CN104623271A - Traditional Chinese medicine composition and determination method thereof - Google Patents
Traditional Chinese medicine composition and determination method thereof Download PDFInfo
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- CN104623271A CN104623271A CN201310555353.3A CN201310555353A CN104623271A CN 104623271 A CN104623271 A CN 104623271A CN 201310555353 A CN201310555353 A CN 201310555353A CN 104623271 A CN104623271 A CN 104623271A
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Abstract
The invention discloses a traditional Chinese medicine composition and a determination method thereof, which belong to the traditional Chinese medicine field. The traditional Chinese medicine composition is composed of gen-seng, coptis, red sage root, Radix Puerariae, anemarrhena, fleece-flower root, epimeddium and the like. The determination method is accurate, and is helpful for controlling the quality of the traditional Chinese medicine composition, and increasing the security and reliability of the traditional Chinese medicine composition.
Description
Technical field
The invention belongs to the field of Chinese medicines, be specifically related to Chinese medicine composition and its discrimination method.
Background technology
Treatment by Chinese herbs disease has the history of several thousand, along with the development of science and technology, Chinese medicine is also faced with modernization, go on world market, this just requires the control must carrying out Chinese medicine quality, and the composition quality of Chinese medicine controls to be then most critical, especially for the Chinese medicine preparation of compound recipe, want the quality comprehensively controlling Chinese medicine, the discriminating of each composition must be carried out.
This Chinese medicine composition is made up of Radix Ginseng, Rhizoma Polygonati, Rhizoma Atractylodis, Radix Sophorae Flavescentis, Radix Ophiopogonis, Radix Rehmanniae, Radix Polygoni Multiflori, Fructus Corni, Poria, Herba Eupatorii, Rhizoma Coptidis, the Rhizoma Anemarrhenae, Herba Epimedii, Radix Salviae Miltiorrhizae, Radix Puerariae, Semen Litchi, Cortex Lycii.For this Chinese medicine composition, only disclose ingredient and preparation method at present, do not provide the discrimination method of corresponding ingredient.
Summary of the invention
The object of the invention is to provide a kind of Chinese medicine composition and differentiates the method for effective ingredient in this Chinese medicine composition.
The technical solution adopted in the present invention is:
A kind of Chinese medicine composition, this Chinese medicine composition is made up of the crude drug of following parts by weight: Radix Ginseng 50-150, Rhizoma Polygonati 60-180, Rhizoma Atractylodis 40-90, Radix Sophorae Flavescentis 30-58, Radix Ophiopogonis 60-180, Radix Rehmanniae 60-110, Radix Polygoni Multiflori 40-90, Fructus Corni 60-180, Poria 40-90, Herba Eupatorii 35-58, Rhizoma Coptidis 35-58, Rhizoma Anemarrhenae 35-90, Herba Epimedii 35-58, Radix Salviae Miltiorrhizae 40-110, Radix Puerariae 60-180, Semen Litchi 80-140, Cortex Lycii 40-90.
The active fraction preparation method of described Chinese medicine composition is made up of following steps:
A, take Chinese crude drug according to crude drug part by weight, clean, cataclasm;
B, Herba Eupatorii, Rhizoma Atractylodis add 5-9 times amount water extraction volatile oil, extract 3-6 hour, and the another device of volatile oil is collected, and aqueous solution is for subsequent use after filtering;
C, Fructus Corni 5-9 times amount 50-90% ethanol make solvent, flood after 12-48 hour, carry out percolation, collect percolate, reclaim ethanol, and be condensed into 60 DEG C measure relative densities be the thick paste of 1.30-1.35, dry, for subsequent use;
D, Radix Ginseng, Radix Ophiopogonis, Herba Epimedii, the Rhizoma Anemarrhenae, Radix Puerariae, add 6-10 times amount 50-90% ethanol, reflux, extract, 1-3 time, each 1-3 hour, extracting liquid filtering, reclaims ethanol, be condensed into thick paste, dries, for subsequent use;
E, Rhizoma Polygonati, Radix Sophorae Flavescentis, Radix Rehmanniae, Radix Polygoni Multiflori, Poria, Rhizoma Coptidis, Radix Salviae Miltiorrhizae, Semen Litchi, Cortex Lycii, add 7-11 times of water gaging, decoct 1-2 time, each 1-3 hour, extracting liquid filtering, carries the aqueous solution after oil merge with Herba Eupatorii, Rhizoma Atractylodis in step b, be condensed into clear paste, adding ethanol regulates determining alcohol to be 50-80%, and cold preservation is placed, and filters, filtrate recycling ethanol, be concentrated into thick paste, dry, for subsequent use;
The active component that cream, the dry cream of step e gained water extract-alcohol precipitation and step b gained volatile oil form this Chinese medicine composition jointly promoted by the dry cream of step c gained Fructus Corni, steps d gained alcohol.
The preparation formulation of this Chinese medicine composition is capsule, tablet or granule.
The preparation of this Chinese medicinal composition granules is made up of following steps:
A, take Chinese crude drug according to crude drug part by weight, clean, cataclasm;
B, Herba Eupatorii, Rhizoma Atractylodis merge, and add 5-9 times of water gaging, and vapour method extracts volatile oil, extract 3-6 hour, and the another device of volatile oil is collected, and aqueous solution is for subsequent use after filtering;
C, Fructus Corni 5-9 times amount 50-90% ethanol make solvent, flood after 12-48 hour, carry out percolation, collect percolate, reclaim ethanol, and be condensed into 60 DEG C measure relative densities be the thick paste of 1.30-1.35, dry, for subsequent use;
D, Radix Ginseng, Radix Ophiopogonis, Herba Epimedii, the Rhizoma Anemarrhenae, Radix Puerariae, add 6-10 times amount 50-90% ethanol, reflux, extract, 1-3 time, each 1-3 hour, extracting liquid filtering, reclaims ethanol, be condensed into thick paste, dries, for subsequent use;
E, Rhizoma Polygonati, Radix Sophorae Flavescentis, Radix Rehmanniae, Radix Polygoni Multiflori Preparata, Poria, Rhizoma Coptidis, Radix Salviae Miltiorrhizae, Semen Litchi, Cortex Lycii, add 7-11 times of water gaging, decoct 1-2 time, each 1-3 hour, extracting liquid filtering, carries the aqueous solution after oil merge with Herba Eupatorii, Rhizoma Atractylodis in step b, be condensed into clear paste, adding ethanol regulates determining alcohol to be 50-80%, and cold preservation is placed, and filters, filtrate recycling ethanol, be concentrated into thick paste, dry, for subsequent use;
F, by the dry cream of step c gained Fructus Corni, steps d gained alcohol promote cream, the dry cream mix homogeneously of step e gained water extract-alcohol precipitation, pulverize, add adjuvant granulate;
G, step b gained volatile oil add dissolve with ethanol, spray into the granule of step f gained, and mixing, airtight, subpackage, to obtain final product.
