluene, methanol, ethanol, ether, a kind of or their any mixed solvents in the petroleum ether extract impurity, use ethanol then, methanol, ethyl acetate, a kind of or their any mixed solvents in the water extract back reconcentration method, the reuse n-butyl alcohol, water, ammonia solution extracts purified method, developing solvent is a chloroform, methanol, water formulated according to conventional ratio, the condition of inspecting is the method for spray to inspect under the ultraviolet of 2～30% sulphuric acid ethanol colour developing back;
Discriminating for Radix Salviae Miltiorrhizae: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is an a certain volume between 0.5 μ l～30 μ l, with the Radix Salviae Miltiorrhizae control medicinal material, danshensu, salvianolic acid B, all or part of kind product in contrast in the tanshinone, sample pre-treatments is with chloroform, ether, petroleum ether uses separately or the impurity of mixed solvent extraction according to a certain percentage, use ethanol then, methanol, ethyl acetate, a kind of or dissolved method of they any mixed solvents in the water, developing solvent is a benzene, toluene, ethyl acetate, the condition of inspecting are to inspect under the daylight.
Discriminating for Rhizoma Chuanxiong: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is an a certain volume between 0.5 μ l～30 μ l, with the product in contrast of all or part of kind in Rhizoma Chuanxiong control medicinal material, the ferulic acid, sample pre-treatments is to use separately or the impurity of mixed solvent extraction according to a certain percentage with chloroform, ether, petroleum ether, use a kind of or dissolved method of they any mixed solvents in ethanol, methanol, ethyl acetate, the water then, developing solvent is normal hexane, ethyl acetate, and the condition of inspecting is that 365nm inspects under the ultra-violet lamp.
Discriminating for Fructus Crataegi: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is an a certain volume between 0.5 μ l～30 μ l, with the product in contrast of all or part of kind in Fructus Crataegi control medicinal material, ursolic acid, hyperin, the vitexin, extract back reconcentration method with a kind of or their any mixed solvents in ethyl acetate, chloroform, dichloromethane, n-butyl alcohol, methanol, ethanol, acetone, the water, developing solvent is cyclohexane extraction, ethyl acetate, formic acid, spray is with 2% ferric chloride alcoholic solution, and the condition of inspecting is to inspect under ultra-violet lamp or the daylight.
The method of quality control of the YIXINSHU Chinese medicine preparation of a kind of Yiqi and vein recovery of the present invention, blood circulation promoting and blood stasis dispelling, for the assay technology, adopt all or part of method as quality control in the following method:
Method 1: with the total saponin content in visible determined by ultraviolet spectrophotometry this product, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, measuring wavelength is a certain wavelength among 200～600nm, adopt standard curve method or reference substance method to measure, reference substance commonly used is Rg1, astragaloside;
Method 2: with the general flavone content in visible determined by ultraviolet spectrophotometry this product, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, measuring wavelength is a certain wavelength among 200～600nm, adopt standard curve method or reference substance method to measure, reference substance commonly used is rutin, Quercetin, Quercitroside;
Method 3: with the total sugar content in visible determined by ultraviolet spectrophotometry this product, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, measuring wavelength is a certain wavelength among 200～650nm, adopt standard curve method or reference substance method to measure, reference substance commonly used is a glucose;
Method 4: with the ginsenoside Rg1 in high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method mensuration this product, the ginsenoside Re, the ginsenoside Rh2, the panoxadiol, the panaxatriol, the ginsenoside Rb1, the Ginsenoside Rc, the ginsenoside Rb2, the ginsenoside Rd, the ginsenoside Ra 1, ginsenoside Rh1, the ginsenoside Rf, ginsenoside Rg2, all or part of kind among the ginsenoside Rg3, sample pre-treatments comprises direct sample or the method for reconcentration behind cruel or chloroform or dichloromethane or the n-butanol extraction with acetic acid second, the chromatographic column of use 8 or C18 type filler, with acetonitrile, water, methanol, one or more kind solvents in the phosphoric acid are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 5: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method to measure ophiopogonin D in this product, ruscogenin, diosgenin, ophiopogonin B, Ruscus aculeatus L. sapogenin, all or part of kind in the cupreol, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with acetonitrile, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 6: adopt schisandrin in high effective liquid chromatography for measuring this product, schisantherin B, deoxyschizandrin, schisandrin B, schisandrin C, and the cruel first of Fructus Schisandrae Chinensis, all or part of kind in the cruel second of Fructus Schisandrae Chinensis, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, acetonitrile, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 7: adopt evaporative light scattering detector and high performance liquid chromatography coupling method to measure astragaloside in this product, kaempferol, Quercetin, all or part of kind in the isorhamnetin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, acetonitrile, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 8: adopt astragaloside in tlc determination this product, kaempferol, Quercetin, all or part of kind in the isorhamnetin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use silica gel G or silica GF254 or silica gel H to be lamellae, the point sample amount is arbitrary volume between 0.5～30ul, with astragaloside, kaempferol, Quercetin, all or part of kind product in contrast in the isorhamnetin, sample pre-treatments comprises direct sample, method with reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be ethyl acetate, methanol, water, normal hexane, chloroform, acetone, n-butyl alcohol, diethylamine, pyridine, toluene, formic acid, cyclohexane extraction, benzene, glacial acetic acid, one or more reagent in the petroleum ether are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with ethanol solution of sulfuric acid, concentrated sulfuric acid aqueous solution, the anisaldehyde sulfuric acid solution, 10% sulfuric acid solution, method for scanning is carried out with thin-layer chromatogram scanner in solution such as 5% ferric chloride alcoholic solution colour developing back;
Method 9: adopt Tanshinone I in high effective liquid chromatography for measuring this product, tanshinone, Tanshinone II B, salvianolic acid A, salvianolic acid B, salvianolic acid C, danshensu, all or part of kind in the danshensuan B, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, acetonitrile, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 10, adopt high performance liquid chromatography or employing evaporative light scattering detector and high performance liquid chromatography coupling method to measure ligustrazine in this product, ferulic acid, adenine, adenosine, all or part of kind in the vanillin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, acetonitrile, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
All or part of kind in hyperin, vitexin, oleanolic acid, ursolic acid, the Fumaric acid in method 11, employing high effective liquid chromatography for measuring this product, sample pre-treatments comprises direct sample, with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, is mobile phase with one or more kind solvents in methanol, water, acetonitrile, glacial acetic acid, oxolane, the phosphoric acid solution under the proper ratio condition of routine, detects wavelength in 200～600nm scope;
The method of quality control of the YIXINSHU Chinese medicine preparation of a kind of Yiqi and vein recovery of the present invention, blood circulation promoting and blood stasis dispelling, for the assay technology, can also adopt all or part of method as quality control in the following method:
Method 1, for the content assaying method of Radix Ginseng: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Radix Ginseng control medicinal material, the panoxadiol, the panaxatriol, the ginsenoside Rd, the ginsenoside Rb1, the ginsenoside Rf, the ginsenoside Rg3, the ginsenoside Rg1, ginsenoside Rb3, all or part of kind product in contrast among the ginsenoside Re, sample pre-treatments comprises direct sample or with the method for refining reconcentration behind ethanol or methanol or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be chloroform, acetone, formic acid, water, methanol, dichloromethane, ethyl acetate, glacial acetic acid, in the n-butyl alcohol one or more are formulated according to a certain percentage, coloration method comprise spray with 2-30% sulphuric acid ethanol or the spray with 1-10% triketohydrindene hydrate alcoholic solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 500～750nm;
Method 2, for the discrimination method of Radix Ophiopogonis: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with control medicinal material Radix Ophiopogonis, ophiopogonin D, ruscogenin, diosgenin, ophiopogonin B, Ruscus aculeatus L. sapogenin, cupreol, all or part of kind product in contrast in the glucose, sample pre-treatments comprises direct sample or with reconcentration behind ethanol or methanol or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, the method of acid hydrolysis, developing solvent can be ethyl acetate, methanol, water, normal hexane, chloroform, acetone, n-butyl alcohol, diethylamine, pyridine, toluene, formic acid, cyclohexane extraction, benzene, glacial acetic acid, one or more reagent in the petroleum ether are formulated according to a certain percentage, coloration method comprises that spray is with ethanol solution of sulfuric acid or concentrated sulfuric acid aqueous solution or anisaldehyde sulfuric acid solution or 10% sulfuric acid solution or 5% ferric chloride alcoholic solution, speckle adopts the scanning of single wavelength fixed point on thin-layer chromatogram scanner, scanning wavelength is 500～700nm;
Method 3, for the discrimination method of Fructus Schisandrae Chinensis: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Fructus Schisandrae Chinensis control medicinal material, schisandrin, schisantherin B, deoxyschizandrin, schisandrin B, schisandrin C, and schisantherin A, all or part of kind product in contrast in the schisantherin B, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, put under the ultra-violet lamp or adopt and comprise the method for spray with chromotropic acid sulfuric acid solution or anisaldehyde sulfuric acid solution or iodine vapor or 10% phosphomolybdic acid ethanol solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 200～400nm;
Method 4, for the discrimination method of the Radix Astragali: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with Radix Astragali control medicinal material, astragaloside, kaempferol, rutin, Quercetin, Quercitroside, isorhamnetin, all or part of kind product in contrast in the glucose, sample pre-treatments comprises direct sample or with the purified method of reuse chromatography behind water or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be ethyl acetate, methanol, water, normal hexane, chloroform, acetone, n-butyl alcohol, diethylamine, pyridine, toluene, formic acid, cyclohexane extraction, benzene, glacial acetic acid, one or more reagent in the petroleum ether are formulated according to a certain percentage, colour developing comprises the method for spray with ethanol solution of sulfuric acid or concentrated sulfuric acid solution or anisaldehyde sulfuric acid solution or 10% sulfuric acid solution or 5% ferric chloride alcoholic solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 500～750nm;
Method 5, for the discrimination method of Radix Salviae Miltiorrhizae: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Radix Salviae Miltiorrhizae control medicinal material, Tanshinone I, tanshinone, Tanshinone II B, salvianolic acid A, salvianolic acid B, salvianolic acid C, danshensu, all or part of kind product in contrast in the danshensuan B, sample pre-treatments comprises direct sample or with reconcentration method behind water or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, put under the ultra-violet lamp or adopt ammonia smoked after put ultra-violet lamp under again or method that spray develops the color with chromotropic acid sulfuric acid solution or anisaldehyde sulfuric acid solution or iodine vapor or 10% phosphomolybdic acid ethanol solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 400～750nm;
Method 6, for the discrimination method of Rhizoma Chuanxiong: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin, sample pre-treatments comprises reconcentration method behind direct sample or ethanol or methanol or water or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be chloroform, methanol, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, put under the ultra-violet lamp or adopt ammonia smoked after put again and inspect under the ultra-violet lamp or spray method with chromotropic acid sulfuric acid solution or anisaldehyde sulfuric acid solution or iodine vapor or the colour developing of 10% phosphomolybdic acid ethanol solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 200～400nm;
Method 7, for the discrimination method of Fructus Crataegi: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Fructus Crataegi control medicinal material, hyperin, vitexin, oleanolic acid, ursolic acid, all or part of kind product in contrast in the Fumaric acid, sample pre-treatments comprises direct sample or with reconcentration method behind ethanol or methanol or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be chloroform, ethyl acetate, acetone, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, colour developing comprises the method for spray with 1～10% ferric chloride alcoholic solution or chromotropic acid sulfuric acid solution or anisaldehyde sulfuric acid solution or iodine vapor or 10% phosphomolybdic acid ethanol solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 450～750nm.
