CN1325072C - Method for preparing traditional Chinese medicine - Google Patents
Method for preparing traditional Chinese medicine Download PDFInfo
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- CN1325072C CN1325072C CNB2005100388592A CN200510038859A CN1325072C CN 1325072 C CN1325072 C CN 1325072C CN B2005100388592 A CNB2005100388592 A CN B2005100388592A CN 200510038859 A CN200510038859 A CN 200510038859A CN 1325072 C CN1325072 C CN 1325072C
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Abstract
The present invention discloses a method for preparing Yixinshu particles and a quality control technology. Raw material traditional Chinese medicines are prepared from ginseng, astragalus root, red sage root, ophiopogon root, schisandra fruit, chuanxiong rhizome and haw. The present invention is characterized in that the ginseng is taken to be crushed into fine powder; the schisandra fruit and the red sage root are extracted by ethanol reflux to be concentrated into a paste after extracting solution is concentrated; water is added into the ophiopogon root, the chuanxiong rhizome, the haw, the astragalus root, etc. to be decocted and extracted, and ethanol solution is added after extracting solution is filtered and concentrated, the extracting solution and the ethanol solution are filtered off precipitates after the extracting solution and the ethanol solution are fully stirred and stood, ethanol is recovered from filter liquid, and the filter liquid is concentrated into a paste; after the two pastes are combined, the ginseng fine powder and a proper quantity of dextrin and stevioside are added to be uniformly mixed, granulated, dried and prepared into granular formulation. The quality control technology is to qualitatively identify and quantitatively measure the total amount of ginsenoside Rg1(C42H72O14) and ginsenoside Re(C48H82O18), and is reliable.
Description
Technical field
The invention belongs to a kind of Chinese medicine, specifically is the novel form of Chinese medicine YIXINSHU JIAONANG---particulate preparation method of YIXINSHU and Quality Control Technology.
Background technology
" YIXINSHU JIAONANG " is that office of National Drug Administration issues the 13 in standard Chinese traditional patent formulation preparation (the 13 in former Ministry of Public Health ministry standard Chinese traditional patent formulation preparation) and records kind, but capsule exists absorption slow, preparation technology is unreasonable, the not high shortcoming of effective ingredient.
Summary of the invention
The objective of the invention is existing YIXINSHU JIAONANG is carried out dosage changing form, propose particulate preparation method of a kind of YIXINSHU and Quality Control Technology, better YIXINSHU Chinese medicine is served broad masses of the people's needs of medical treatment.
Technical scheme of the present invention is as follows:
The particulate preparation method of YIXINSHU, raw material Chinese medicine is made up of Radix Ginseng, the Radix Astragali, Radix Salviae Miltiorrhizae, Radix Ophiopogonis, Fructus Schisandrae Chinensis, Rhizoma Chuanxiong, Fructus Crataegi, it is characterized in that getting the Radix Ginseng powder and is broken into fine powder; Fructus Schisandrae Chinensis, Radix Salviae Miltiorrhizae alcohol reflux, concentrate behind the extracting liquid filtering clear paste; Radix Ophiopogonis, Rhizoma Chuanxiong, Fructus Crataegi, the Radix Astragali etc. decoct with water extraction, extracting liquid filtering, add alcoholic solution after concentrating, after fully stirring, leave standstill, the elimination precipitate, filtrate recycling ethanol and concentrate clear paste, after will above-mentioned two kinds of clear paste merging, adding Radix Ginseng fine powder and an amount of dextrin, stevioside, mix homogeneously, granulate, drying is made granule promptly.
The particulate preparation method of described YIXINSHU is characterized in that
(1), the weight ratio of each raw material components is:
200 Radix Ophiopogonis 150 of Radix Ginseng 150 Radixs Astragali 150 Radix Salviae Miltiorrhizaes
Fructus Schisandrae Chinensis 100 Rhizoma Chuanxiongs 100 Fructus Crataegis 150
(2), preparation process:
Fructus Schisandrae Chinensis, Radix Salviae Miltiorrhizae are with 75～85% alcohol reflux 1～2 time, extracting solution filters, merging filtrate, concentrating under reduced pressure get pure clear paste, and Radix Ophiopogonis, Rhizoma Chuanxiong, Fructus Crataegi, the Radix Astragali etc. decoct with water 1～2 time, collecting decoction, filter, after filtrate concentrates, add 75～85% ethanol, after fully stirring, left standstill 8～24 hours, the elimination precipitate, filtrate recycling ethanol also concentrates to such an extent that water is carried clear paste, after above-mentioned two kinds of clear paste merging, add Radix Ginseng fine powder and an amount of dextrin, stevioside, mix homogeneously is granulated, drying is made granule promptly.