The discrimination method of Radix Ginseng in described Chinese medicine composition, is made up of following steps:
A, get the preparation being equivalent to this Chinese medicine composition crude drug amount 22-34g, add 80% methanol 50ml, supersound process 20 minutes, filtrate is put in evaporating dish, water bath method, the residue 20ml that adds water makes dissolving, extract 2 times with chloroform jolting, each 20ml, discard chloroform layer, the jolting of water layer water-saturated n-butanol extracts 3 times, merge n-butyl alcohol liquid, wash 2 times with 1% sodium hydroxide solution, each 30ml, 2 times are washed again with n-butyl alcohol saturation water, water consumption is 30ml, divides and gets n-butanol layer, evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution;
B, separately get Radix Ginseng control medicinal material, be made in the same way of control medicinal material solution, then get ginsenoside Rg
1, Re, Rb
1reference substance, adds methanol and makes every 1ml respectively containing the mixed solution of 0.5mg, product solution in contrast;
C, test according to thin layer chromatography, draw need testing solution, control medicinal material solution and each 5 μ l of reference substance solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, take ratio as lower floor's solution that the chloroform-acetate-methanol-less than 10 DEG C, water-glacial acetic acid of 50:20:30:10:10 is placed be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, spot development is heated to clear at 105 DEG C, in test sample chromatograph, with on control medicinal material and reference substance chromatograph relevant position, the principal spot of aobvious same color respectively.
The discrimination method of Rhizoma Coptidis in described Chinese medicine composition, is made up of following steps:
A, get the preparation being equivalent to this Chinese medicine composition crude drug amount 11-17g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is as need testing solution;
B, separately get Rhizoma Coptidis control medicinal material, add methanol, supersound process 20 minutes, filter, filtrate is medical material solution in contrast;
C, according to thin layer chromatography test, draw need testing solution and each 5 μ l of control medicinal material solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, with the acetate-methanol-isopropyl alcohol of 8:1:1:1-dense ammonia for developing solvent, at developing tank opposite side enriching ammonia 1ml, after saturated 5 minutes, launch, take out, dry, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious more than 2 same colors.
The discrimination method of Radix Salviae Miltiorrhizae and Radix Puerariae in described Chinese medicine composition, is made up of following steps:
A, get the preparation being equivalent to this Chinese medicine composition crude drug amount 11-17g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is as need testing solution;
B, separately get Radix Salviae Miltiorrhizae control medicinal material, add methanol, supersound process 20 minutes, filter, filtrate is medical material solution in contrast, gets puerarin reference substance, adds methanol and make the solution of every 1ml containing 1mg, product solution in contrast;
C, the test of photograph thin layer chromatography, draw each 5 μ l of need testing solution, Radix Salviae Miltiorrhizae control medicinal material solution and puerarin reference substance solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, with 5:3:1 chloroform-acetone-formic acid for developing solvent, launch, take out, dry, put smoke to red rooted salvia spot development in saturated ammonia steam clear, take out, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to Radix Salviae Miltiorrhizae and puerarin reference substance chromatograph, the fluorescence principal spot of aobvious same color respectively.
The discrimination method of the Rhizoma Anemarrhenae in described Chinese medicine composition, is made up of following steps:
A, get the preparation being equivalent to this Chinese medicine composition crude drug amount 11-17g, add 50% acetone 10ml, supersound process 20 minutes, filter, get filtrate as need testing solution;
B, separately get Rhizoma Anemarrhenae control medicinal material, be made in the same way of control medicinal material solution;
C, according to thin layer chromatography test, draw need testing solution and each 3 μ l of control medicinal material solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel H lamellae on, with 6:2:2 n-butyl alcohol-glacial acetic acid-water for developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid,, inspect under putting 365nm ultra-violet lamp immediately, in test sample chromatograph after 5 minutes 105 DEG C of heating, on the position corresponding to control medicinal material chromatograph, the fluorescence principal spot of aobvious same color.
The discrimination method of Radix Polygoni Multiflori and Herba Epimedii in described Chinese medicine composition, is made up of following steps:
A, get the preparation being equivalent to this Chinese medicine composition crude drug amount 22-34g, add 80% methanol 50ml, supersound process 20 minutes, filter, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, 2 times are extracted, each 20ml, combined ethyl acetate liquid with ethyl acetate jolting, evaporate to dryness, residue is transferred on polyamide column, with methanol 3ml eluting after adding methanol 3ml dissolving, collect eluent, as need testing solution;
B, separately get Radix Polygoni Multiflori control medicinal material, add methanol, supersound process 20 minutes, filter, get filtrate and put on polyamide column, collect effluent as Radix Polygoni Multiflori control medicinal material solution, get icariin reference substance again, add methanol and make the solution of every 1ml containing 0.4mg, as icariin reference substance solution;
C, test according to thin layer chromatography, draw need testing solution 3 μ l, Radix Polygoni Multiflori control medicinal material solution and each 1 μ l of icariin reference substance solution, put respectively on same polyamide film, with 5:5:1:0.5:0.5 ethyl acetate-butanone-methyl alcohol-formic acid-water for developing solvent, launch, take out, dry, inspect under putting 365nm ultra-violet lamp immediately, in test sample chromatograph, on the position corresponding to Radix Polygoni Multiflori control medicinal material chromatograph, the fluorescence principal spot of aobvious same color, spray with 1% aluminum chloride alcoholic solution again, hot blast drying, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to icariin reference substance chromatograph, the fluorescence speckle of aobvious same color.
As optimal way, described Chinese medicine composition is made up of the crude drug of following parts by weight: Radix Ginseng 102, Rhizoma Polygonati 136, Rhizoma Atractylodis 68, Radix Sophorae Flavescentis 56, Poria 83, Radix Ophiopogonis 136, Radix Polygoni Multiflori 83, Radix Rehmanniae 102, Fructus Corni 136, Rhizoma Coptidis 56, Herba Eupatorii 56, Semen Litchi 136, Herba Epimedii 56, the Rhizoma Anemarrhenae 68, Radix Salviae Miltiorrhizae 89, Radix Puerariae 136, Cortex Lycii 83.
Or
Radix Ginseng 50, Rhizoma Polygonati 180g, Rhizoma Atractylodis 40g, Radix Sophorae Flavescentis 58, Poria 40, Radix Ophiopogonis 180, Radix Polygoni Multiflori 40, Radix Rehmanniae 110, Fructus Corni 60, Rhizoma Coptidis 58, Herba Eupatorii 35, Semen Litchi 140, Herba Epimedii 35, the Rhizoma Anemarrhenae 90, Radix Salviae Miltiorrhizae 40, Radix Puerariae 180, Cortex Lycii 40.