The method of quality control of the YIXINSHU Chinese medicine preparation of a kind of Yiqi and vein recovery of the present invention, blood circulation promoting and blood stasis dispelling, for the assay technology, preferably adopt all or part of method as quality control in the following method:
Method 1: adopt ginsenoside Rg1, ginsenoside Rb1, ginsenoside Re in high effective liquid chromatography for measuring this product, sample pre-treatments is with chloroform, ether mixed solvent extraction according to a certain percentage impurity, use potassium hydroxide, ethanol or methanol, water extraction then, the method of n-butyl alcohol, refining methanol, use the chromatographic column of C18 type filler, is mobile phase with acetonitrile, phosphoric acid, water under the proper ratio condition of routine, and the detection wavelength is 203nm;
Method 2: adopt salvianolic acid B in high effective liquid chromatography for measuring this product, sample pre-treatments is with the method for methanol, ethanol, water extraction, using the chromatographic column of C18 type filler, is mobile phase with methanol, acetonitrile, formic acid, water under the proper ratio condition of routine, and the detection wavelength is 286nm;
Method 3: adopt evaporative light scattering detector and high performance liquid chromatography coupling method to measure astragaloside in this product, sample pre-treatments is with the mixed solvent extraction according to a certain percentage of potassium hydroxide, methanol, water, ethyl acetate, n-butyl alcohol, the purified method of ammonia solution then, using the chromatographic column of C18 type filler, is mobile phase with acetonitrile, water under the proper ratio condition of routine.
Compared with prior art, method of quality control provided by the invention can better be controlled the product quality of the YIXINSHU Chinese medicine preparation of a kind of Yiqi and vein recovery, blood circulation promoting and blood stasis dispelling, guarantee the safety of medication, after using the present invention, from producing, select for use raw material, processing step to each production process all must be carried out in strict accordance with technological procedure, can guarantee the quality of finished drug product; We find when testing: adopt the present invention will require to select for use the grade of Radix Ginseng, the Radix Astragali, Radix Salviae Miltiorrhizae, Radix Ophiopogonis, Fructus Schisandrae Chinensis, Rhizoma Chuanxiong, Fructus Crataegi medical material to reach more than the one-level, otherwise underproof situation can appear in manufactured goods; So more help instruct producing, make technology controlling and process rationally strict more, allow consumer's full appreciation product quality, this quasi drugs of relieved use.The assay index components that the present invention chooses is the effective active composition of this product according to theory of Chinese medical science monarch, minister, the monarch drug of helping, make ordering and ministerial drug, is very necessary to the control drug quality, and is very desirable as the index of content control.Find the Radix Ginseng among the we under study for action, the Radix Astragali, Radix Ophiopogonis, Fructus Crataegi contains a large amount of glycoside materials, and Fructus Schisandrae Chinensis, the Radix Astragali, Radix Ginseng, all contain polysaccharide Radix Ophiopogonis, because the glycoside material is that a class polarity is bigger, baroque chemical compound, its no uv absorption, there is not single-minded developer, add saponin and measure the interference that often is subjected to sugar, when adopting the routine techniques condition to measure, because sensitivity is low during the ultraviolet detection end absorption, noise effect is big, and Interference Peaks is arranged, be difficult to use, therefore, the applicant equates a series of investigations of condition determination through flowing, the assay of final Radix Ginseng is under the mobile phase elution requirement of 0.1% phosphoric acid-acetonitrile (80: 20), investigated respectively in different-waveband typical wavelengths 203,210,230, chromatographic peak situation under 254, the result shows that chromatographic peak is more in Radix Ginseng and the YIXINSHU formulation samples under 203nm, peak shape is better, so select for use 203nm as detecting wavelength; And the assay of Radix Salviae Miltiorrhizae is under the mobile phase elution requirement of methanol-acetonitrile-0.5% aqueous formic acid, investigated the chromatographic peak situation under different-waveband typical wavelengths 224,254,286,300 respectively, the result shows, chromatographic peak is more in Radix Salviae Miltiorrhizae and the YIXINSHU formulation samples under 286nm, peak shape is better, so select for use 286nm as detecting wavelength; So select for use 286nm as detecting wavelength; Because astragaloside only has weak end absorption at the 201nm place, therefore noise is bigger, the separating degree repeatability is relatively poor, the applicant adopts high performance liquid chromatography-evaporative light scattering detector method to carry out the assay of astragaloside in the Radix Astragali, good, the favorable reproducibility of separating degree, response rate height as a result, the collection of illustrative plates that obtains can be good at the testing product quality.So the present invention has selected a series of composition and the method technological means as control, testing product quality, makes the production technology of YIXINSHU Chinese medicine preparation that guarantee arranged, the preparation that obtains is more reliable, has reached the purpose of invention.
Utilize method of quality control provided by the invention for proof and can better control a kind of product quality of giving birth to the YIXINSHU Chinese medicine preparation, the medicine that obtains has effective effect, and the applicant has carried out a series of experiments;
Experimental example 1 ginsenoside Rg 1, the Re assay methodological study
YIXINSHU JIAONANG is made up of seven flavor medicine materials such as Radix Ginseng, Radix Ophiopogonis, Fructus Schisandrae Chinensis, the Radix Astragali, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong and Fructus Crataegis, monarch drug in the Radix Ginseng side of being, it is reported, mainly contain saponins compound in the Radix Ginseng, identified 29 kinds of saponin constituents: ginsenoside (Ginsenoside); The malonyl ginsenoside; Arasaponin (Notogindenoside); Radix Panacis Quinquefolii saponin (Quinqueoside).All saponin constituent is divided into 3 types, that is: the A type comprises ginsenoside Rb 1, Rb 2, Rc, Rd, generate panaxadiol (Panaxadiol) after the hydrolysis; Type B comprises ginsenoside Re, Rf, Rg 1, Rg 2, generate panaxitriol (Panaxtriol) after the hydrolysis; The C type, the ginsenoside Ro is the derivant of oleanolic acid (Oleanolic acid).The assay of chemical constituent in the Radix Ginseng, that bibliographical information is more is the ginsenoside Rg 1, Rb 1, saponins such as Re assay, method for measuring mostly is high performance liquid chromatography, thin layer chromatography scanning etc.The applicant is to the ginsenoside Rg in the YIXINSHU Chinese medicine preparation 1, ginsenoside Re's content measures, and method for measuring studied.
1.1 instrument Waters high performance liquid chromatograph, 2693 infusion pump column oven automatic sampling apparatus; 2487 UV-detector; The Millennium32 chromatographic work station.The HP1100 chromatograph, Chem Station chromatographic work station, diode display detector; The thermocolumn case; TCQ-250 ultrasonic cleaner (Beijing armarium two factories).
1.2 reagent methanol (chromatographically pure, analytical pure), phosphoric acid (analytical pure), potassium hydroxide (analytical pure), ether (analytical pure), chloroform (analytical pure), n-butyl alcohol (analytical pure), ammonia (analytical pure), potassium dihydrogen phosphate (analytical pure), water are pure water; The ginsenoside Rg 1, ginsenoside Re's reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides, for assay usefulness, the ginsenoside Rg 1Lot number: 0703-200221, ginsenoside Re's lot number: 0754-200217).Sample YIXINSHU JIAONANG and negative blank sample (pharmaceutical Co. Ltd of Guizhou letter nation).
1.3 chromatographic condition chromatographic column: Di Ma, C 18(4.6 * 200mm); Mobile phase: 0.1% phosphoric acid solution-acetonitrile (80: 20); Detect wavelength: 203nm; Flow velocity: 1ml/min; Sample size: 10 μ l.
1.4 system suitability test
Get the ginsenoside Rg respectively 1, ginsenoside Re's reference substance solution, need testing solution and the shortage of staff negative blank solution of joining medical material injects chromatograph of liquid, record chromatograph (seeing Fig. 1～3).As seen from the figure, ginsenoside Rg 1, the ginsenoside Re retention time be respectively: 44 minutes and 47 minutes, negative blank chromatogram was the ginsenoside Rg 1, the ginsenoside Re position all do not have peak, ginsenoside Rg 1, other peak that the ginsenoside Re is close with it separates fully (separating degree＞1.5), i.e. ginsenoside Rg under this experimental condition 1, the ginsenoside Re separates with other components fully.In the number of theoretical plate reference substance: the ginsenoside Rg 1, Re is respectively 7952 and 7836; In the number of theoretical plate sample: the ginsenoside Rg 1, the ginsenoside Re is respectively 7889 and 7451.The ginsenoside Rg 1, ginsenoside Re and other component peaks separating degree greater than 1.5.(seeing Fig. 4～5) should be not less than 2500 so decide number of theoretical plate with the calculating of ginsenoside Re peak.
1.5 linear relationship is investigated
1.5.1 the preparation precision of standard solution takes by weighing the ginsenoside Rg 1, ginsenoside Re's reference substance is an amount of, adds dissolve with methanol, make every 1ml and contain the ginsenoside Rg 10.5188mg the mixing reference substance solution of ginsenoside Re 0.4268mg.
1.5.2 accurate above-mentioned mixing reference substance solution 4 μ l, 8 μ l, 12 μ l, 16 μ l, the 20 μ l of drawing of the drafting of standard curve, inject chromatograph of liquid respectively, record chromatograph (seeing Table 1) is carried out linear regression with peak area A to mass number (μ g) and is calculated, and gets equation of linear regression and is:
The ginsenoside Rg 1: A=325872X-14655, r=0.9999 (ginsenoside Rg 1Good in 2.0752～10.376 μ g scope internal linear relation.)
Ginsenoside Re: A=292726X-111543, (ginsenoside Re is good in 1.7072～8.5360 μ g scope internal linear relation for r=0.9999.)
Table 1 ginsenoside Rg 1, the Re linear relationship investigates
Experiment number The ginsenoside Rg 1 The ginsenoside Re
Sample size (μ g) Peak area Sample size (μ g) Peak area
1 2 3 4 5 2.0752 4.1504 6.2256 8.3008 10.376 653797 1329482 2035711 2703370 3348097 1.7072 3.4144 5.1216 6.8288 8.5360 395134 868506 1396929 1899491 2378349
1.6 the selective extraction method of need testing solution extraction time: reflux, extract,, measurement result sees Table 2.
The investigation of table 2 different extraction times
Extraction time (min) 20 40 60 80 100
Rg 1Content (mg/g) Re content (mg/g) 0.5905 0.5146 0.7430 0.6471 1.0718 0.7428 1.0170 0.7479 1.0578 0.7393
As seen, 60 minutes extraction times can be with the ginsenoside Rg in the preparation from table 2 1, Re extracts fully, so selection reflux 1 hour.
1.7 precision test
Get the ginsenoside Rg 1, the Re reference substance solution, repeat sample introduction 5 times, measure peak area, the results are shown in Table 3, the ginsenoside Rg 1, Re average peak area be respectively 1632643,1142200; RSD is respectively 0.98%, 2.2%.
The precision test that table 3 ginsenoside measures
The sample introduction number of times 1 2 3 4 5 Meansigma methods RSD(％)
Rg 1Peak area Re peak area 1628349 1118262 1623847 1161310 1612807 1174360 1648673 1119948 1649539 1137120 1632643 1142200 0.98 2.19
1.8 replica test
Get this product (lot number: 20020509) content, press in quality standard (revision) text preparation method of test liquid under the assay item, 5 parts of test solutions of parallel preparation, difference sample introduction 10 μ l, measure peak area, result of calculation is listed table 4 in, and the average content of ginsenoside Rg1, Re is respectively 0.1035% and 0.0696%, and RSD is respectively 2.41%, 1.91%.