The particulate preparation method of described YIXINSHU is characterized in that preparation process is:
Fructus Schisandrae Chinensis, Radix Salviae Miltiorrhizae was with 85% alcohol reflux 2 times, 3 hours for the first time, 1.5 hours for the second time, filter, merging filtrate is evaporated to relative density 1.15～1.20 (20 ℃), get pure clear paste, decoct with water 2 all the other Radix Ophiopogonis etc., 2.5 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, filtrate is concentrated into 500ml, adds equivalent 85% ethanol, after fully stirring, left standstill 8～24 hours, the elimination precipitate, filtrate recycling ethanol also is concentrated into relative density 1.30～1.36 (80 ℃), gets water and carries clear paste, after above-mentioned two kinds of clear paste merging, add Radix Ginseng fine powder and an amount of dextrin, stevioside, mix homogeneously is granulated, drying is made granule promptly.
The particulate Quality Control Technology of YIXINSHU is characterized in that
(1), qualitative identification
A, to get this product Chinese medicine content an amount of, adds the ethyl acetate reflux, extract,, filters, and filter paper, filtering residue are retained; Filtrate merges, and puts evaporate to dryness in the water-bath, and residue adds methanol makes dissolving in right amount, as need testing solution; Other gets the schisandrin B reference substance, adds methanol and makes the schisandrin B reference substance solution; Draw need testing solution 10 μ l, reference substance solution 5 μ l, put in same silica gel G F respectively
254On the lamellae, the toluene-ethyl acetate that is with volume ratio is developing solvent, launches, and takes out, and dries, and puts under the ultra-violet lamp (254nm) and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
B, to get the Radix Salviae Miltiorrhizae control medicinal material an amount of, adds the ethyl acetate reflux, extract,, filters, and filtrate is put evaporate to dryness in the water-bath, and residue adds methanol makes dissolving in right amount, in contrast medical material solution; Draw differentiating need testing solution under a item, each 5 μ l of Radix Salviae Miltiorrhizae control medicinal material solution, respectively on the same silica gel g thin-layer plate of idea, is that benzene-ethyl acetate of 19: 1 is developing solvent with volume ratio, launches, and takes out, and dries; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
C, get and differentiate a item filter paper, filtering residue down, add alcohol reflux, filter, filtrate merges, and puts evaporate to dryness in the water-bath, and residue adds an amount of heating of water makes dissolving, filtration, and filtrate is passed through D
101(φ 1.8cm * 40cm 50ml), washes with water earlier to closely colourless macroporous adsorptive resins, discards water lotion; Continuing, it is closely colourless to be washed till with 30～50% ethanol, discards ethanol elution; Reuse 50～80% ethanol are washed till closely colourless, collect ethanol elution, put and are concentrated into 10～25ml in the water-bath, add water-saturated n-butanol and extract, leave standstill, divide and get n-butyl alcohol liquid, merge, add the saturated ammonia solution washing of n-butyl alcohol 1～4 time, each 5～20ml leaves standstill, divide and get n-butyl alcohol liquid, put evaporate to dryness in the water-bath, residue adds methanol makes dissolving in right amount, as need testing solution; Other gets Radix Ginseng control medicinal material 1g, shines medical material solution in pairs with legal system; Draw need testing solution, each 10ul of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with volume ratio is 15: 40: 22: chloroform-ethyl acetate of 10-methanol-water (lower floor's solution of placing below 10 ℃) is developing solvent, launch, take out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at high temperature; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
D, to get this product Chinese medicine content an amount of, adds water and put in the water-bath in right amount and heat, and stirs and make abundant dissolving, centrifugal, get supernatant, put and be concentrated into 5～20ml in the water-bath, add an amount of heated and boiled of hydrochloric acid 3～10 minutes, put coldly, move in the separatory funnel, add an amount of jolting of chloroform and extract 1～3 time, leave standstill, divide and get chloroform layer, merge, put evaporate to dryness in the water-bath, residue adds ethyl acetate makes dissolving in right amount, as need testing solution; Other gets control medicinal material 1g Radix Ophiopogonis, decocts with water, and filters, and filtrate is concentrated into 5～20ml, makes control medicinal material solution; Drawing need testing solution, each 10 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, is that chloroform-acetone of 6: 1 is developing solvent with volume ratio, launches, and takes out, and dries, and spray is with ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing in high temperature; In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the principal spot of same color;