Or
Radix Ginseng 150, Rhizoma Polygonati 60, Rhizoma Atractylodis 90, Radix Sophorae Flavescentis 30, Poria 90, Radix Ophiopogonis 60, Radix Polygoni Multiflori 90, Radix Rehmanniae 60, Fructus Corni 180, Rhizoma Coptidis 30, Herba Eupatorii 58, Semen Litchi 80, Herba Epimedii 58, the Rhizoma Anemarrhenae 35, Radix Salviae Miltiorrhizae 110, Radix Puerariae 56, Cortex Lycii 90.
Described Rhizoma Atractylodis are parched with bran Rhizoma Atractylodis, and Radix Polygoni Multiflori is Radix Polygoni Multiflori Preparata, and Herba Epimedii is Herba Epimedii Preparata.
Radix Puerariae of the present invention comprises Radix Puerariae and Pachyrhizua angulatus, and the pharmacopeia of 2005 does not distinguish these two, and the pharmacopeia of 2010 is distinguished, and Radix Puerariae derives from legume pueraria lobata, and Pachyrhizua angulatus derives from leguminous plant Radix Puerariae rattan, and the present invention is preferably Pachyrhizua angulatus.
The scope that the scope of the ratio of each taste medicine of Chinese medicine composition of the present invention is through great many of experiments and preferably draws, if the selection of each taste medicine of pharmaceutical composition is outside this scope, so its effect can weaken greatly.
Owing to have employed technique scheme, the technological progress that the present invention obtains is:
Method of the present invention can accurately identify the composition of Radix Ginseng, Rhizoma Coptidis, Radix Salviae Miltiorrhizae, Radix Puerariae, the Rhizoma Anemarrhenae, Radix Polygoni Multiflori, Herba Epimedii in this Chinese medicine composition, and specificity is strong, contributes to the quality control of medicine, improves Drug safety and reliability.
Accompanying drawing explanation
Fig. 1 is the thin-layer chromatogram of Radix Ginseng, and from left to right, 1 is negative control, and 2 is Radix Ginseng control medicinal materials, and 3-5 is ginsenoside Rg respectively
1, Re, Rb
1contrast, 6 is samples;
Fig. 2 is the thin-layer chromatogram of Rhizoma Coptidis, and from left to right, 1 is negative control, and 2 is Rhizoma Coptidis control medicinal materials, and 3-5 is sample;
Fig. 3 is the thin-layer chromatogram of Radix Salviae Miltiorrhizae and Radix Puerariae, from left to right, 1 Radix Salviae Miltiorrhizae negative control, 2 Radix Salviae Miltiorrhizae control medicinal materials, 3-5 is sample, 6 puerarin contrasts, and 7 Radix Puerariaes are negative;
Fig. 4 is the thin-layer chromatogram of the Rhizoma Anemarrhenae, and from left to right, 1 is negative control, and 2 is Rhizoma Anemarrhenae control medicinal materials, and 3-5 is sample;
Fig. 5 is the thin-layer chromatogram of Radix Polygoni Multiflori and Herba Epimedii, and left figure is before aluminum chloride colour developing, and right figure is after aluminum chloride colour developing, in two figure from left to right, and 1 Radix Polygoni Multiflori negative control, 2 Radix Polygoni Multiflori contrasts, 3-5 sample, 6 Herba Epimedii contrasts, 7 Herba Epimedii negative controls.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further details:
Embodiment 1
The proportioning of this Chinese medicine composition is as follows:
Radix Ginseng 102 g, Rhizoma Polygonati 136 g, parched with bran Rhizoma Atractylodis 68 g, Radix Sophorae Flavescentis 56 g, Poria 83 g, Radix Ophiopogonis 136 g, Radix Polygoni Multiflori Preparata 83 g, Radix Rehmanniae 102 g, Fructus Corni 136 g, Rhizoma Coptidis 56 g, Herba Eupatorii 56 g, Semen Litchi 136 g, Herba Epimedii Preparata 56 g, the Rhizoma Anemarrhenae 68 g, Radix Salviae Miltiorrhizae 89 g, Radix Puerariae 136 g, Cortex Lycii 83 g.
The preparation process of this Chinese medicinal composition granules is:
A, take Chinese crude drug according to recipe quantity, clean, cataclasm;
B, Herba Eupatorii, Rhizoma Atractylodis add 6 times of water gagings, extract volatile oil, and carrying the oil time is 5 hours, and the another device of volatile oil is collected, and aqueous solution is for subsequent use after filtering, and residue discards;
C, Fructus Corni after 24 hours, carry out percolation by 7 times amount 75% alcohol dipping, collect percolate, reclaim ethanol, and be condensed into 60 DEG C measure relative densities be the thick paste of 1.30,70 DEG C of oven dry, for subsequent use;
D, Radix Ginseng, Radix Ophiopogonis, Herba Epimedii, the Rhizoma Anemarrhenae, Radix Puerariae, add 8 times amount 70% ethanol, reflux, extract, 3 times, each 2 hours.Extracting liquid filtering, reclaims ethanol, and being concentrated into 60 DEG C of mensuration relative densities is the thick paste of 1.30, and 65 DEG C of oven dry are for subsequent use;
E, Rhizoma Polygonati, Radix Sophorae Flavescentis, Radix Rehmanniae, Radix Polygoni Multiflori, Poria, Rhizoma Coptidis, Radix Salviae Miltiorrhizae, Semen Litchi, Cortex Lycii, add 9 times of water gagings, decocts 2 times, each 2 hours, extracting liquid filtering, carried the aqueous solution after oil with Herba Eupatorii, Rhizoma Atractylodis and merges, measuring relative density when being concentrated into 60 DEG C is the clear paste of 1.15, adding 95% ethanol conciliation determining alcohol is 60%, and cold preservation places 24 hours, filters, filtrate recycling ethanol, and to measure relative density when being concentrated into 60 DEG C be the thick paste of 1.30,70 DEG C of oven dry, for subsequent use;
F, by the dry cream of step c gained Fructus Corni, steps d gained alcohol promote cream, the dry cream mix homogeneously of step e gained water extract-alcohol precipitation, pulverize;
G, step f gained dried cream powder to be mixed homogeneously by 4:5:1 with lactose powder, dextrin, be adhesive with 60% ethanol, soft material processed, 14 eye mesh screen granules, 60 DEG C of oven dry, 12-60 eye mesh screen granulate, sift out part fine powder, spray into step b gained volatile oil, mixing, airtight half an hour, obtain 556 grams of granules.