Ginsenoside's repeatability test in table 4 YIXINSHU JIAONANG
The sample introduction number of times 1 2 3 4 5 Meansigma methods RSD(％)
Rg 1Content (%) Re content (%) 0.1061 0.0706 0.1038 0.0701 0.1056 0.0677 0.1024 0.0688 0.0999 0.0708 0.1036 0.0696 2.43 1.89
1.9 stability test
Get this product (lot number: 20020509) content, preparation method by test liquid under the assay item in quality standard (revision) text prepares test liquid, measure ginsenoside's peak area respectively at 0,1,2,4,8,12 hour sample introduction, the result lists table 5 in, the ginsenoside Rg 1, the Re average peak area is respectively 1643149,1091529, RSD is respectively 0.78% and 0.73%, illustrates that test liquid is good at 12 hours internal stabilities.
Ginsenoside's stability test in table 5 YIXINSHU JIAONANG
Minute (h) 0 1 2 4 8 12 Meansigma methods RSD(％)
Rg 1Peak area Re peak area 1641639 1091886 1648022 1092542 1627485 1081204 1665395 1105656 1636028 1088358 1640327 1089525 1643149 1091528 0.78 0.73
1.10 recovery test
Adopt the application of sample absorption method, precision takes by weighing 5 parts of sample (ginsenoside Rgs that measured content respectively 1, Re content be respectively 0.1036% and 0.0696%) about 2g, accurate add the ginsenoside Rg 1(0.5064mg/ml), the reference substance mixed solution 4.0ml of Re (0.4084mg/ml) puts in the apparatus,Soxhlet's, and it is an amount of to add chloroform-ether (1: 1), reflux 3 hours discards chloroform solution, and medicinal residues volatilize solvent, move in the tool plug conical flask together with filtration paper cylinder, add 2% potassium hydroxide methanol solution 50ml, reflux 1 hour, take off, put coldly, filter, wash residue 3 times with small amount of methanol, merge washing liquid and filtrate, put evaporate to dryness in the evaporating dish, residue adds water 50ml dissolving bottle and is transferred in the separatory funnel, with 4 (20ml of water saturated n-butanol extraction, 20ml, 10ml, 10ml), merge n-butyl alcohol liquid, n-butyl alcohol liquid is used ammonia solution respectively, water, 1% potassium dihydrogen phosphate respectively washs 1 time, and each 40ml discards cleaning mixture, n-butyl alcohol liquid is put evaporate to dryness in the evaporating dish, residue adds dissolve with methanol, and moves in the 5ml measuring bottle, is diluted to scale with methanol, shake up, filter with microporous filter membrane (0.45 μ m), measure, the results are shown in Table 6,7.
Ginsenoside Rg in table 6 YIXINSHU JIAONANG 1Recovery test
Test number (TN) Sample size (g) Contain ginsenoside (mg) Add ginsenoside (mg) The amount of recording (mg) The response rate (%) Average recovery rate (%) RSD (％)
1 2 3 4 5 2.6173 2.0381 2.3017 2.0071 2.3124 2.7115 2.1115 2.3846 2.0794 2.3956 2.0256 2.0256 2.0256 2.0256 2.0256 4.7229 4.1343 4.3615 4.0689 4.3980 99.30 99.86 97.60 98.22 98.85 98.77 0.90
Ginsenoside Re's recovery test in table 7 YIXINSHU JIAONANG
Test number (TN) Sample size (g) Contain ginsenoside (mg) Add ginsenoside (mg) The amount of recording (mg) The response rate (%) Average recovery rate (%) RSD (％)
1 2 3 4 5 2.6173 2.0381 2.3017 2.0071 2.3124 1.8216 1.4185 1.6020 1.3969 1.6094 1.6336 1.6336 1.6336 1.6336 1.6336 3.4450 3.0262 3.2199 2.9904 3.2230 99.38 98.41 99.04 97.54 98.78 98.63 0.72
1.11 sample determination
Press quality standard (revision) preparation test sample and reference substance solution, sample introduction 10 μ l write down chromatograph respectively, measure peak area, are calculated as follows content:
Figure A20071007772500391
In the formula: Ai: need testing solution peak area W: test sample claims sample (g)
As: reference substance solution peak area W 1: average particle heavy (g)
Cs: reference substance solution concentration (mg/ml)
The ginsenoside total quantitative determination the results are shown in Table 8 in 10 batch samples.
Ginsenoside total quantitative determination result in table 8 10 batch samples
Lot number The ginsenoside Rg 1Content (mg/ grain) Ginsenoside Re's content (mg/ grain) Ginsenoside's total amount
1 2 Meansigma methods 1 2 Meansigma methods
20020509 20020615 20020702 20021122 20021203 20030107 20030117 20030214 20030508 20030610 0.321 0.202 0.229 0.131 0.243 0.236 0.325 0.252 0.287 0.237 0.294 0.212 0.218 0.139 0.219 0.227 0.298 0.229 0.304 0.208 0.308 0.207 0.224 0.135 0.231 0.232 0.312 0.240 0.296 0.222 0.257 0.176 0.177 0.105 0.198 0.183 0.666 0.328 0.323 0.202 0.268 0.173 0.169 0.112 0.173 0.182 0.618 0.393 0.364 0.186 0.262 0.174 0.173 0.108 0.186 0.182 0.642 0.360 0.344 0.194 0.570 0.381 0.397 0.243 0.417 0.414 0.954 0.600 0.640 0.416
According to 10 batch sample measurement results, ginsenoside Rg 1With ginsenoside Re's total amount in 0.243～0.954mg/ grain scope, so tentative every of this product contains Radix Ginseng with the ginsenoside Rg 1(C 42H 72O 14) and ginsenoside (C 48H 82O 18) total, must not be less than 0.20mg.
Experimental example 2 content of danshinolic acid B methods for measuring are investigated
2.1 instrument condition: Tianjin, island high performance liquid chromatograph, LC-2010A HT.
2.2 reagent: methanol (chromatographically pure, analytical pure), acetonitrile (chromatographically pure), formic acid (analytical pure), water are high purity water; Salvianolic acid B reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides, and uses for assay), sample YIXINSHU JIAONANG (pharmaceutical Co. Ltd of Guizhou letter nation).
2.3 chromatographic condition: chromatographic column: VP-ODS; Mobile phase: methanol-acetonitrile-0.5% aqueous formic acid (28: 8: 64) column temperature: 30 ℃; Detect wavelength: 286nm; Flow velocity: 1ml/min; Sample size: 10ul.
2.4 system suitability test
Get the salvianolic acid B reference substance respectively, (lot number: 20051201) solution lacks the negative blank solution injecting chromatograph of red rooted salvia to the YIXINSHU JIAONANG test sample, the record chromatogram, from figure, the retention time of salvianolic acid B is 16.1 minutes, negative blank chromatogram is at salvianolic acid B position Wu Feng, other peak separating degrees complete (separating degree＞1.5) that salvianolic acid B is close with it, and promptly salvianolic acid B separates with other components fully under this experiment condition.In the theoretical cam curve reference substance: be 2952; In the theoretical cam curve sample: salvianolic acid B is 2965; The separating degree of salvianolic acid B and other component peaks is greater than 1.5.So theoretical cam curve is calculated with the salvianolic acid B peak, should be not less than 2000.
2.5 linear relationship is investigated
2.5.1 the preparation of standard solution
It is an amount of that precision is got the salvianolic acid B reference substance, adds dissolve with methanol, makes the reference substance solution that every 1ml contains salvianolic acid B 0.1392mg.
2.5.2 the drafting of standard curve
Accurate above-mentioned reference substance solution 1ul, 2ul, 4ul, 8ul, 12ul, 16ul, the 20ul of drawing.Inject chromatograph of liquid respectively, the record chromatograph the results are shown in Table 9, with peak area A mass number X (μ g) is carried out linear regression and calculates, and gets equation of linear regression and is:
Salvianolic acid B: A=1015012X-28940, r=0.9995 (salvianolic acid B is good in 0.1392 μ g～2.784 μ g scope internal linear relation).
Table 9 salvianolic acid B linear relationship is investigated
Experiment number 1 2 3 4 5 6 7
Sample introduction (μ g) peak area 0.1392 132194 0.2784 267205 0.5568 537111 1.1136 1084428 1.6704 1629014 2.2272 2198719 2.784 2850002
2.6 the selective extraction method of need testing solution extraction time: reflux, extract, (75% methanol), measurement result table 10.
Table 10 different time extracts investigates (sample: YIXINSHU JIAONANG 20051201)
Extraction time (min) 20 40 60 80 100
Sample weighting amount g peak area content (mg/g) 1.1290 492031 2.21 1.1207 490495 2.22 1.1508 522577 2.31 1.1330 514279 2.30 1.1099 505094 2.31
Result: from table 10, as seen, extract and the salvianolic acid B in the preparation can be extracted fully in 60 minutes, so select heating and refluxing extraction 1 hour.
2.7 precision test
Get salvianolic acid B reference substance 10ul, repeat sample introduction 6 times, measure peak area, ask average peak area and relative mean standard deviation (RSD).The results are shown in Table 11:
The precision test that table 11 salvianolic acid B is measured
The sample introduction number of times 1 2 3 4 5 6 Meansigma methods RSD(％)
The salvianolic acid B peak area 1366776 1364923 1375889 1356356 1361092 1359636 1364112 0.50％
2.8 stability test
Get this product (lot number: 20051201) content, put in the tool plug conical flask, the accurate 75% methanol 50ml that adds claims decide weight, reflux 1 hour is taken out and is put coldly, supplies the weight that subtracts mistake with 75% methanol, shakes up, filtration promptly gets need testing solution.Measure respectively at 0,1,2,4,8,12 hour, the result lists table 12 in, and the salvianolic acid B average peak area is 528853, and RSD is 1.69%, illustrates that need testing solution is good at 12 hours internal stabilities.
Salvianolic acid B is measured stability test in table 12 YIXINSHU JIAONANG
Minute (h) 0 1 2 4 8 12 Meansigma methods RSD(％)
The salvianolic acid B peak area 522577 515294 536223 538599 525078 535349 528853 1.69
2.9 replica test
Get this product (lot number: 20051201) content, preparation method is the same, 5 parts of test liquids of parallel preparation, respectively sample introduction 10 μ l measure peak area, result of calculation sees Table 13, the average content of salvianolic acid B is 2.35mg/g, RSD is 1.56%.
Salvianolic acid B is measured replica test in table 13 YIXINSHU JIAONANG
The sample introduction number of times 1 2 3 4 5 Meansigma methods RSD(％)
Sample weighting amount g peak area content (mg/g) 1.0250 427369 2.38 1.0055 420919 2.39 1.0031 408253 2.33 1.0004 401721 2.30 1.0056 413321 2.35 2.35 1.56
2.10 recovery test
Adopt the application of sample absorption method, precision takes by weighing 6 parts of about 0.5g of sample (content of salvianolic acid is 2.35mg/g) that measured content respectively, and accurate salvianolic acid B (0.2304mg/ml) the contrast liquid 5ml that adds puts in the tool plug conical flask, add 75% methanol to 50ml, claim to decide weight, reflux 1 hour, taking-up is put cold, supply the weight that subtracts mistake with 75% methanol, shake up, filter, promptly get need testing solution.Accurate respectively each the 10 μ l of above-mentioned test liquid that draw, injecting chromatograph is measured, promptly.The results are shown in Table 14.