E, to get this product Chinese medicine content an amount of, and an amount of reflux, extract, of hydro-oxidation potassium methanol solution filters, filtrate is put evaporate to dryness in the water-bath, and residue adds water makes dissolving in right amount, and the chloroform-n-butyl alcohol mixed solution that adds volume ratio and be 2: 1 extracts, leave standstill, divide and get extracting solution, merge, add the saturated ammonia solution washing of n-butyl alcohol again, leave standstill, divide and get chloroform-n-butyl alcohol liquid, put evaporate to dryness in the water-bath, residue adds an amount of heating of water makes dissolving, puts coldly, passes through D
101Macroporous adsorptive resins (φ 1.8cm * 40cm, 40ml), an amount of eluting of first water discards water lotion; Continue with an amount of eluting of 30～50% ethanol, discard ethanol elution; With an amount of eluting of 50～80% ethanol, collect ethanol elution again, put evaporate to dryness in the water-bath, residue adds methanol makes dissolving in right amount, as need testing solution; Other gets the astragaloside reference substance, add methanol and make the astragaloside reference substance solution: draw need testing solution 10 μ l, reference substance solution 5 μ l, putting respectively on same silica gel g thin-layer plate, is that lower floor's solution of chloroform-methanol-water of 13: 7: 2 is developing solvent with volume ratio, launches, take out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at high temperature; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
F, to get this product Chinese medicine content an amount of, adds volume ratio and be ethyl acetate-an amount of reflux, extract, of formic acid mixed solution of 9.5: 0.5, filters, filtrate is put evaporate to dryness in the water-bath, and residue hydro-oxidation sodium solution makes dissolving in right amount, and extraction adds diethyl ether, leave standstill, divide and get ether layer, discard; The alkali liquor layer adds concentrated hydrochloric acid and transfers PH1～2, and the extraction that adds diethyl ether is left standstill, and divides and gets ether layer, merges, and puts in the water-bath to volatilize, and residue adds methanol makes dissolving in right amount, as need testing solution; Other gets Rhizoma Chuanxiong control medicinal material 1g, adds water and decocts in right amount, filters, and filtrate hydro-oxidation sodium solution is transferred pH＞9, and remainder is made control medicinal material solution from " add diethyl ether and extract 3 times " with the need testing solution preparation method; Draw need testing solution, each 10 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with volume ratio is that benzene-methanol-glacial acetic acid of 30: 3: 1 is developing solvent, launch, take out, dry, it is clear that spray with the volume ratio of new preparation is that 1: 1 ferric chloride and potassium ferricyanide mixed solution to speckle develops the color; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
(2), quantitative assay
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-0.05% phosphoric acid solution (99: 400) is a mobile phase; The detection wavelength is 203nm; Number of theoretical plate calculates by the ginsenoside Re peak should be not less than 2500; The preparation of reference substance solution: precision takes by weighing the ginsenoside Rg
1Reference substance, ginsenoside Re's reference substance are an amount of, add methanol and make every 1ml respectively and contain the ginsenoside Rg
10.125mg, the solution of ginsenoside Re 0.1mg, promptly; The preparation of need testing solution: get this product Chinese medicine content 2.0g, the accurate title, decide, and puts in the apparatus,Soxhlet's, it is closely colourless to extracting solution to add an amount of reflux, extract, of chloroform, discards chloroform solution, and medicinal residues are flung to chloroform, move in the tool plug conical flask together with filtration paper cylinder, it is an amount of to add water saturated n-butyl alcohol, close plug, placement is spent the night, and supersound extraction filters, filter paper, filtering residue adds an amount of supersound extraction of water saturated n-butyl alcohol, filters, and filtrate merges, put in the water-bath and concentrate, put coldly, be transferred in the separatory funnel, add the saturated ammonia solution washing of n-butyl alcohol 1～5 time, each 5～25ml, add an amount of washing of the saturated water of n-butyl alcohol 1～3 time again, get n-butyl alcohol liquid, put evaporate to dryness in the water-bath, residue adds an amount of gradation of methanol makes dissolving, and quantitatively move in the 5ml measuring bottle, solubilizer is diluted to scale again, close plug, shake up, promptly; Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get the every 4g of this product Chinese medicine and contain Radix Ginseng with the ginsenoside Rg
1(C
42H
72O
14) and ginsenoside Re (C
48H
82O
18) total amount must not be less than 1.2mg.