The discrimination method of Radix Ginseng in this Chinese medicine composition, is made up of following steps:
A, get said composition granule, porphyrize, take 10g, add 80% methanol 50ml, supersound process 20 minutes, filtrate is put in evaporating dish, water bath method, the residue 20ml that adds water makes dissolving, 2 times are extracted with chloroform jolting, each 20ml, discard chloroform layer, 3 (20ml are extracted in the jolting of water layer water-saturated n-butanol, 20ml, 15ml), merge n-butyl alcohol liquid, 2 times are washed with 1% sodium hydroxide solution, each 30ml, 2 times are washed again with n-butyl alcohol saturation water, water consumption is 30ml, divide and get n-butanol layer, evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution,
B, separately get Radix Ginseng control medicinal material 1g, be made in the same way of control medicinal material solution, then get ginsenoside Rg
1, Re, Rb
1reference substance, adds methanol and makes every 1ml respectively containing the mixed solution of 0.5mg, product solution in contrast;
C, test according to thin layer chromatography, draw need testing solution, control medicinal material solution and each 5 μ l of reference substance solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, take ratio as lower floor's solution that the chloroform-acetate-methanol-less than 10 DEG C, water-glacial acetic acid of 50:20:30:10:10 is placed be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, spot development is heated to clear at 105 DEG C, in test sample chromatograph, with on control medicinal material and reference substance chromatograph relevant position, the principal spot of aobvious same color respectively.See Fig. 1.
Embodiment 2:
Crude drug formula is and preparation method is with embodiment 1.
The discrimination method of Rhizoma Coptidis in described Chinese medicine composition, is made up of following steps:
A, get said composition granule, porphyrize, take 5g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is as need testing solution;
B, separately get Rhizoma Coptidis control medicinal material 0.03g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is medical material solution in contrast;
C, according to thin layer chromatography test, draw need testing solution and each 5 μ l of control medicinal material solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, with the acetate-methanol-isopropyl alcohol of 8:1:1:1-dense ammonia for developing solvent, at developing tank opposite side enriching ammonia 1ml, after saturated 5 minutes, launch, take out, dry, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious more than 2 same colors.See Fig. 2.
Embodiment 3
Crude drug formula is and preparation method is with embodiment 1.
The discrimination method of Radix Salviae Miltiorrhizae and Radix Puerariae in described Chinese medicine composition, is made up of following steps:
A, get said composition granule, porphyrize, take 5g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is as need testing solution;
B, separately get Radix Salviae Miltiorrhizae control medicinal material 0.5g, add methanol 5ml, supersound process 20 minutes, filter, filtrate is medical material solution in contrast, gets puerarin reference substance, adds methanol and make the solution of every 1ml containing 1mg, product solution in contrast;
C, the test of photograph thin layer chromatography, draw each 5 μ l of need testing solution, Radix Salviae Miltiorrhizae control medicinal material solution and puerarin reference substance solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, with 5:3:1 chloroform-acetone-formic acid for developing solvent, launch, take out, dry, put smoke to red rooted salvia spot development in saturated ammonia steam clear, take out, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to Radix Salviae Miltiorrhizae and puerarin reference substance chromatograph, the fluorescence principal spot of aobvious same color respectively.See Fig. 3.
Embodiment 4
Crude drug formula is and preparation method is with embodiment 1.
The discrimination method of the Rhizoma Anemarrhenae in described Chinese medicine composition, is made up of following steps:
A, get said composition granule, porphyrize, take 5g, add 50% acetone 10ml, supersound process 20 minutes, filter, get filtrate as need testing solution;
B, separately get Rhizoma Anemarrhenae control medicinal material 0.2g, be made in the same way of control medicinal material solution;
C, according to thin layer chromatography test, draw need testing solution and each 3 μ l of control medicinal material solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel H lamellae on, with 6:2:2 n-butyl alcohol-glacial acetic acid-water for developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid,, inspect under putting 365nm ultra-violet lamp immediately, in test sample chromatograph after 5 minutes 105 DEG C of heating, on the position corresponding to control medicinal material chromatograph, the fluorescence principal spot of aobvious same color.See Fig. 4
Embodiment 5
Crude drug formula is and preparation method is with embodiment 1.
The discrimination method of Radix Polygoni Multiflori and Herba Epimedii in described Chinese medicine composition, is made up of following steps:
A, get said composition granule, porphyrize, take 10g, add 80% methanol 50ml, supersound process 20 minutes, filter, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, extracts 2 times with ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue is transferred on polyamide column, with methanol 3ml eluting after adding methanol 3ml dissolving, collect eluent, as need testing solution;
B, separately get Radix Polygoni Multiflori control medicinal material 0.5g, add methanol 8ml, supersound process 20 minutes, filter, getting filtrate puts on polyamide column, collects effluent as Radix Polygoni Multiflori control medicinal material solution, then gets icariin reference substance, add methanol and make the solution of every 1ml containing 0.4mg, as icariin reference substance solution;
C, test according to thin layer chromatography, draw need testing solution 3 μ l, Radix Polygoni Multiflori control medicinal material solution and each 1 μ l of icariin reference substance solution, put respectively on same polyamide film, with 5:5:1:0.5:0.5 ethyl acetate-butanone-methyl alcohol-formic acid-water for developing solvent, launch, take out, dry, inspect under putting 365nm ultra-violet lamp immediately, in test sample chromatograph, on the position corresponding to Radix Polygoni Multiflori control medicinal material chromatograph, the fluorescence principal spot of aobvious same color, spray with 1% aluminum chloride alcoholic solution again, hot blast drying, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to icariin reference substance chromatograph, the fluorescence speckle of aobvious same color.See Fig. 5.
Embodiment 6
Crude drug formula is:
Radix Ginseng 50 g, Rhizoma Polygonati 180 g, Rhizoma Atractylodis 40 g, Radix Sophorae Flavescentis 58 g, Poria 40 g, Radix Ophiopogonis 180 g, Radix Polygoni Multiflori 40 g, Radix Rehmanniae 110 g, Fructus Corni 60 g, Rhizoma Coptidis 58 g, Herba Eupatorii 35 g, Semen Litchi 140 g, Herba Epimedii 35 g, the Rhizoma Anemarrhenae 90 g, Radix Salviae Miltiorrhizae 40 g, Radix Puerariae 180 g, Cortex Lycii 40 g.
Preparation method is:
A, take Chinese crude drug by recipe quantity, clean, cataclasm;
B, Herba Eupatorii, Rhizoma Atractylodis add 5 times of water gagings, extract volatile oil, and carrying the oil time is 3 hours, and the another device of volatile oil is collected, and aqueous solution is for subsequent use after filtering, and residue discards;
C, Fructus Corni after 12 hours, carry out percolation by 5 times amount 50% alcohol dipping, collect percolate, reclaim ethanol, and be condensed into 60 DEG C measure relative densities be the thick paste of 1.30,65 DEG C of oven dry, for subsequent use;
D, Radix Ginseng, Radix Ophiopogonis, Herba Epimedii, the Rhizoma Anemarrhenae, Radix Puerariae, add 6 times amount 5% ethanol, reflux, extract, 2 times, each 1 hour.Extracting liquid filtering, reclaims ethanol, and being concentrated into 60 DEG C of mensuration relative densities is the thick paste of 1.30, and 65 DEG C of oven dry are for subsequent use;
E, Rhizoma Polygonati, Radix Sophorae Flavescentis, Radix Rehmanniae, Radix Polygoni Multiflori, Poria, Rhizoma Coptidis, Radix Salviae Miltiorrhizae, Semen Litchi, Cortex Lycii, add 7 times of water gagings, decocts 1 hour, extracting liquid filtering, carry the aqueous solution after oil with Herba Eupatorii, Rhizoma Atractylodis to merge, measuring relative density when being concentrated into 60 DEG C is the clear paste of 1.10, and adding 95% ethanol conciliation determining alcohol is 50%, cold preservation places 24 hours, filter, filtrate recycling ethanol, and to measure relative density when being concentrated into 60 DEG C be the thick paste of 1.30,65 DEG C of oven dry, for subsequent use;
F, by the dry cream of step c gained Fructus Corni, steps d gained alcohol promote cream, the dry cream mix homogeneously of step e gained water extract-alcohol precipitation, pulverize, make granule;
G, step b gained volatile oil is added dissolve with ethanol, spray into step f gained granule, formulation method is made tablet and be get final product routinely.