(lot number: salvianolic acid B is measured recovery test to table 14 YIXINSHU JIAONANG 20051201)
Test number (TN) Sample size (g) Contain salvianolic acid B (mg) Add salvianolic acid B (mg) The amount of recording (mg) The response rate (%) Average recovery rate (%) RSD (％)
1 2 3 4 5 6 0.5001 0.5009 0.5008 0.5003 0.5018 0.5062 1.1752 1.1771 1.1769 1.1757 1.1792 1.1896 1.152 1.152 1.152 1.152 1.152 1.152 2.3588 2.3028 2.2979 2.2831 2.3374 2.3289 102.7 97.7 97.3 96.1 100.5 98.9 98.9 2.43
2.11 sample determination
Prepare test liquid and contrast solution by preceding method, sample introduction 10 μ l write down chromatogram respectively, measure peak area, calculate content by external standard method, and the content of danshinolic acid B measurement result sees Table 15 in 10 batch samples.
Content of danshinolic acid B measurement result in table 15 10 batch samples
Lot number Content (%) Meansigma methods mg/g RSD％
1 2
20060301 20060201 20051201 20050102 20060502 20050601 20060701 20060801 20060401 20051001 3.40 4.55 2.42 2.71 3.24 3.80 3.00 2.97 2.08 1.00 3.35 4.57 2.36 2.72 3.29 3.88 2.99 2.99 2.04 0.99 3.38 4.56 2.39 2.72 3.26 3.84 3.00 2.98 2.06 1.00 1.05 0.31 1.77 0.26 1.08 1.47 0.24 0.24 1.37 0.71
Experimental example 3 Astragaloside content methods for measuring are investigated
3.1 instrument condition: Tianjin, island high performance liquid chromatograph, LC-2010A HT; Evaporative light scattering detection: ELSD2000
3.2 reagent: acetonitrile is a chromatographically pure, and methanol, ethyl acetate, n-butyl alcohol, ammonia are analytical pure, and potassium hydroxide is a chemical pure, and water is redistilled water; Astragaloside (Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides, and uses for assay), sample YIXINSHU JIAONANG (pharmaceutical Co. Ltd of Guizhou letter nation).
3.3 chromatographic condition: chromatographic column: the U.S. C18 of Phenomenex company post; Mobile phase: acetonitrile-water (37: 63) column temperature: 25 ℃; Flow velocity: 0.5ml/min; ELSD drift tube temperature: 100 ℃; Flow rate of carrier gas: 2.7L/min; Sample size: 10ul.
3.4 system suitability test
Get the astragaloside reference substance respectively, (lot number: 20051201) solution lacks the negative blank solution injecting chromatograph of Milkvetch Root to the YIXINSHU JIAONANG test sample, the record chromatogram, from figure, the retention time of astragaloside is 16.1 minutes, negative blank chromatogram is at astragaloside position Wu Feng, other peak separating degrees complete (separating degree＞1.5) that astragaloside is close with it, and promptly the salvianolic acid B astragaloside separates with other components fully under this experiment condition.
3.5 the standard curve and the range of linearity
Precision takes by weighing astragaloside reference substance 19.8mg, adds the reference substance solution that 50ml methanol is made 0.396mg/ml, in contrast the product stock solution.Accurate respectively above-mentioned reference substance solution 1ml, 3ml, 5ml, 7ml, the 9ml of drawing, put in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, respectively sample introduction 10 (ul), common logarithm value with sample size (ug) is an abscissa, common logarithm value with peak area is a vertical coordinate, makes standard curve, and getting regression equation is Y=4.9358+1.4956X, r=0.9995, sample size is good in 0.396 ~ 3.564ug scope internal linear relation.Because of this standard curve initial point only, sample determination adopts the external standard two-point method to calculate.
3.6 precision experiment
Get with a need testing solution, repeat sample introduction continuously 6 times, each sample introduction 10ul measures peak area, and RSD is 0.48%.
3.7 stability test
Get need testing solution, respectively at 0h, 2h, 4h, 6h, 8h, 24h, sample introduction, carry out stability test, measurement result shows that the astragaloside chromatographic peak area does not have obvious change within 24h.RSD is 1.1%.
3.8 repeatability test
Get same sample 6 parts of test liquids of preparation method preparation by need testing solution, the difference sample introduction, the peak area of mensuration astragaloside calculates content, and RSD is 1.15%.
3.9 recovery test
Precision takes by weighing 18.8mg astragaloside reference substance and puts in the 200ml measuring bottle, adds 2%KOH-methanol and makes dissolving and be diluted to scale, shakes up, in contrast the product stock solution.Precision takes by weighing sample 0.15g, and the accurate reference substance stock solution 5ml that adds makes need testing solution by the method under " 3 " item, and each sample size is 10ul.Average recovery rate is 97.94%, and RSD is 0.68%.
3.10 the assay of sample
Get 10 batch samples, be equipped with test liquid, carry out measurement result and see Table 16 by assay item below legal system:
Astragaloside content measurement result in table 16 10 batch samples
Lot number Astragaloside content mg/g Meansigma methods mg/g RSD％
1 2
20060301 20050102 20051201 20060201 20060502 20050601 20060701 20060401 20060801 20051001 0.1201 0.1198 0.1228 0.1311 0.1243 0.1251 0.1315 0.1225 0.1302 0.1284 0.1221 0.1204 0.1244 0.1291 0.1251 0.1257 0.1303 0.1233 0.1288 0.1276 0.1211 0.1201 0.1236 0.1301 0.1247 0.1254 0.1309 0.1229 0.1295 0.1280 1.17 0.35 0.91 1.10 0.45 0.34 0.65 0.46 0.76 0.44
Specific embodiment
The method of quality control of the YIXINSHU Chinese medicinal capsule agent of 1 one kinds of Yiqi and vein recoveries of embodiment, blood circulation promoting and blood stasis dispelling mainly comprises projects such as discriminating, assay.
1, prescription:
Radix Ginseng 200g 200g Radix Ophiopogonis Fructus Schisandrae Chinensis 133g Radix Astragali 200g
Radix Salviae Miltiorrhizae 267g Rhizoma Chuanxiong 133g Fructus Crataegi 200g
2, method for making: above seven flavors, getting the Radix Ginseng powder, to be broken into behind the fine powder back standby.Fructus Schisandrae Chinensis, Radix Salviae Miltiorrhizae filter with 85% alcohol reflux secondary 3 hours first time 1.5 hours second time, and merging filtrate is evaporated to relative density 1.12～1.15 (80 ℃), gets pure extractum.Decoct with water secondary all the other Radix Ophiopogonis etc., 2.5 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, filtrate is concentrated into about 500ml, adds equivalent 85% ethanol, after fully stirring, standing over night, the elimination precipitate, filtrate recycling ethanol also is concentrated into relative density 1.30～1.36 (80 ℃), gets the water extracted immersing paste.After above-mentioned two kinds of extractum merging, add Radix Ginseng fine powder and appropriate amount of starch, mix homogeneously, drying is pulverized, and crosses 100 mesh sieves, and is encapsulated, makes 1000, promptly.
3, differentiate: (1) gets this product content 5g for the discriminating of Radix Ginseng, adds chloroform-ether (1: 1) 20ml, ultrasonic 30 minutes, discard chloroform-ether solution, medicinal residues volatilize solvent, add methanol 20ml, heated back sulfur 30 minutes, filter, the filtrate evaporate to dryness, residue adds water 30ml makes dissolving, transfers in the separatory funnel, extracts twice with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, wash twice, each 25ml with ammonia solution, twice of the saturated water washing of reuse n-butyl alcohol, each 25ml discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds the 0.5ml dissolve with methanol, as need testing solution.Other gets among ginsenoside Rb1, Re, the Rg1 all or part of kind product in contrast, and reference substance adds methanol and makes solution that every 1ml contains 2mg product solution in contrast.Draw each 10 μ l of above-mentioned reference substance solution, need testing solution 15 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (3: 7: 2), placing stratified lower floor solution below 10 ℃ is developing solvent, launches, take out, dry, spray is heated to clear spot with 10% ethanol solution of sulfuric acid at 105 ℃.Put respectively under daylight and the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, respectively with reference substance chromatograph relevant position on, show the speckle or the fluorescence speckle of same color.
(2) for the discriminating of Radix Ophiopogonis, get this product content 20g, add kieselguhr 20g, add water 50ml and stir, 80 ℃ of dryings 20 minutes, add ethyl acetate 120ml, reflux 1 hour filters, filtrate evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution.Other gets control medicinal material 1g Radix Ophiopogonis, adds water 100ml and decocts 15 minutes, filters, and filtrate is regulated pH to 1 with hydrochloric acid, extracts once with ether 30ml jolting, and ether solution volatilizes, and residue adds ethanol 1ml dissolving, medical material solution in contrast.Drawing each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with chloroform-acetone (4: 1), launches, and takes out, and dries, and spray is heated to clear spot with 10% ethanol solution of sulfuric acid at 105 ℃.Put respectively under daylight and the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, respectively with reference substance chromatograph relevant position on, show the speckle or the fluorescence speckle of same color.
(3) for the discriminating of Fructus Schisandrae Chinensis, get this product content 10g, add chloroform 20ml, reflux 30 minutes filters, and filtrate evaporate to dryness, residue add the 1ml chloroform makes dissolving, as need testing solution.Other gets Fructus Schisandrae Chinensis control medicinal material 10g, gets control medicinal material solution with legal system.Get the deoxyschizandrin reference substance again, add methanol and make the reference substance solution that every 1ml contains 1mg.Draw above-mentioned control medicinal material, each 4 μ l of reference substance solution, need testing solution 10 μ l, putting respectively on same silica GF254 lamellae, is developing solvent with the upper solution of petroleum ether (30-60 ℃)-Ethyl formate-formic acid (15: 5: 1), launches, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, respectively with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of identical color.
(4) for the discriminating of Fructus Crataegi, get this product content 20g, add methanol 50ml, reflux 30 minutes filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, extracts 2 times with the ethyl acetate jolting, each 20ml, combined ethyl acetate, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the ursolic acid reference substance and makes solution that every 1ml contains 1mg product solution in contrast.Drawing each 10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, is developing solvent with cyclohexane extraction-ethyl acetate-formic acid (20: 20: 1), and spray is heated to clear spot with 2% ferric chloride alcoholic solution at 105 ℃.Launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(5) for the discriminating of the Radix Astragali: get this product content 5g, add chloroform-ether (1: 1) 20ml, ultrasonic 30 minutes, discard chloroform-ether solution, medicinal residues volatilize solvent, add methanol 20ml, heated back sulfur 30 minutes, filter, filtrate evaporate to dryness, residue add water 30ml makes dissolving, transfer in the separatory funnel, extract twice with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, wash twice with ammonia solution, each 25ml, the water washing twice that the reuse n-butyl alcohol is saturated, each 25ml, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds the 0.5ml dissolve with methanol, as need testing solution.Other gets Radix Astragali control medicinal material and shines medical material solution in pairs with legal system.Getting the astragaloside reference substance again adds methanol and makes solution that every 1ml contains 2mg product solution in contrast.Draw above-mentioned reference substance solution 10 μ l, need testing solution 15 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (13: 7: 2), placing stratified lower floor solution below 10 ℃ is developing solvent, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃.Put respectively under daylight and the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, respectively with reference substance chromatograph relevant position on, show the speckle or the fluorescence speckle of same color.