This product contains Radix Ginseng with the ginsenoside Rg for every bag
1(C
42H
72O
14) and ginsenoside Re (C
48H
82O
18) total amount must not be less than 1.2mg.
Function with cure mainly: Yiqi and vein recovery, blood circulation promoting and blood stasis dispelling, 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.
Usage and consumption: oral, one time 1 bag, 3 times on the one.
Specification: every packed 4g.
Storage: sealing.
YIXINSHU granule of the present invention has preparation technology's science, and the active constituent content height absorbs fast, characteristics such as produce effects is rapid, taking convenience, raising curative effect.
The specific embodiment
1, prescription
Radix Ginseng 150g Radix Astragali 150g Radix Salviae Miltiorrhizae 200g 150g Radix Ophiopogonis
Fructus Schisandrae Chinensis 100g Rhizoma Chuanxiong 100g Fructus Crataegi 150g
More than make the 1000g granule
2, method for making
More than seven flavors, get behind the Radix Ginseng crushing fine powder standby.Fructus Schisandrae Chinensis, Radix Salviae Miltiorrhizae was with 85% alcohol reflux 2 times, 3 hours for the first time, 1.5 hours for the second time, filter, merging filtrate is evaporated to relative density 1.15～1.20 (20 ℃), get pure clear paste, decoct with water 2 all the other Radix Ophiopogonis etc., 2.5 hours for the first time, 1.5 hours for the second time, collecting decoction filtered, filtrate is concentrated into 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 ℃), get water and carry clear paste, after above-mentioned two kinds of clear paste merging, add Radix Ginseng fine powder and an amount of dextrin, stevioside, mix homogeneously, granulate, drying is made 1000g, promptly.
3, differentiate
Character, this product are granule, and content is that yellowish-brown is to brown granule; Feeble QI perfume (or spice), sweet, little hardship of distinguishing the flavor of.
Qualitative identification
(1), get this product 10g, porphyrize adds the ethyl acetate reflux, extract, 2 times, each 50ml, 1 hour filters, filter paper, filtering residue are retained.Filtrate merges, and puts evaporate to dryness in the water-bath, and residue adds methanol 2ml makes dissolving, as need testing solution.Other gets the schisandrin B reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, draw need testing solution 10 ul, reference substance solution 5 μ l, put in same silica gel G F respectively
254On the lamellae, be developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect with toluene-ethyl acetate (9: 1).In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(2), get Radix Salviae Miltiorrhizae control medicinal material 1g, add ethyl acetate 20m1 reflux, extract, 1 hour, filter, filtrate is put evaporate to dryness in the water-bath, residue adds methanol 1ml makes dissolving, in contrast medical material solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, draw and differentiate (1) item need testing solution, each 5 μ l of Radix Salviae Miltiorrhizae control medicinal material solution down, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate (19: 1) is developing solvent, launch, take out, dry.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color.