The discrimination method of Radix Ginseng in this Chinese medicine composition, is made up of following steps:
A, get said composition tablet, porphyrize, take 12g, add 80% methanol 50ml, supersound process 20 minutes, filtrate is put in evaporating dish, water bath method, the residue 20ml that adds water makes dissolving, 2 times are extracted with chloroform jolting, each 20ml, discard chloroform layer, 3 (20ml are extracted in the jolting of water layer water-saturated n-butanol, 20ml, 15ml), merge n-butyl alcohol liquid, 2 times are washed with 1% sodium hydroxide solution, each 30ml, 2 times are washed again with n-butyl alcohol saturation water, water consumption is 30ml, divide and get n-butanol layer, evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution,
B, separately get Radix Ginseng control medicinal material 1g, be made in the same way of control medicinal material solution, then get ginsenoside Rg
1, Re, Rb
1reference substance, adds methanol and makes every 1ml respectively containing the mixed solution of 0.5mg, product solution in contrast;
C, test according to thin layer chromatography, draw need testing solution, control medicinal material solution and each 5 μ l of reference substance solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, take ratio as lower floor's solution that the chloroform-acetate-methanol-less than 10 DEG C, water-glacial acetic acid of 50:20:30:10:10 is placed be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, spot development is heated to clear at 105 DEG C, in test sample chromatograph, with on control medicinal material and reference substance chromatograph relevant position, the principal spot of aobvious same color respectively.
Embodiment 7:
Crude drug formula is and preparation method is with embodiment 6.
The discrimination method of Rhizoma Coptidis in described Chinese medicine composition, is made up of following steps:
A, get said composition tablet, porphyrize, take 6g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is as need testing solution;
B, separately get Rhizoma Coptidis control medicinal material 0.03g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is medical material solution in contrast;
C, according to thin layer chromatography test, draw need testing solution and each 5 μ l of control medicinal material solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, with the acetate-methanol-isopropyl alcohol of 8:1:1:1-dense ammonia for developing solvent, at developing tank opposite side enriching ammonia 1ml, after saturated 5 minutes, launch, take out, dry, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious more than 2 same colors.
Embodiment 8
Crude drug formula is and preparation method is with embodiment 6.
The discrimination method of Radix Salviae Miltiorrhizae and Radix Puerariae in described Chinese medicine composition, is made up of following steps:
A, get said composition tablet, porphyrize, take 6g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is as need testing solution;
B, separately get Radix Salviae Miltiorrhizae control medicinal material 0.5g, add methanol 5ml, supersound process 20 minutes, filter, filtrate is medical material solution in contrast, gets puerarin reference substance, adds methanol and make the solution of every 1ml containing 1mg, product solution in contrast;
C, the test of photograph thin layer chromatography, draw each 5 μ l of need testing solution, Radix Salviae Miltiorrhizae control medicinal material solution and puerarin reference substance solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, with 5:3:1 chloroform-acetone-formic acid for developing solvent, launch, take out, dry, put smoke to red rooted salvia spot development in saturated ammonia steam clear, take out, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to Radix Salviae Miltiorrhizae and puerarin reference substance chromatograph, the fluorescence principal spot of aobvious same color respectively.
Embodiment 9
Crude drug formula is and preparation method is with embodiment 6.
The discrimination method of the Rhizoma Anemarrhenae in described Chinese medicine composition, is made up of following steps:
A, get said composition tablet, porphyrize, take 6g, add 50% acetone 10ml, supersound process 20 minutes, filter, get filtrate as need testing solution;
B, separately get Rhizoma Anemarrhenae control medicinal material 0.2g, be made in the same way of control medicinal material solution;
C, according to thin layer chromatography test, draw need testing solution and each 3 μ l of control medicinal material solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel H lamellae on, with 6:2:2 n-butyl alcohol-glacial acetic acid-water for developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid,, inspect under putting 365nm ultra-violet lamp immediately, in test sample chromatograph after 5 minutes 105 DEG C of heating, on the position corresponding to control medicinal material chromatograph, the fluorescence principal spot of aobvious same color.
Embodiment 10
Crude drug formula is and preparation method is with embodiment 6.
The discrimination method of Radix Polygoni Multiflori and Herba Epimedii in described Chinese medicine composition, is made up of following steps:
A, get said composition tablet, porphyrize, take 12g, add 80% methanol 50ml, supersound process 20 minutes, filter, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, extracts 2 times with ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue is transferred on polyamide column, with methanol 3ml eluting after adding methanol 3ml dissolving, collect eluent, as need testing solution;
B, separately get Radix Polygoni Multiflori control medicinal material 0.5g, add methanol 8ml, supersound process 20 minutes, filter, getting filtrate puts on polyamide column, collects effluent as Radix Polygoni Multiflori control medicinal material solution, then gets icariin reference substance, add methanol and make the solution of every 1ml containing 0.4mg, as icariin reference substance solution;
C, test according to thin layer chromatography, draw need testing solution 3 μ l, Radix Polygoni Multiflori control medicinal material solution and each 1 μ l of icariin reference substance solution, put respectively on same polyamide film, with 5:5:1:0.5:0.5 ethyl acetate-butanone-methyl alcohol-formic acid-water for developing solvent, launch, take out, dry, inspect under putting 365nm ultra-violet lamp immediately, in test sample chromatograph, on the position corresponding to Radix Polygoni Multiflori control medicinal material chromatograph, the fluorescence principal spot of aobvious same color, spray with 1% aluminum chloride alcoholic solution again, hot blast drying, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to icariin reference substance chromatograph, the fluorescence speckle of aobvious same color.
Embodiment 11:
Crude drug formula is:
Radix Ginseng 150 g, Rhizoma Polygonati 60 g, Rhizoma Atractylodis 90 g, Radix Sophorae Flavescentis 30 g, Poria 90 g, Radix Ophiopogonis 60 g, Radix Polygoni Multiflori 90 g, Radix Rehmanniae 60 g, Fructus Corni 180 g, Rhizoma Coptidis 30 g, Herba Eupatorii 58 g, Semen Litchi 80 g, Herba Epimedii 58 g, the Rhizoma Anemarrhenae 35 g, Radix Salviae Miltiorrhizae 110 g, Radix Puerariae 56 g, Cortex Lycii 90 g.