(6) for the discriminating of Radix Salviae Miltiorrhizae: get this product content 2g, the 20ml that adds diethyl ether, supersound process 40 minutes filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Radix Salviae Miltiorrhizae control medicinal material 1g, shines medical material solution in pairs with legal system.Get the tanshinone reference substance again, add ethyl acetate and make the solution that every 1ml contains 2mg, in contrast product solution.Drawing each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, is that developing solvent launches with benzene-ethyl acetate (19: 1), takes out, and dries.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical kermesinus speckle.
(7) for the discriminating of Rhizoma Chuanxiong: get this product content 20g, add ethyl acetate 60ml, reflux, extract, 30min filters, and filtrate is used 5%NaHNO 3Solution extraction 3 times merges the aqueous alkali layer, is acidified to pH1 with dilute sulfuric acid, with extracted with diethyl ether 3 times, combined ether layer, is recycled to driedly, adds methanol 1m and makes dissolving, as need testing solution.Other gets the Rhizoma Chuanxiong control medicinal material and prepares control medicinal material solution as stated above.Get the ferulic acid reference substance more in addition, add methanol and be mixed with the reference substance solution that contains 0.5mg among every 1ml.Draw each 10 μ l of above-mentioned solution respectively, point is on same silica gel G-CMC lamellae, with benzene-ethyl acetate-glacial acetic acid (4: 1: 0.3) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
4, assay: (1) adopts high effective liquid chromatography for measuring for the assay of Radix Ginseng.
The test of chromatographic condition system suitability is a filler with octadecylsilane chemically bonded silica; 0.1% phosphoric acid-acetonitrile (80: 20) is mobile phase; Flow velocity: 1ml/min; Detect wavelength 203nm.Number of theoretical plate calculates with the ginsenoside Re peak should be not less than 2500.
The preparation precision of reference substance solution takes by weighing the ginsenoside Rg 1Reference substance 12.5mg, ginsenoside Re 10mg add methanol and make every 1ml respectively and contain the ginsenoside Rg 10.5mg, the solution of ginsenoside Re 0.4mg, promptly.
The content of 30 of this product is got in the preparation of need testing solution, and accurate the title decided mixing, get 4g, the accurate title, decide, and puts in the apparatus,Soxhlet's, it is an amount of to add chloroform-ether (1: 1), and reflux 3 hours discards chloroform-ether solution, medicinal residues volatilize solvent, move in the tool plug conical flask together with filtration paper cylinder, add 2% potassium hydroxide alcohol liquid 50ml, reflux 1 hour is taken off, and puts cold, filter, wash residue 3 times, merge washing liquid and filtrate with small amount of methanol, put evaporate to dryness in the evaporating dish, residue adds water 50ml dissolving bottle and moves in the separatory funnel, with 4 (20ml of water saturated n-butanol extraction, 20ml, 10ml 10ml), merges n-butyl alcohol liquid, n-butyl alcohol liquid is put evaporate to dryness in the evaporating dish, residue adds dissolve with methanol and moves in the 5ml measuring bottle, is diluted to scale with methanol, shakes up, filter with microporous filter membrane (0.45 μ m), promptly.
Accurate respectively above-mentioned reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
This product contains the ginsenoside Rg 1(C 42H 72O 14) and ginsenoside Re (C 48H 82O 18Total amount must not be less than 0.5mg/g.
(2) for the assay of Radix Salviae Miltiorrhizae, adopt high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test octadecylsilane chemically bonded silica are filler; Mobile phase: methanol-acetonitrile-0.5% aqueous formic acid (28: 8: 64); Flow velocity: 1ml/min; Detect wavelength: 286nm.Theoretical pedal number calculates with the salvianolic acid B peak and is not less than 2000.
Reference substance solution prepares precision, and to take by weighing the salvianolic acid B reference substance an amount of, adds methanol and make the solution that every 1ml contains 0.14mg, promptly.
This product content 1g is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug conical flask, the accurate 75% methanol 50ml that adds.Claim decide weight, reflux 1 hour is taken out, and puts coldly, claims to decide weight again, supplies the weight that subtracts mistake with 75% methanol, shakes up, and filtration is got subsequent filtrate, promptly.
Accurate respectively above-mentioned contrast liquid and the need testing solution 10ul of drawing of algoscopy injects high performance liquid chromatograph, measures, promptly.
This product contains salvianolic acid B (C 36H 30O 16) must not be less than 1.0mg/g.
(3) for the assay of the Radix Astragali, adopt high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test octadecylsilane chemically bonded silica are filler; Mobile phase: acetonitrile-water (37: 63); Flow velocity: 0.5ml/min; Evaporative light scattering detection: ELSD drift tube temperature: 100 ℃; Flow rate of carrier gas: 2.7L/min; Sample size: 10ul.
Reference substance solution prepares precision, and to take by weighing the astragaloside reference substance an amount of, adds methanol and make the solution that every 1ml contains 0.4mg, promptly.
This product content 1g is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug conical flask, the accurate 2%KOH-methanol 50ml that adds, backflow 1h, methanol extract liquid steam to do to the greatest extent, add water 20ml make dissolving after, be transferred in the separatory funnel, use ethyl acetate extraction 2 times, each 20ml; Merge ethyl acetate liquid, add water 15ml washing, merge water liquid; With water saturation n-butanol extraction 4 times, each 20ml; Merge n-butanol extracting liquid, with ammonia solution washing 3 times, each 20ml; Discard ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue add methanol makes solution transfer to the 5ml measuring bottle, adds methanol to scale, shakes up, and filters with the 0.45um microporous filter membrane, promptly.
Accurate respectively above-mentioned contrast liquid and the need testing solution 10ul of drawing of algoscopy injects high performance liquid chromatograph, measures, promptly.
This product contains astragaloside (C 11H 68O 14) must not be less than 0.125mg/g.
The method of quality control of the YIXINSHU Chinese medicinal capsule agent of 2 one kinds of Yiqi and vein recoveries of embodiment, blood circulation promoting and blood stasis dispelling mainly comprises projects such as discriminating, assay.
1, prescription:
Radix Ginseng 200g 200g Radix Ophiopogonis Fructus Schisandrae Chinensis 133g Radix Astragali 200g
Radix Salviae Miltiorrhizae 267g Rhizoma Chuanxiong 133g Fructus Crataegi 200g
2, method for making: above seven flavors, getting the Radix Ginseng powder, to be broken into behind the fine powder back standby.Fructus Schisandrae Chinensis, Radix Salviae Miltiorrhizae filter with 85% alcohol reflux secondary 3 hours first time 1.5 hours second time, and merging filtrate is evaporated to relative density 1.12～1.15 (80 ℃), gets pure extractum.Decoct with water secondary all the other Radix Ophiopogonis etc., 2.5 hours for the first time, 1.5 hours for the second time, collecting decoction, filter, filtrate is concentrated into about 500ml, adds equivalent 85% ethanol, after fully stirring, standing over night, the elimination precipitate, filtrate recycling ethanol also is concentrated into relative density 1.30～1.36 (80 ℃), gets the water extracted immersing paste.After above-mentioned two kinds of extractum merging, add Radix Ginseng fine powder and appropriate amount of starch, mix homogeneously, drying is pulverized, and crosses 100 mesh sieves, and is encapsulated, makes 1000, promptly.
3, differentiate: (1) gets this product content 20g for the discriminating of Radix Ginseng, uses n-butyl alcohol reflux, extract, 30 minutes, filter, filtrate evaporate to dryness, residue add vitriolic 45% alcoholic solution 20ml, reflux 1 hour, fling to ethanol, extract chloroform, wash with water to neutrality with chloroform 10ml jolting, with an amount of anhydrous sodium sulfide dehydration, filter, filtrate is concentrated into 1ml, as need testing solution.Other gets Radix Ginseng control medicinal material 2g, shines medical material solution in pairs with legal system.Get in panoxadiol's reference substance, the panaxatriol's reference substance all or part of kind product in contrast again, reference substance adds dehydrated alcohol and makes solution that every 1ml contains 1mg product solution in contrast.Draw above-mentioned each solution 10 μ l, putting respectively on same silica gel g thin-layer plate, is developing solvent with cyclohexane extraction-acetone (2: 1), launches, take out, dry, spray is with the sulphuric acid methanol solution, about 10 minutes of 105 ℃ of heating, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with control medicinal material, reference substance chromatograph relevant position on, show the fluorescence speckle of same color.
(2) for the discriminating of Radix Ophiopogonis, get this product content 20g, extracted 30 minutes with methanol eddy, filter, filtrate evaporate to dryness, residue add 20ml water makes dissolving, use the ether washed twice, each 10ml discards, continue with water saturated n-butanol extraction 4 times each 15ml, merging n-butyl alcohol liquid, wash 2 times with ammonia solution, each 10ml discards ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue 5ml dissolve with methanol is as need testing solution.Other gets control medicinal material Radix Ophiopogonis, shines medical material solution in pairs with legal system.The ophiopogonin D reference substance of phosphorus pentoxide drying under reduced pressure of learning from else's experience in addition again is an amount of, adds methanol and makes the solution that every 1ml contains ophiopogonin D 0.2mg, in contrast product solution.Above-mentioned each the solution 20 μ l of accurate absorption inject high performance liquid chromatograph respectively, flow velocity: 1.0ml/min, 30 ℃ of column temperatures; 98 ℃ of evaporative light scattering detector drift tube temperatures, gas flow 2.8L; Number of theoretical plate is not less than 3000 by the ophiopogonin D peak.In the test sample chromatograph, with reference substance and the corresponding retention time of control medicinal material chromatograph, show identical chromatographic peak.
(3) for the discriminating of Fructus Schisandrae Chinensis, get this product content 5g, the 20ml that adds diethyl ether, supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add 1ml methanol makes dissolving, as need testing solution.Other gets Fructus Schisandrae Chinensis control medicinal material 2g, gets control medicinal material solution with legal system.Get schisantherin A, schisandrin reference substance again, add methanol respectively and make the reference substance solution that every 1ml contains 0.5mg.Draw above-mentioned control medicinal material, each 10 μ l of reference substance solution, need testing solution 20 μ l, putting respectively on same silica GF254 lamellae, is developing solvent with toluene-ethyl acetate (9: 4), launches, take out, dry, put under the ultra-violet lamp (254nm) and inspect, in the test sample chromatograph, respectively with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of identical color.
(4) for the discriminating of Fructus Crataegi; get this product content 20g; respectively behind supersound extraction 30min, the 20min, filter merging filtrate; filtrate adds 20% hydrochloric acid 25ml; heating in water bath 40min, puts and is chilled to room temperature, volatilizes; residue adds the mobile phase dissolving, as need testing solution with 50ml, 30ml dehydrated alcohol.Other gets Fructus Crataegi control medicinal material 2g, shines medical material solution in pairs with legal system.Getting the vitexin reference substance again adds mobile phase and makes solution that every 1ml contains 0.25mg product solution in contrast.Above-mentioned each the solution 20 μ l of accurate absorption inject high performance liquid chromatograph respectively, mobile phase: acetonitrile-3% acetum (10: 90); Flow velocity: 1.0ml/min; Detect wavelength: 270nm.In the test sample chromatograph, with reference substance and the corresponding retention time of control medicinal material chromatograph, show identical chromatographic peak.