(3), get discriminating (1) filter paper, filtering residue down, add alcohol reflux 2 times, each 50ml, 1 hour filters, filtrate merges, and puts evaporate to dryness in the water-bath, residue adds water 10ml heating makes dissolving, filtration, filtrate is passed through D
101(φ 1.8cm * 40cm 50ml), washes with water earlier to closely colourless macroporous adsorptive resins, discards water lotion; Continuing, it is closely colourless to be washed till with 40% ethanol, discards 40% ethanol elution; Reuse 70% ethanol is washed till closely colourless, collects 70% ethanol elution, puts and is concentrated into 20ml in the water-bath, add water-saturated n-butanol and extract 3 times, each 20ml leaves standstill, divide and get n-butyl alcohol liquid, merge, add the saturated ammonia solution washing of n-butyl alcohol 3 times, each 15ml, leave standstill, divide and get n-butyl alcohol liquid, put evaporate to dryness in the water-bath, residue adds methanol 2ml makes dissolving, as need testing solution.Other gets Radix Ginseng control medicinal material 1g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (15: 40: 22: 10) lower floor's solution of placing below 10 ℃ was developing solvent with chloroform-ethyl acetate-methanol-water, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color.
(4), get this product 10g, porphyrize adds water 50ml and puts in the water-bath heating 10 minutes, stirring makes abundant dissolving, and is centrifugal, gets supernatant, put and be concentrated into 10ml in the water-bath, add hydrochloric acid 0.5ml heated and boiled 5 minutes, put cold, move in the separatory funnel, add chloroform 20ml jolting and extract 2 times, leave standstill, divide and get chloroform layer, merge, put evaporate to dryness in the water-bath, residue adds ethyl acetate 1ml makes dissolving, as need testing solution.Other gets control medicinal material 1g Radix Ophiopogonis, adds water 20ml and decocts 2 hours, filters, and filtrate is concentrated into 10ml, and remainder is made control medicinal material solution from " adding hydrochloric acid 0.5ml " with the need testing solution preparation method.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-acetone (6: 1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing in 100 ℃.In the test sample chromatograph, with control medicinal material chromatograph relevant position on, show the principal spot of same color.
(5), get this product 10g, add 2% potassium hydroxide methanol solution 50ml reflux, extract, 1 hour, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds water 30ml makes dissolving, adds chloroform-n-butyl alcohol (2: 1) mixed solution and extracts 2 times, each 20ml leaves standstill, and divides and gets chloroform-n-butyl alcohol (2: 1) extracting solution, merge, add the saturated ammonia solution washing of n-butyl alcohol 3 times again, each 15ml, leave standstill, divide and get chloroform-n-butyl alcohol liquid, put evaporate to dryness in the water-bath, residue adds an amount of heating of water makes dissolving, puts coldly, passes through D
101Macroporous adsorptive resins (φ 1.8cm * 40cm, 40ml), first water 50ml eluting discards water lotion; Continue with 40% ethanol 50ml eluting, discard 40% ethanol elution; With 70% ethanol 100ml eluting, collect 70% ethanol elution again, put evaporate to dryness in the water-bath, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 10 μ l, reference substance solution 5 μ l, putting respectively on same silica gel g thin-layer plate, is developing solvent with lower floor's solution of chloroform-methanol-water (13: 7: 2), 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 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(6), get this product 10g, add the mixed solution 50ml reflux, extract, 1 hour of ethyl acetate-formic acid (9.5: 0.5), filter, filtrate is put evaporate to dryness in the water-bath, the sodium hydroxide solution 20ml that residue adds 0.1mol/L makes dissolving, adds diethyl ether to extract 3 times, each 15ml, leave standstill, divide and get ether layer, discard.The alkali liquor layer adds concentrated hydrochloric acid and transfers PH1～2, adds diethyl ether and extracts 3 times, and each 15ml leaves standstill, and divides and gets ether layer, merges, and puts in the water-bath to volatilize, and residue adds methanol 2ml makes dissolving, as need testing solution.Other gets Rhizoma Chuanxiong control medicinal material 1g, adds water 20ml and decocts 2 hours, filters, and filtrate adds the 10mol/L sodium hydroxide solution and transfers pH＞9, and remainder is made control medicinal material solution from " add diethyl ether and extract 3 times " with the need testing solution preparation method.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-methanol-glacial acetic acid (30: 3: 1) is developing solvent, launch, take out, dry, spray is clear to the speckle colour developing with 1% ferric chloride and 1% potassium ferricyanide (1: the 1) mixed solution of new preparation.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color.
Check, should meet every regulation relevant under the granule item (an appendix I of Chinese Pharmacopoeia version in 2000 C).