Preparation method is:
A, take Chinese crude drug by recipe quantity, clean, cataclasm;
B, Herba Eupatorii, Rhizoma Atractylodis add 9 times of water gagings, extract volatile oil, and carrying the oil time is 6 hours, and the another device of volatile oil is collected, and aqueous solution is for subsequent use after filtering, and residue discards;
C, Fructus Corni after 48 hours, carry out percolation by 9 times amount 90% alcohol dipping, collect percolate, reclaim ethanol, and be condensed into 60 DEG C measure relative densities be the thick paste of 1.35,70 DEG C of oven dry, for subsequent use;
D, Radix Ginseng, Radix Ophiopogonis, Herba Epimedii, the Rhizoma Anemarrhenae, Radix Puerariae, add 10 times amount 90% ethanol, reflux, extract, 3 times, each 3 hours.Extracting liquid filtering, reclaims ethanol, and being concentrated into 60 DEG C of mensuration relative densities is the thick paste of 1.35, and 70 DEG C of oven dry are for subsequent use;
E, Rhizoma Polygonati, Radix Sophorae Flavescentis, Radix Rehmanniae, Radix Polygoni Multiflori, Poria, Rhizoma Coptidis, Radix Salviae Miltiorrhizae, Semen Litchi, Cortex Lycii, add 11 times of water gagings, decocts 2 times, each 3 hours, extracting liquid filtering, carried the aqueous solution after oil with Herba Eupatorii, Rhizoma Atractylodis and merges, measuring relative density when being concentrated into 60 DEG C is the clear paste of 1.15, and adding 95% ethanol conciliation determining alcohol is 80%, and cold preservation places 24 hours, filter, filtrate recycling ethanol, and to measure relative density when being concentrated into 60 DEG C be the thick paste of 1.35,70 DEG C of oven dry, pulverize, for subsequent use;
F, step b gained volatile oil is added dissolve with ethanol, spray in step e gained dried cream powder, formulation method is made capsule and be get final product routinely.
The discrimination method of Radix Ginseng in this Chinese medicine composition, is made up of following steps:
A, get said composition capsule, porphyrize, take 8g, add 80% methanol 50ml, supersound process 20 minutes, filtrate is put in evaporating dish, water bath method, the residue 20ml that adds water makes dissolving, 2 times are extracted with chloroform jolting, each 20ml, discard chloroform layer, 3 (20ml are extracted in the jolting of water layer water-saturated n-butanol, 20ml, 15ml), merge n-butyl alcohol liquid, 2 times are washed with 1% sodium hydroxide solution, each 30ml, 2 times are washed again with n-butyl alcohol saturation water, water consumption is 30ml, divide and get n-butanol layer, evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution,
B, separately get Radix Ginseng control medicinal material 1g, be made in the same way of control medicinal material solution, then get ginsenoside Rg
1, Re, Rb
1reference substance, adds methanol and makes every 1ml respectively containing the mixed solution of 0.5mg, product solution in contrast;
C, test according to thin layer chromatography, draw need testing solution, control medicinal material solution and each 5 μ l of reference substance solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, take ratio as lower floor's solution that the chloroform-acetate-methanol-less than 10 DEG C, water-glacial acetic acid of 50:20:30:10:10 is placed be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, spot development is heated to clear at 105 DEG C, in test sample chromatograph, with on control medicinal material and reference substance chromatograph relevant position, the principal spot of aobvious same color respectively.
Embodiment 12:
Crude drug formula is and preparation method is with embodiment 11.
The discrimination method of Rhizoma Coptidis in described Chinese medicine composition, is made up of following steps:
A, get said composition capsule, porphyrize, take 4g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is as need testing solution;
B, separately get Rhizoma Coptidis control medicinal material 0.03g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is medical material solution in contrast;
C, according to thin layer chromatography test, draw need testing solution and each 5 μ l of control medicinal material solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, with the acetate-methanol-isopropyl alcohol of 8:1:1:1-dense ammonia for developing solvent, at developing tank opposite side enriching ammonia 1ml, after saturated 5 minutes, launch, take out, dry, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious more than 2 same colors.
Embodiment 13
Crude drug formula is and preparation method is with embodiment 11.
The discrimination method of Radix Salviae Miltiorrhizae and Radix Puerariae in described Chinese medicine composition, is made up of following steps:
A, get said composition capsule, porphyrize, take 4g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is as need testing solution;
B, separately get Radix Salviae Miltiorrhizae control medicinal material 0.5g, add methanol 5ml, supersound process 20 minutes, filter, filtrate is medical material solution in contrast, gets puerarin reference substance, adds methanol and make the solution of every 1ml containing 1mg, product solution in contrast;
C, the test of photograph thin layer chromatography, draw each 5 μ l of need testing solution, Radix Salviae Miltiorrhizae control medicinal material solution and puerarin reference substance solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, with 5:3:1 chloroform-acetone-formic acid for developing solvent, launch, take out, dry, put smoke to red rooted salvia spot development in saturated ammonia steam clear, take out, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to Radix Salviae Miltiorrhizae and puerarin reference substance chromatograph, the fluorescence principal spot of aobvious same color respectively.
Embodiment 14
Crude drug formula is and preparation method is with embodiment 11.
The discrimination method of the Rhizoma Anemarrhenae in described Chinese medicine composition, is made up of following steps:
A, get said composition capsule, porphyrize, take 4g, add 50% acetone 10ml, supersound process 20 minutes, filter, get filtrate as need testing solution;
B, separately get Rhizoma Anemarrhenae control medicinal material 0.2g, be made in the same way of control medicinal material solution;
C, according to thin layer chromatography test, draw need testing solution and each 3 μ l of control medicinal material solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel H lamellae on, with 6:2:2 n-butyl alcohol-glacial acetic acid-water for developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid,, inspect under putting 365nm ultra-violet lamp immediately, in test sample chromatograph after 5 minutes 105 DEG C of heating, on the position corresponding to control medicinal material chromatograph, the fluorescence principal spot of aobvious same color.
Embodiment 15
Crude drug formula is and preparation method is with embodiment 11.