(5) for the discriminating of the Radix Astragali: get this product content 5g, add chloroform-ether (1: 1) 20ml, ultrasonic 30 minutes, discard chloroform-ether solution, medicinal residues volatilize solvent, add methanol 20ml, heated back sulfur 30 minutes, filter, filtrate evaporate to dryness, residue add water 30ml makes dissolving, transfer in the separatory funnel, extract twice with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, wash twice with ammonia solution, each 25ml, the water washing twice that the reuse n-butyl alcohol is saturated, each 25ml, discard water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds the 0.5ml dissolve with methanol, as need testing solution.Other gets Radix Astragali control medicinal material and shines medical material solution in pairs with legal system.Getting the astragaloside reference substance again adds methanol and makes solution that every 1ml contains 2mg product solution in contrast.Draw above-mentioned reference substance solution 10 μ l, need testing solution 15 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (3: 7: 2), placing stratified lower floor solution below 10 ℃ is developing solvent, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃.Put respectively under daylight and the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, respectively with reference substance chromatograph relevant position on, show the speckle or the fluorescence speckle of same color.
(6) for the discriminating of Radix Salviae Miltiorrhizae: get this product content 2g, add water 40ml, supersound process 30 minutes is regulated PH to 1～2 with hydrochloric acid, extracts 2 times with the ether jolting, and each 25ml merges ether solution, volatilizes, and residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Salviae Miltiorrhizae control medicinal material 1g, shines medical material solution in pairs with legal system.Get the danshensu reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Drawing each 8 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with chloroform-acetone-formic acid (20: 4: 0.5), launches, and takes out, and dries, and it is smoked clear to the speckle colour developing to put in the iodine vapor.In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show identical skin dark stain point.
(7) for the discriminating of Rhizoma Chuanxiong: get this product content 20g, add 20ml methanol, supersound extraction 20min filters, and medicinal residues add methanol 20ml supersound extraction 1 time as stated above again, filter, and filtrate merges, and methanol constant volume is to 50ml, and is standby.Other gets control medicinal material 2g, shines medical material solution in pairs with legal system.Get the cnidium lactone reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.Above-mentioned each the solution 20 μ l of accurate absorption inject high performance liquid chromatograph respectively, mobile phase: methanol-5% isopropanol water solution (55: 45); The detection wavelength is 280nm; Flow velocity is 1ml/min; Column temperature is 25 ℃.In the test sample chromatograph, with reference substance and the corresponding retention time of control medicinal material chromatograph, show identical chromatographic peak.
4, assay: (1) adopts tlc scanning determination for the assay of Radix Ginseng.
Get the about 5g of this product, porphyrize, the accurate title, decide, put in the tool plug conical flask, with water saturated n-butanol extraction 3 times, each 20ml, n-butyl alcohol liquid evaporate to dryness, add 7% sulphuric acid and 45% alcoholic acid mixed solution 20ml, put in the 50ml round-bottomed flask, put in the water-bath hydrolysis 2 hours, ethanol is removed in evaporation in the water-bath, move in the 60ml separatory funnel, water and chloroform are cleaned evaporating dish in right amount respectively and are incorporated into.With chloroform extraction 3 times, each 10ml, chloroform layer be with distillation washing 1 time, water layer with the 10ml chloroform extraction once, combined chloroform is recycled to driedly, residue adds the chloroform dissolving, quantitatively is transferred in the 2ml measuring bottle, and is diluted to scale, shakes up, as need testing solution.Other gets panoxadiol's reference substance chlorination and copies into every 1ml and contain 1mg solution, in contrast product solution.Drawing need testing solution 5 μ l, 10 μ l and reference substance solution 3 μ l, 5 μ l difference cross point on same silica gel g thin-layer plate, is developing solvent with chloroform-ether (1: 2.5), launches, take out, airing, spray are with 10% ethanol solution of sulfuric acid, at 105 ℃ of heating 10min, clear to the speckle colour developing, take out, on lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, retouch instrument, wavelength to thin-layer chromatogram scanner: λ S=530nm, λ R=700nm measures test sample absorbance integrated value and reference substance absorbance integrated value, calculates, promptly
This product contains panoxadiol (C 42H 72O 14) must not be less than the 1.0mg/ grain.
(2) for the assay of Radix Salviae Miltiorrhizae, adopt high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test octadecylsilane chemically bonded silica are filler; Mobile phase: methanol-water (15: 5), detect wavelength: 270nm.Theoretical pedal number calculates with the tanshinone peak and is not less than 2000.
Reference substance solution prepares precision and takes by weighing tanshinone reference substance 10mg, puts in the 50ml brown bottle, adds methanol to scale, shakes up; Precision is measured 2ml, puts in the brown bottle, adds methanol to scale, shakes up, and promptly gets (every ml contains tanshinone 16 μ g).
10 of this product contents are got in the preparation of need testing solution, and inclining content, porphyrize, get 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 10ml that adds, close plug claims to decide weight, reflux 1 hour, put cold, close plug, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly.
Accurate respectively above-mentioned contrast liquid and the need testing solution 10ul of drawing of algoscopy injects high performance liquid chromatograph, measures, promptly.
Every of this product contains tanshinone (C 19H 18O 3) meter, must not be less than 0.10mg.
(3) for the assay of the Radix Astragali, adopt tlc scanning determination.
Get this product 1.75g, precision takes by weighing, and puts tool plug conical flask, precision adds water 25ml, close plug, and jolting makes dissolving, filter, precision is measured subsequent filtrate 10ml, puts in the separatory funnel, with water saturated n-butanol extraction 4 times (25,20,20,20ml), merge n-butyl alcohol liquid, extract 3 times (20 with ammonia solution, 20,20ml), discard ammoniacal liquor, n-butyl alcohol liquid evaporate to dryness, residue add water 3～5ml makes dissolving, puts cold, by D101 type macroporous adsorptive resins (internal diameter 1.5cm, long 12cm), with water 50ml eluting, discard water liquid, reuse 40% ethanol 30ml eluting discards 40% ethanol liquid, continue with 70% ethanol 50ml eluting, collect eluent, evaporate to dryness, with dissolve with methanol and be transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution.Precision takes by weighing the astragaloside reference substance in addition, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (Chinese Pharmacopoeia appendix VIB in 2005), the accurate need testing solution 5 μ l that draw, reference substance solution 2 μ l and 4 μ l, the cross point is on same silica gel g thin-layer plate respectively, with chloroform-methanol-water (30: 10: 1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 105 ℃, take out, on lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan wavelength according to thin layer chromatography (Chinese Pharmacopoeia appendix VIB thin layer chromatography scanning in 2005): λ S=530nm, λ R=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, promptly.
This product contains the Radix Astragali by astragaloside (C 41H 68O 14) meter, every must not be less than 0.3mg.

Claims (8)

1; a kind of Yiqi and vein recovery; the method of quality control of the YIXINSHU Chinese medicine preparation of blood circulation promoting and blood stasis dispelling; mainly comprise discriminating; projects such as assay is characterized in that: it is with the Radix Ginseng control medicinal material; the ginsenoside Rg1; the ginsenoside Re; the ginsenoside Rh2; the panoxadiol; the panaxatriol; the ginsenoside Rb1; the Ginsenoside Rc; the ginsenoside Rb2; Radix Ginseng soap two Rd; the ginsenoside Ra 1; ginsenoside Rh1; the ginsenoside Rf; ginsenoside Rg2; the ginsenoside Rg3; Radix Ophiopogonis control medicinal material; ophiopogonin D; ruscogenin; diosgenin; ophiopogonin B; Ruscus aculeatus L. sapogenin; cupreol; glucose; the Fructus Schisandrae Chinensis control medicinal material; schisandrin; schisantherin B; deoxyschizandrin; schisandrin B; schisandrin C and schisantherin A; schisantherin B; Radix Astragali control medicinal material; acetyl astragaloside I; astragaloside I; astragaloside II; astragaloside III; astragaloside; different astragaloside I; different astragaloside II; astramembrannin; Cycloastragenol; soybean saponin I; formononetin; calycosin; kaempferol; rutin; Quercetin; Quercitroside; isorhamnetin; the rhamnocitrin aglycon; isoquercitrin; the cotton wool astragaloside; cotton wool astragaloside VI; cotton wool astragaloside II; the Radix Salviae Miltiorrhizae control medicinal material; Tanshinone I; tanshinone; Tanshinone II B; cryptotanshinone; salvianolic acid A; salvianolic acid B; salvianolic acid C; salvianolic acid D; salvianolic acid E; salvianolic acid G; salvianolic acid H; salvianolic acid I; salvianolic acid J; the red sour F of tetramethyl; different salvianolic acid C; rosmarinic acid; alkannic acid; Radix Salviae Miltiorrhizae quinone A; Radix Salviae Miltiorrhizae quinone B; Radix Salviae Miltiorrhizae quinone C; danshensu; danshensuan B; the Rhizoma Chuanxiong control medicinal material; ligustrazine; ferulic acid; adenine; adenosine; cnidium lactone; chuanxingol; fourth fork benzene peptide lactones; methyl phenylacetate; vanillin; the Fructus Crataegi control medicinal material; hyperin; vitexin; oleanolic acid; ursolic acid; Fumaric acid; succinic acid; stigmasterol; all or part of kind in the daucosterol is as the detection index of the quality control of this Chinese medicine preparation.
2, according to the described a kind of Yiqi and vein recovery of claim 1, the method of quality control of the YIXINSHU Chinese medicine preparation of blood circulation promoting and blood stasis dispelling is characterized in that: with the panoxadiol, the panaxatriol, the ginsenoside Rd, ginsenoside Rb3, the ginsenoside Rf, the ginsenoside Rg3, the ginsenoside Rg1, the ginsenoside Rb1, the ginsenoside Re, the Radix Ginseng control medicinal material, ophiopogonin D, ophiopogonin B, Radix Ophiopogonis control medicinal material, schisandrin, schisantherin B, deoxyschizandrin, schisandrin B, schisandrin C, and schisantherin A, schisantherin B, the Fructus Schisandrae Chinensis control medicinal material, astragaloside, kaempferol, rutin, Quercetin, Quercitroside, isorhamnetin, Radix Astragali control medicinal material, glucose, Tanshinone I, tanshinone, Tanshinone II B, salvianolic acid A, salvianolic acid B, salvianolic acid C, danshensu, danshensuan B, the Radix Salviae Miltiorrhizae control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, vanillin, the Rhizoma Chuanxiong control medicinal material, hyperin, vitexin, oleanolic acid, ursolic acid, Fumaric acid, all or part of kind in the Fructus Crataegi control medicinal material is as the discrimination method of this Chinese medicine preparation, the detection index of content assaying method.