Assay
Measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-0.05% phosphoric acid solution (99: 400) is a mobile phase; The detection wavelength is 203nm.Number of theoretical plate calculates by 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, ginsenoside Re's reference substance are an amount of, add methanol and make every 1ml respectively and contain the ginsenoside Rg
10.125mg, the solution of ginsenoside Re 0.1mg, promptly.
This product content under the content uniformity is got in the preparation of need testing solution, and porphyrize is got about 2.0g, the accurate title, decide, and puts in the apparatus,Soxhlet's, and it is closely colourless to extracting solution to add an amount of reflux, extract, of chloroform, discard chloroform solution, medicinal residues are flung to chloroform, move in the tool plug conical flask together with filtration paper cylinder, add water saturated n-butyl alcohol 50ml, close plug, placement is spent the night, supersound extraction 30 minutes filters filter paper, filtering residue adds water saturated n-butyl alcohol 30ml supersound extraction 2 times, each 30 minutes, filter, filtrate merges, put and be concentrated into 60ml in the water-bath, put coldly, be transferred in the separatory funnel, add the saturated ammonia solution washing of n-butyl alcohol 3 times, each 20ml adds the saturated water 20ml washing of n-butyl alcohol 1 time again, get n-butyl alcohol liquid, put evaporate to dryness in the water-bath, residue adds methanol 5ml gradation makes dissolving, and quantitatively moves in the 5ml measuring bottle, solubilizer is diluted to scale again, close plug shakes up, promptly.
Accurate respectively reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Claims (1)
1, the particulate method of quality control of YIXINSHU is characterized in that:
One, make this product medicine by following technology:
(1), the weight ratio of each raw material components is:
200 Radix Ophiopogonis 150 of Radix Ginseng 150 Radixs Astragali 150 Radix Salviae Miltiorrhizaes
Fructus Schisandrae Chinensis 100 Rhizoma Chuanxiongs 100 Fructus Crataegis 150
(2), preparation process:
Fructus Schisandrae Chinensis, Radix Salviae Miltiorrhizae are with 75～85% alcohol reflux 1～2 time, extracting solution filters, merging filtrate, concentrating under reduced pressure get pure clear paste, and Radix Ophiopogonis, Rhizoma Chuanxiong, Fructus Crataegi, the Radix Astragali etc. decoct with water 1～2 time, collecting decoction, filter, after filtrate concentrates, add 75～85% ethanol, after fully stirring, left standstill 8～24 hours, the elimination precipitate, filtrate recycling ethanol also concentrates to such an extent that water is carried clear paste, after above-mentioned two kinds of clear paste merging, add Radix Ginseng fine powder and an amount of dextrin, stevioside, mix homogeneously is granulated, drying is made granule promptly;
Two, this product medicine that makes is differentiated:
(1), qualitative identification
A, to get this product Chinese medicine content an amount of, adds the ethyl acetate reflux, extract,, filters, and filter paper, filtering residue are retained.Filtrate merges, and puts evaporate to dryness in the water-bath, and residue adds methanol makes dissolving in right amount, as need testing solution; Other gets the schisandrin B reference substance, adds methanol and makes the schisandrin B reference substance solution; Draw need testing solution 10 μ l, reference substance solution 5 μ l, put in same silica gel G F respectively
254On the lamellae, the toluene-ethyl acetate that is with volume ratio is developing solvent, launches, and takes out, and dries, and puts under the 254nm ultra-violet lamp and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
B, to get the Radix Salviae Miltiorrhizae control medicinal material an amount of, adds the ethyl acetate cocurrent flow and extract, and filters, and filtrate is put evaporate to dryness in the water-bath, and residue adds methanol makes dissolving in right amount, in contrast medical material solution; Draw differentiating need testing solution under a item, each 5 μ l of Radix Salviae Miltiorrhizae control medicinal material solution, put respectively on same silica gel g thin-layer plate, is that benzene-ethyl acetate of 19: 1 is developing solvent with volume ratio, launches, and takes out, and dries.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
C, get and differentiate a item filter paper, filtering residue down, add alcohol reflux, filter, filtrate merges, and puts evaporate to dryness in the water-bath, and residue adds an amount of heating of water makes dissolving, filters, and filtrate is passed through φ 1.8cm * 40cm, the D of 50ml