The discrimination method of Radix Polygoni Multiflori and Herba Epimedii in described Chinese medicine composition, is made up of following steps:
A, get said composition capsule, porphyrize, take 8g, add 80% methanol 50ml, supersound process 20 minutes, filter, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, extracts 2 times with ethyl acetate jolting, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue is transferred on polyamide column, with methanol 3ml eluting after adding methanol 3ml dissolving, collect eluent, as need testing solution;
B, separately get Radix Polygoni Multiflori control medicinal material 0.5g, add methanol 8ml, supersound process 20 minutes, filter, getting filtrate puts on polyamide column, collects effluent as Radix Polygoni Multiflori control medicinal material solution, then gets icariin reference substance, add methanol and make the solution of every 1ml containing 0.4mg, as icariin reference substance solution;
C, test according to thin layer chromatography, draw need testing solution 3 μ l, Radix Polygoni Multiflori control medicinal material solution and each 1 μ l of icariin reference substance solution, put respectively on same polyamide film, with 5:5:1:0.5:0.5 ethyl acetate-butanone-methyl alcohol-formic acid-water for developing solvent, launch, take out, dry, inspect under putting 365nm ultra-violet lamp immediately, in test sample chromatograph, on the position corresponding to Radix Polygoni Multiflori control medicinal material chromatograph, the fluorescence principal spot of aobvious same color, spray with 1% aluminum chloride alcoholic solution again, hot blast drying, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to icariin reference substance chromatograph, the fluorescence speckle of aobvious same color.
Claims (10)
1. a Chinese medicine composition, is characterized in that this Chinese medicine composition is made up of the crude drug of following parts by weight: Radix Ginseng 50-150, Rhizoma Polygonati 60-180, Rhizoma Atractylodis 40-90, Radix Sophorae Flavescentis 30-58, Radix Ophiopogonis 60-180, Radix Rehmanniae 60-110, Radix Polygoni Multiflori 40-90, Fructus Corni 60-180, Poria 40-90, Herba Eupatorii 35-58, Rhizoma Coptidis 35-58, Rhizoma Anemarrhenae 35-90, Herba Epimedii 35-58, Radix Salviae Miltiorrhizae 40-110, Radix Puerariae 60-180, Semen Litchi 80-140, Cortex Lycii 40-90.
2. Chinese medicine composition according to claim 1, is characterized in that the active fraction preparation of this Chinese medicine composition is made up of following steps:
A, take Chinese crude drug according to crude drug part by weight, clean, cataclasm;
B, Herba Eupatorii, Rhizoma Atractylodis add 5-9 times amount water extraction volatile oil, extract 3-6 hour, and the another device of volatile oil is collected, and aqueous solution is for subsequent use after filtering;
C, Fructus Corni 5-9 times amount 50-90% ethanol make solvent, flood after 12-48 hour, carry out percolation, collect percolate, reclaim ethanol, and be condensed into 60 DEG C measure relative densities be the thick paste of 1.30-1.35, dry, for subsequent use;
D, Radix Ginseng, Radix Ophiopogonis, Herba Epimedii, the Rhizoma Anemarrhenae, Radix Puerariae, add 6-10 times amount 50-90% ethanol, reflux, extract, 1-3 time, each 1-3 hour, extracting liquid filtering, reclaims ethanol, be condensed into thick paste, dries, for subsequent use;
E, Rhizoma Polygonati, Radix Sophorae Flavescentis, Radix Rehmanniae, Radix Polygoni Multiflori, Poria, Rhizoma Coptidis, Radix Salviae Miltiorrhizae, Semen Litchi, Cortex Lycii, add 7-11 times of water gaging, decoct 1-2 time, each 1-3 hour, extracting liquid filtering, carries the aqueous solution after oil merge with Herba Eupatorii, Rhizoma Atractylodis in step b, be condensed into clear paste, adding ethanol regulates determining alcohol to be 50-80%, and cold preservation is placed, and filters, filtrate recycling ethanol, be concentrated into thick paste, dry, for subsequent use;
The active component that cream, the dry cream of step e gained water extract-alcohol precipitation and step b gained volatile oil form this Chinese medicine composition jointly promoted by the dry cream of step c gained Fructus Corni, steps d gained alcohol.
3. Chinese medicine composition according to claim 1, is characterized in that the preparation formulation of this Chinese medicine composition is capsule, tablet or granule.
4. Chinese medicine composition according to claim 3, is characterized in that the preparation of this Chinese medicinal composition granules is made up of following steps:
A, take Chinese crude drug according to crude drug part by weight, clean, cataclasm;
B, Herba Eupatorii, Rhizoma Atractylodis merge, and add 5-9 times of water gaging, and vapour method extracts volatile oil, extract 3-6 hour, and the another device of volatile oil is collected, and aqueous solution is for subsequent use after filtering;
C, Fructus Corni 5-9 times amount 50-90% ethanol make solvent, flood after 12-48 hour, carry out percolation, collect percolate, reclaim ethanol, and be condensed into 60 DEG C measure relative densities be the thick paste of 1.30-1.35, dry, for subsequent use;
D, Radix Ginseng, Radix Ophiopogonis, Herba Epimedii, the Rhizoma Anemarrhenae, Radix Puerariae, add 6-10 times amount 50-90% ethanol, reflux, extract, 1-3 time, each 1-3 hour, extracting liquid filtering, reclaims ethanol, be condensed into thick paste, dries, for subsequent use;
E, Rhizoma Polygonati, Radix Sophorae Flavescentis, Radix Rehmanniae, Radix Polygoni Multiflori Preparata, Poria, Rhizoma Coptidis, Radix Salviae Miltiorrhizae, Semen Litchi, Cortex Lycii, add 7-11 times of water gaging, decoct 1-2 time, each 1-3 hour, extracting liquid filtering, carries the aqueous solution after oil merge with Herba Eupatorii, Rhizoma Atractylodis in step b, be condensed into clear paste, adding ethanol regulates determining alcohol to be 50-80%, and cold preservation is placed, and filters, filtrate recycling ethanol, be concentrated into thick paste, dry, for subsequent use;
F, by the dry cream of step c gained Fructus Corni, steps d gained alcohol promote cream, the dry cream mix homogeneously of step e gained water extract-alcohol precipitation, pulverize, add adjuvant granulate;
G, step b gained volatile oil add dissolve with ethanol, spray into the granule of step f gained, and mixing, airtight, subpackage, to obtain final product.
5. the discrimination method of Radix Ginseng in the Chinese medicine composition according to claim 3 or 4, is characterized in that the method is made up of following steps:
A, get the preparation being equivalent to this Chinese medicine composition crude drug amount 22-34g, add 80% methanol 50ml, supersound process 20 minutes, filtrate is put in evaporating dish, water bath method, the residue 20ml that adds water makes dissolving, extract 2 times with chloroform jolting, each 20ml, discard chloroform layer, the jolting of water layer water-saturated n-butanol extracts 3 times, merge n-butyl alcohol liquid, wash 2 times with 1% sodium hydroxide solution, each 30ml, 2 times are washed again with n-butyl alcohol saturation water, water consumption is 30ml, divides and gets n-butanol layer, evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution;
B, separately get Radix Ginseng control medicinal material, be made in the same way of control medicinal material solution, then get ginsenoside Rg
1, Re, Rb
1reference substance, adds methanol and makes every 1ml respectively containing the mixed solution of 0.5mg, product solution in contrast;
C, test according to thin layer chromatography, draw need testing solution, control medicinal material solution and each 5 μ l of reference substance solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, take ratio as lower floor's solution that the chloroform-acetate-methanol-less than 10 DEG C, water-glacial acetic acid of 50:20:30:10:10 is placed be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, spot development is heated to clear at 105 DEG C, in test sample chromatograph, with on control medicinal material and reference substance chromatograph relevant position, the principal spot of aobvious same color respectively.