3, according to the method for quality control of the YIXINSHU Chinese medicine preparation of claim 1 or 2 described a kind of Yiqi and vein recoveries, blood circulation promoting and blood stasis dispelling, it is characterized in that:, adopt all or part of method in the following method as quality control for authentication technique:
Discrimination method for Radix Ginseng: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Radix Ginseng control medicinal material, the panoxadiol, the panaxatriol, the ginsenoside Rd, the ginsenoside Rb1, the ginsenoside Rf, the ginsenoside Rg3, the ginsenoside Rg1, ginsenoside Rb3, all or part of kind product in contrast among the ginsenoside Re, sample pre-treatments comprises direct sample or with the method for refining reconcentration behind ethanol or methanol or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be chloroform, acetone, formic acid, water, methanol, dichloromethane, ethyl acetate, glacial acetic acid, in the n-butyl alcohol one or more are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with 2-30% sulphuric acid ethanol, or spray is with the method for solution such as 1-10% triketohydrindene hydrate ethanol colour developing;
Discrimination method for Radix Ophiopogonis: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with control medicinal material Radix Ophiopogonis, ophiopogonin D, ruscogenin, diosgenin, ophiopogonin B, Ruscus aculeatus L. sapogenin, cupreol, all or part of kind product in contrast in the glucose, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be ethyl acetate, methanol, water, normal hexane, chloroform, acetone, n-butyl alcohol, diethylamine, pyridine, toluene, formic acid, cyclohexane extraction, benzene, glacial acetic acid, one or more reagent in the petroleum ether are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with ethanol solution of sulfuric acid, concentrated sulfuric acid aqueous solution, the anisaldehyde sulfuric acid solution, 10% sulfuric acid solution, the method of solution such as 5% ferric chloride alcoholic solution colour developing;
Discrimination method for Fructus Schisandrae Chinensis: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Fructus Schisandrae Chinensis control medicinal material, schisandrin, schisantherin B, deoxyschizandrin, schisandrin B, schisandrin C, and schisantherin A, all or part of kind product in contrast in the schisantherin B, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with the chromotropic acid sulfuric acid solution, the anisaldehyde sulfuric acid solution, iodine vapor, the method of 10% phosphomolybdic acid ethanol solution solution colour developing;
Discrimination method for the Radix Astragali: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with Radix Astragali control medicinal material, astragaloside, kaempferol, rutin, Quercetin, Quercitroside, isorhamnetin, all or part of kind product in contrast in the glucose, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be ethyl acetate, methanol, water, normal hexane, chloroform, acetone, n-butyl alcohol, diethylamine, pyridine, toluene, formic acid, cyclohexane extraction, benzene, glacial acetic acid, one or more reagent in the petroleum ether are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with ethanol solution of sulfuric acid, concentrated sulfuric acid solution, the anisaldehyde sulfuric acid solution, 10% sulfuric acid solution, the method of solution such as 5% ferric chloride alcoholic solution colour developing;
Discrimination method for Radix Salviae Miltiorrhizae: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Radix Salviae Miltiorrhizae control medicinal material, Tanshinone I, tanshinone, Tanshinone II B, salvianolic acid A, salvianolic acid B, salvianolic acid C, danshensu, all or part of kind product in contrast in the danshensuan B, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with the chromotropic acid sulfuric acid solution, the anisaldehyde sulfuric acid solution, iodine vapor, the method of 10% phosphomolybdic acid ethanol solution solution colour developing;
Discrimination method for Rhizoma Chuanxiong: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with the chromotropic acid sulfuric acid solution, the anisaldehyde sulfuric acid solution, iodine vapor, the method of 10% phosphomolybdic acid ethanol solution solution colour developing;
Discrimination method for Fructus Crataegi: adopt thin layer chromatography, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Fructus Crataegi control medicinal material, hyperin, vitexin, oleanolic acid, ursolic acid, all or part of kind product in contrast in the Fumaric acid, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with 1～10% ferric chloride alcoholic solution, the chromotropic acid sulfuric acid solution, the anisaldehyde sulfuric acid solution, iodine vapor, the method of 10% phosphomolybdic acid ethanol solution solution colour developing.
4, according to the method for quality control of the YIXINSHU Chinese medicine preparation of claim 1 or 2 described a kind of Yiqi and vein recoveries, blood circulation promoting and blood stasis dispelling, it is characterized in that:, adopt all or part of method in the following method as quality control for authentication technique:
Discrimination method for Radix Ginseng: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with the second eyeball, water, methanol, one or more kind solvents in the phosphoric acid are mobile phase under the proper ratio condition of routine, with the Radix Ginseng control medicinal material, the ginsenoside Rg1, the ginsenoside Re, the ginsenoside Rh2, the panoxadiol, the panaxatriol, the ginsenoside Rb1, the Ginsenoside Rc, the ginsenoside Rb2, the ginsenoside Rd, the ginsenoside Ra 1, ginsenoside Rh1, the ginsenoside Rf, ginsenoside Rg2, all or part of kind product in contrast among the ginsenoside Rg3 detect wavelength in 200～600nm scope;
Discrimination method for Radix Ophiopogonis: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with the second eyeball, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with control medicinal material Radix Ophiopogonis, ophiopogonin D, ruscogenin, diosgenin, ophiopogonin B, Ruscus aculeatus L. sapogenin, cupreol, all or part of kind product in contrast in the glucose detect wavelength in 200～600nm scope;
Discrimination method for Fructus Schisandrae Chinensis: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate vinegar or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, the second eyeball, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the suitable ratio condition of routine, with the Fructus Schisandrae Chinensis control medicinal material, schisandrin, schisantherin B, deoxyschizandrin, schisandrin B, schisandrin C, and schisantherin A, all or part of kind product in contrast in the schisantherin B detect wavelength in 200～600nm scope;
Discrimination method for the Radix Astragali: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with the second eyeball, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with Radix Astragali control medicinal material, astragaloside, kaempferol, Quercetin, Quercitroside, isorhamnetin, all or part of kind product in contrast in the glucose detect wavelength in 200～600nm scope;
Discrimination method for Radix Salviae Miltiorrhizae: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with the second eyeball, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with the Radix Salviae Miltiorrhizae control medicinal material, Tanshinone I, tanshinone, Tanshinone II B, salvianolic acid A, salvianolic acid B, salvianolic acid C, danshensu, all or part of kind product in contrast in the danshensuan B detect wavelength in 200～600nm scope;
Discrimination method for Rhizoma Chuanxiong: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with the second eyeball, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin detect wavelength in 200～600nm scope;
Discrimination method for Fructus Crataegi: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with the second eyeball, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, with the Fructus Crataegi control medicinal material, hyperin, vitexin, oleanolic acid, ursolic acid, all or part of kind product in contrast in the Fumaric acid detect wavelength in 200～600nm scope.
5, according to the method for quality control of the YIXINSHU Chinese medicine preparation of claim 3 or 4 described a kind of Yiqi and vein recoveries, blood circulation promoting and blood stasis dispelling, it is characterized in that:, adopt all or part of method in the following method as quality control for authentication technique:
Discriminating for Radix Ginseng: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is 0.5～20 μ l, with the ginsenoside Rb1, Re, all or part of kind product in contrast among the Rg1, sample pre-treatments is with chloroform-ether mixed solvent extraction according to a certain percentage impurity, use ethanol then, methanol, ethyl acetate, a kind of or their any mixed solvents in the water extract back reconcentration method, the reuse n-butyl alcohol, the purified method of water extraction, developing solvent is a chloroform, methanol, water is formulated according to conventional ratio, and the condition of inspecting is the method for spray to inspect under the ultraviolet of 2～30% sulphuric acid ethanol colour developing back;
Discriminating for Radix Ophiopogonis: adopt thin layer chromatography, use silica gel G to be lamellae, the point sample amount is 0.5～20 μ l, with control medicinal material Radix Ophiopogonis product in contrast, sample pre-treatments is with methanol, ethanol, ethyl acetate, ether, acetone, chloroform, dichloromethane, petroleum ether, n-butyl alcohol, a kind of or their any mixed solvents in the water extract back reconcentration method, developing solvent is a chloroform, acetone is formulated according to conventional ratio, and the condition of inspecting is the method liquid of spray to inspect under the ultraviolet of 2～30% sulphuric acid ethanol colour developing back, concentrated sulfuric acid aqueous solution, the anisaldehyde sulfuric acid solution, 10% sulfuric acid solution, the method of 5% ferric chloride alcoholic solution solution colour developing;
Discriminating for Fructus Schisandrae Chinensis: adopt thin layer chromatography, use silica gel G F 254Lamellae, the point sample amount is an a certain volume between 0.5～20 μ l, with Fructus Schisandrae Chinensis control medicinal material, deoxyschizandrin product in contrast, sample pre-treatments is that a kind of or their any mixed solvents in chloroform, dichloromethane, ethyl acetate, acetone, Ethyl formate, n-butyl alcohol, benzene, toluene, methanol, ethanol, ether, the petroleum ether extract back reconcentration method, developing solvent is the upper strata liquid of petroleum ether, Ethyl formate, formic acid, and the condition of inspecting is that 254nm inspects under the ultra-violet lamp.
Discriminating for the Radix Astragali: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is an a certain volume between 0.5 μ l～30 μ l, with Radix Astragali control medicinal material, astragaloside is product in contrast, sample pre-treatments is a chloroform, dichloromethane, ethyl acetate, acetone, Ethyl formate, n-butyl alcohol, benzene, toluene, methanol, ethanol, ether, a kind of or their any mixed solvents in the petroleum ether extract impurity, use ethanol then, methanol, ethyl acetate, a kind of or their any mixed solvents in the water extract back reconcentration method, the reuse n-butyl alcohol, water, ammonia solution extracts purified method, developing solvent is a chloroform, methanol, water formulated according to conventional ratio, the condition of inspecting is the method for spray to inspect under the ultraviolet of 2～30% sulphuric acid ethanol colour developing back;
Discriminating for Radix Salviae Miltiorrhizae: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is an a certain volume between 0.5 μ l～30 μ l, with the Radix Salviae Miltiorrhizae control medicinal material, danshensu, salvianolic acid B, all or part of kind product in contrast in the tanshinone, sample pre-treatments is with chloroform, ether, petroleum ether uses separately or the impurity of mixed solvent extraction according to a certain percentage, use ethanol then, methanol, ethyl acetate, a kind of or dissolved method of they any mixed solvents in the water, developing solvent is a benzene, toluene, ethyl acetate, the condition of inspecting are to inspect under the daylight.
Discriminating for Rhizoma Chuanxiong: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is an a certain volume between 0.5 μ l～30 μ l, with the product in contrast of all or part of kind in Rhizoma Chuanxiong control medicinal material, the ferulic acid, sample pre-treatments is to use separately or the impurity of mixed solvent extraction according to a certain percentage with chloroform, ether, petroleum ether, use a kind of or dissolved method of they any mixed solvents in ethanol, methanol, ethyl acetate, the water then, developing solvent is normal hexane, ethyl acetate, and the condition of inspecting is that 365nm inspects under the ultra-violet lamp.