6. the discrimination method of Rhizoma Coptidis in the Chinese medicine composition according to claim 3 or 4, is characterized in that the method is made up of following steps:
A, get the preparation being equivalent to this Chinese medicine composition crude drug amount 11-17g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is as need testing solution;
B, separately get Rhizoma Coptidis control medicinal material, add methanol, supersound process 20 minutes, filter, filtrate is medical material solution in contrast;
C, according to thin layer chromatography test, draw need testing solution and each 5 μ l of control medicinal material solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, with the acetate-methanol-isopropyl alcohol of 8:1:1:1-dense ammonia for developing solvent, at developing tank opposite side enriching ammonia 1ml, after saturated 5 minutes, launch, take out, dry, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to control medicinal material chromatograph, the fluorescence speckle of aobvious more than 2 same colors.
7. the discrimination method of Radix Salviae Miltiorrhizae and Radix Puerariae in the Chinese medicine composition according to claim 3 or 4, is characterized in that the method is made up of following steps:
A, get the preparation being equivalent to this Chinese medicine composition crude drug amount 11-17g, add methanol 10ml, supersound process 20 minutes, filter, filtrate is as need testing solution;
B, separately get Radix Salviae Miltiorrhizae control medicinal material, add methanol, supersound process 20 minutes, filter, filtrate is medical material solution in contrast, gets puerarin reference substance, adds methanol and make the solution of every 1ml containing 1mg, product solution in contrast;
C, the test of photograph thin layer chromatography, draw each 5 μ l of need testing solution, Radix Salviae Miltiorrhizae control medicinal material solution and puerarin reference substance solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel g thin-layer plate on, with 5:3:1 chloroform-acetone-formic acid for developing solvent, launch, take out, dry, put smoke to red rooted salvia spot development in saturated ammonia steam clear, take out, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to Radix Salviae Miltiorrhizae and puerarin reference substance chromatograph, the fluorescence principal spot of aobvious same color respectively.
8. the discrimination method of the Rhizoma Anemarrhenae in the Chinese medicine composition according to claim 3 or 4, is characterized in that the method is made up of following steps:
A, get the preparation being equivalent to this Chinese medicine composition crude drug amount 11-17g, add 50% acetone 10ml, supersound process 20 minutes, filter, get filtrate as need testing solution;
B, separately get Rhizoma Anemarrhenae control medicinal material, be made in the same way of control medicinal material solution;
C, according to thin layer chromatography test, draw need testing solution and each 3 μ l of control medicinal material solution, put respectively in same with sodium carboxymethyl cellulose be binding agent silica gel H lamellae on, with 6:2:2 n-butyl alcohol-glacial acetic acid-water for developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid,, inspect under putting 365nm ultra-violet lamp immediately, in test sample chromatograph after 5 minutes 105 DEG C of heating, on the position corresponding to control medicinal material chromatograph, the fluorescence principal spot of aobvious same color.
9. the discrimination method of Radix Polygoni Multiflori and Herba Epimedii in the Chinese medicine composition according to claim 3 or 4, is characterized in that the method is made up of following steps:
A, get the preparation being equivalent to this Chinese medicine composition crude drug amount 22-34g, add 80% methanol 50ml, supersound process 20 minutes, filter, filtrate evaporate to dryness, the residue 20ml that adds water makes dissolving, 2 times are extracted, each 20ml, combined ethyl acetate liquid with ethyl acetate jolting, evaporate to dryness, residue is transferred on polyamide column, with methanol 3ml eluting after adding methanol 3ml dissolving, collect eluent, as need testing solution;
B, separately get Radix Polygoni Multiflori control medicinal material, add methanol, supersound process 20 minutes, filter, get filtrate and put on polyamide column, collect effluent as Radix Polygoni Multiflori control medicinal material solution, get icariin reference substance again, add methanol and make the solution of every 1ml containing 0.4mg, as icariin reference substance solution;
C, test according to thin layer chromatography, draw need testing solution 3 μ l, Radix Polygoni Multiflori control medicinal material solution and each 1 μ l of icariin reference substance solution, put respectively on same polyamide film, with 5:5:1:0.5:0.5 ethyl acetate-butanone-methyl alcohol-formic acid-water for developing solvent, launch, take out, dry, inspect under putting 365nm ultra-violet lamp immediately, in test sample chromatograph, on the position corresponding to Radix Polygoni Multiflori control medicinal material chromatograph, the fluorescence principal spot of aobvious same color, spray with 1% aluminum chloride alcoholic solution again, hot blast drying, inspect under putting 365nm ultra-violet lamp, in test sample chromatograph, on the position corresponding to icariin reference substance chromatograph, the fluorescence speckle of aobvious same color.
10. assay method according to claim 1, it is characterized in that described Rhizoma Atractylodis are parched with bran Rhizoma Atractylodis, Radix Polygoni Multiflori is Radix Polygoni Multiflori Preparata, and Herba Epimedii is Herba Epimedii Preparata.
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| CN105738554A (en) * | 2016-02-05 | 2016-07-06 | 四川德成动物保健品有限公司 | Thin-layer chromatography detection method for rhizoma anemarrhenae for antipyretic and antitoxic powder |
| CN110031588A (en) * | 2019-03-26 | 2019-07-19 | 浙江金大康动物保健品有限公司 | An a kind of quick thin-layer identification method of plate multiple medicine taste of livestock and poultry antiviral granule |
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| CN101584807A (en) * | 2008-05-22 | 2009-11-25 | 河北以岭医药研究院有限公司 | Application of traditional Chinese medicine composition in preparing medicament of insulin sensitizer |
| CN101612312A (en) * | 2008-06-25 | 2009-12-30 | 河北以岭医药研究院有限公司 | The application of a kind of Chinese medicine composition in the diabetes complicated disease drug of preparation treatment |
| CN101780215A (en) * | 2009-01-19 | 2010-07-21 | 河北以岭医药研究院有限公司 | Refining method of traditional Chinese medicine composition water extract containing ginseng |
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| CN105738554A (en) * | 2016-02-05 | 2016-07-06 | 四川德成动物保健品有限公司 | Thin-layer chromatography detection method for rhizoma anemarrhenae for antipyretic and antitoxic powder |
| CN110031588A (en) * | 2019-03-26 | 2019-07-19 | 浙江金大康动物保健品有限公司 | An a kind of quick thin-layer identification method of plate multiple medicine taste of livestock and poultry antiviral granule |
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