Discriminating for Fructus Crataegi: adopt thin layer chromatography, use silica gel g thin-layer plate, the point sample amount is an a certain volume between 0.5 μ l～30 μ l, with the product in contrast of all or part of kind in Fructus Crataegi control medicinal material, ursolic acid, hyperin, the vitexin, extract back reconcentration method with a kind of or their any mixed solvents in ethyl acetate, chloroform, dichloromethane, n-butyl alcohol, methanol, ethanol, acetone, the water, developing solvent is cyclohexane extraction, ethyl acetate, formic acid, spray is with 2% ferric chloride alcoholic solution, and the condition of inspecting is to inspect under ultra-violet lamp or the daylight;
6, according to the method for quality control of the YIXINSHU Chinese medicine preparation of claim 1 or 2 described a kind of Yiqi and vein recoveries, blood circulation promoting and blood stasis dispelling, it is characterized in that:, adopt all or part of method in the following method as quality control for the assay technology:
Method 1: with the total saponin content in visible determined by ultraviolet spectrophotometry this product, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, measuring wavelength is a certain wavelength among 200～600nm, adopt standard curve method or reference substance method to measure, reference substance commonly used is Rg1, astragaloside;
Method 2: with the general flavone content in visible determined by ultraviolet spectrophotometry this product, sample pre-treatments comprises direct sample or with the method for reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, measuring wavelength is a certain wavelength among 200～600nm, adopt standard curve method or reference substance method to measure, reference substance commonly used is rutin, Quercetin, Quercitroside;
Method 3: with the total sugar content in visible determined by ultraviolet spectrophotometry this product, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, measuring wavelength is a certain wavelength among 200～650nm, adopt standard curve method or reference substance method to measure, reference substance commonly used is a glucose;
Method 4: with the ginsenoside Rg1 in high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method mensuration this product, the ginsenoside Re, the ginsenoside Rh2, the panoxadiol, the panaxatriol, the ginsenoside Rb1, the Ginsenoside Rc, the ginsenoside Rb2, the ginsenoside Rd, the ginsenoside Ra 1, ginsenoside Rh1, the ginsenoside Rf, ginsenoside Rg2, all or part of kind among the ginsenoside Rg3, sample pre-treatments comprises direct sample or the method for reconcentration behind cruel or chloroform or dichloromethane or the n-butanol extraction with acetic acid second, the chromatographic column of use 8 or C18 type filler, with the second eyeball, water, methanol, one or more kind solvents in the phosphoric acid are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 5: adopt high performance liquid chromatography or evaporative light scattering detector and high performance liquid chromatography coupling method to measure ophiopogonin D in this product, ruscogenin, diosgenin, ophiopogonin B, Ruscus aculeatus L. sapogenin, all or part of kind in the cupreol, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with the second eyeball, water, one or more kind solvents in the methanol are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 6: adopt schisandrin in high effective liquid chromatography for measuring this product, schisantherin B, deoxyschizandrin, schisandrin B, schisandrin C, and the cruel first of Fructus Schisandrae Chinensis, all or part of kind in the cruel second of Fructus Schisandrae Chinensis, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, the second eyeball, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 7: adopt evaporative light scattering detector and high performance liquid chromatography coupling method to measure astragaloside in this product, kaempferol, Quercetin, all or part of kind in the isorhamnetin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, the second eyeball, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 8: adopt astragaloside in tlc determination this product, kaempferol, Quercetin, all or part of kind in the isorhamnetin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use silica gel G or silica GF254 or silica gel H to be lamellae, the point sample amount is arbitrary volume between 0.5～30ul, with astragaloside, kaempferol, Quercetin, all or part of kind product in contrast in the isorhamnetin, sample pre-treatments comprises direct sample, method with reconcentration behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be ethyl acetate, methanol, water, normal hexane, chloroform, acetone, n-butyl alcohol, diethylamine, pyridine, toluene, formic acid, cyclohexane extraction, benzene, glacial acetic acid, one or more reagent in the petroleum ether are formulated according to a certain percentage, and the condition of inspecting comprises under the ultra-violet lamp inspects, put again under the ultra-violet lamp after ammonia is smoked and inspect, or spray is with ethanol solution of sulfuric acid, concentrated sulfuric acid aqueous solution, the anisaldehyde sulfuric acid solution, 10% sulfuric acid solution, method for scanning is carried out with thin-layer chromatogram scanner in solution such as 5% ferric chloride alcoholic solution colour developing back;
Method 9: adopt Tanshinone I in high effective liquid chromatography for measuring this product, tanshinone, Tanshinone II B, salvianolic acid A, salvianolic acid B, salvianolic acid C, danshensu, all or part of kind in the danshensuan B, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, the second eyeball, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
Method 10, adopt high performance liquid chromatography or employing evaporative light scattering detector and high performance liquid chromatography coupling method to measure ligustrazine in this product, ferulic acid, adenine, adenosine, all or part of kind in the vanillin, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, with methanol, water, the second eyeball, glacial acetic acid, oxolane, one or more kind solvents in the phosphoric acid solution are mobile phase under the proper ratio condition of routine, detect wavelength in 200～600nm scope;
All or part of kind in hyperin, vitexin, oleanolic acid, ursolic acid, the Fumaric acid in method 11, employing high effective liquid chromatography for measuring this product, sample pre-treatments comprises direct sample, with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, use the chromatographic column of C8 or C18 type filler, is mobile phase with one or more kind solvents in methanol, water, second eyeball, glacial acetic acid, oxolane, the phosphoric acid solution under the proper ratio condition of routine, detects wavelength in 200～600nm scope;
7, according to the method for quality control of the YIXINSHU Chinese medicine preparation of claim 1 or 2 described a kind of Yiqi and vein recoveries, blood circulation promoting and blood stasis dispelling, it is characterized in that:, adopt all or part of method in the following method as quality control for the assay technology:
Method 1, for the content assaying method of Radix Ginseng: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Radix Ginseng control medicinal material, the panoxadiol, the panaxatriol, the ginsenoside Rd, the ginsenoside Rb1, the ginsenoside Rf, the ginsenoside Rg3, the ginsenoside Rg1, ginsenoside Rb3, all or part of kind product in contrast among the ginsenoside Re, sample pre-treatments comprises direct sample or with the method for refining reconcentration behind ethanol or methanol or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be chloroform, acetone, formic acid, water, methanol, dichloromethane, ethyl acetate, glacial acetic acid, in the n-butyl alcohol one or more are formulated according to a certain percentage, coloration method comprise spray with 2-30% sulphuric acid ethanol or the spray with 1-10% triketohydrindene hydrate alcoholic solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 500～750nm;
Method 2, for the discrimination method of Radix Ophiopogonis: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with control medicinal material Radix Ophiopogonis, ophiopogonin D, ruscogenin, diosgenin, ophiopogonin B, Ruscus aculeatus L. sapogenin, cupreol, all or part of kind product in contrast in the glucose, sample pre-treatments comprises direct sample or with reconcentration behind ethanol or methanol or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, the method of acid hydrolysis, developing solvent can be ethyl acetate, methanol, water, normal hexane, chloroform, acetone, n-butyl alcohol, diethylamine, pyridine, toluene, formic acid, cyclohexane extraction, benzene, glacial acetic acid, one or more reagent in the petroleum ether are formulated according to a certain percentage, coloration method comprises that spray is with ethanol solution of sulfuric acid or concentrated sulfuric acid aqueous solution or anisaldehyde sulfuric acid solution or 10% sulfuric acid solution or 5% ferric chloride alcoholic solution, speckle adopts the scanning of single wavelength fixed point on thin-layer chromatogram scanner, scanning wavelength is 500～700nm;
Method 3, for the discrimination method of Fructus Schisandrae Chinensis: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Fructus Schisandrae Chinensis control medicinal material, schisandrin, schisantherin B, deoxyschizandrin, schisandrin B, schisandrin C, and schisantherin A, all or part of kind product in contrast in the schisantherin B, sample pre-treatments comprises direct sample or with reconcentration method behind ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, put under the ultra-violet lamp or adopt and comprise the method for spray with chromotropic acid sulfuric acid solution or anisaldehyde sulfuric acid solution or iodine vapor or 10% phosphomolybdic acid ethanol solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 200～400nm;
Method 4, for the discrimination method of the Radix Astragali: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with Radix Astragali control medicinal material, astragaloside, kaempferol, rutin, Quercetin, Quercitroside, isorhamnetin, all or part of kind product in contrast in the glucose, sample pre-treatments comprises direct sample or with the purified method of reuse chromatography behind water or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be ethyl acetate, methanol, water, normal hexane, chloroform, acetone, n-butyl alcohol, diethylamine, pyridine, toluene, formic acid, cyclohexane extraction, benzene, glacial acetic acid, one or more reagent in the petroleum ether are formulated according to a certain percentage, colour developing comprises the method for spray with ethanol solution of sulfuric acid or concentrated sulfuric acid solution or anisaldehyde sulfuric acid solution or 10% sulfuric acid solution or 5% ferric chloride alcoholic solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 500～750nm;
Method 5, for the discrimination method of Radix Salviae Miltiorrhizae: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Radix Salviae Miltiorrhizae control medicinal material, Tanshinone I, Tanshinone I I A, Tanshinone I I B, salvianolic acid A, salvianolic acid B, salvianolic acid C, danshensu, all or part of kind product in contrast in the danshensuan B, sample pre-treatments comprises direct sample or with reconcentration method behind water or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be normal hexane, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, put under the ultra-violet lamp or adopt ammonia smoked after put ultra-violet lamp under again or method that spray develops the color with chromotropic acid sulfuric acid solution or anisaldehyde sulfuric acid solution or iodine vapor or 10% phosphomolybdic acid ethanol solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 400～750nm;
Method 6, for the discrimination method of Rhizoma Chuanxiong: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Rhizoma Chuanxiong control medicinal material, ligustrazine, ferulic acid, adenine, adenosine, all or part of kind product in contrast in the vanillin, sample pre-treatments comprises reconcentration method behind direct sample or ethanol or methanol or water or ethyl acetate or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be chloroform, methanol, ethyl acetate, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, put under the ultra-violet lamp or adopt ammonia smoked after put again and inspect under the ultra-violet lamp or spray method with chromotropic acid sulfuric acid solution or anisaldehyde sulfuric acid solution or iodine vapor or the colour developing of 10% phosphomolybdic acid ethanol solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 200～400nm;
Method 7, for the discrimination method of Fructus Crataegi: adopt TLC scanning method, generally use silica gel G or silica gel G F 254Or silica gel H is a lamellae, the point sample amount is arbitrary volume between 0.5～30 μ l, with the Fructus Crataegi control medicinal material, hyperin, vitexin, oleanolic acid, ursolic acid, all or part of kind product in contrast in the Fumaric acid, sample pre-treatments comprises direct sample or with reconcentration method behind ethanol or methanol or chloroform or dichloromethane or the n-butanol extraction, developing solvent can be chloroform, ethyl acetate, acetone, petroleum ether, Ethyl formate, formic acid, dimethylbenzene, toluene, one or more reagent of cyclohexane extraction are formulated according to a certain percentage, colour developing comprises the method for spray with 1～10% ferric chloride alcoholic solution or chromotropic acid sulfuric acid solution or anisaldehyde sulfuric acid solution or iodine vapor or 10% phosphomolybdic acid ethanol solution, speckle adopts single wavelength or dual wavelength to scan on thin-layer chromatogram scanner, and scanning wavelength is 450～750nm.
8, according to the method for quality control of the YIXINSHU Chinese medicine preparation of the described a kind of Yiqi and vein recovery of claim 7, blood circulation promoting and blood stasis dispelling, it is characterized in that:, adopt all or part of method in the following method as quality control for the assay technology:
Method 1: adopt ginsenoside Rg1, ginsenoside Rb1, ginsenoside Re in high effective liquid chromatography for measuring this product, sample pre-treatments is with chloroform, ether mixed solvent extraction according to a certain percentage impurity, use potassium hydroxide, ethanol or methanol, water extraction then, the method of n-butyl alcohol, refining methanol, use the chromatographic column of C18 type filler, is mobile phase with second eyeball, phosphoric acid, water under the proper ratio condition of routine, and the detection wavelength is 203nm;
Method 2: adopt salvianolic acid B in high effective liquid chromatography for measuring this product, sample pre-treatments is with the method for methanol, ethanol, water extraction, using the chromatographic column of C18 type filler, is mobile phase with methanol, acetonitrile, formic acid, water under the proper ratio condition of routine, and the detection wavelength is 286nm.
Method 3: adopt evaporative light scattering detector and high performance liquid chromatography coupling method to measure astragaloside in this product, sample pre-treatments is with the mixed solvent extraction according to a certain percentage of potassium hydroxide, methanol, water, ethyl acetate, n-butyl alcohol, the purified method of ammonia solution then, using the chromatographic column of C18 type filler, is mobile phase with second eyeball, water under the proper ratio condition of routine.
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