101Macroporous adsorptive resins washes with water earlier to closely colourless, discards water lotion; Continuing, it is closely colourless to be washed till with 30～50% ethanol, discards ethanol elution; Reuse 50～80% ethanol are washed till closely colourless, collect ethanol elution, put and are concentrated into 10～25ml in the water-bath, add water-saturated n-butanol and extract, leave standstill, divide and get n-butyl alcohol liquid, merge, add the saturated ammonia solution washing of n-butyl alcohol 1～4 time, each 5～20ml leaves standstill, divide and get n-butyl alcohol liquid, put evaporate to dryness in the water-bath, residue adds methanol makes dissolving in right amount, as need testing solution; Other gets the about material 1g of Radix Ginseng contrast, shines medical material solution in pairs with legal system; Draw need testing solution, each 10 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with volume ratio is 15: 40: 22: chloroform-ethyl acetate of 10-methanol-water is developing solvent at lower floor's solution of placing below 10 ℃, launch, take out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at high temperature.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
D, to get this product Chinese medicine content an amount of, adds water and put in the water-bath in right amount and heat, and stirs and make abundant dissolving, centrifugal, get supernatant, put and be concentrated into 5～20ml in the water-bath, add an amount of heated and boiled of hydrochloric acid 3～10 minutes, put coldly, move in the separatory funnel, add an amount of jolting of chloroform and extract 1～3 time, leave standstill, divide and get chloroform layer, merge, put evaporate to dryness in the water-bath, residue adds ethyl acetate makes dissolving in right amount, as need testing solution; Other gets Radix Ophiopogonis contrast and receives material 1g, decocts with water, and filters, and filtrate is concentrated into 5～20ml, makes control medicinal material solution; Drawing need testing solution, each 10 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, is that chloroform-acetone of 6: 1 is developing solvent with volume ratio, launches, and takes out, and dries, and spray is with ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing in high temperature; In the test sample chromatograph,, show the principal spot of same color composing on the relevant position with the about wood color of contrast;
E, to get this product Chinese medicine content an amount of, and an amount of cocurrent flow of hydro-oxidation potassium methanol solution extracts, and filters, filtrate is put evaporate to dryness in the water-bath, and residue adds water makes dissolving in right amount, and the chloroform-n-butyl alcohol mixed solution that adds volume ratio and be 2: 1 extracts, leave standstill, divide and get extracting solution, merge, add the saturated ammonia solution washing of n-butyl alcohol again, leave standstill, divide and get chloroform-n-butyl alcohol liquid, put evaporate to dryness in the water-bath, residue adds an amount of heating of water makes dissolving, puts cold, by φ 1.8cm * 40cm, the D of 40ml
101Macroporous adsorptive resins, an amount of eluting of first water discards water lotion; Continue with an amount of eluting of 30～50% ethanol, discard ethanol elution; With an amount of eluting of 50～80% ethanol, collect ethanol elution again, put evaporate to dryness in the water-bath, residue adds methanol makes dissolving in right amount, as need testing solution; Other gets the astragaloside reference substance, add methanol and make the astragaloside reference substance solution: draw need testing solution 10 μ l, reference substance solution 5 μ l, distinguishing on the same silica gel g thin-layer plate of idea, is that lower floor's solution of chloroform-methanol-water of 13: 7: 2 is developing solvent with volume ratio, launches, take out, dry, spray is with ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at high temperature.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
F, to get this product Chinese medicine content an amount of, and an amount of cocurrent flow of ethyl acetate-formic acid mixed solution that adds volume ratio and be 9.5: 0.5 extracts, and filters, filtrate is put evaporate to dryness in the water-bath, and residue hydro-oxidation sodium solution makes dissolving in right amount, and extraction adds diethyl ether, leave standstill, divide and get ether layer, discard; The alkali liquor layer adds concentrated hydrochloric acid and transfers PH1～2, and the extraction that adds diethyl ether is left standstill, and divides and gets ether layer, merges, and puts in the water-bath to volatilize, and residue adds methanol makes dissolving in right amount, as need testing solution; Other gets Rhizoma Chuanxiong control medicinal material 1g, adds water and decocts in right amount, filters, and filtrate hydro-oxidation sodium solution is transferred pH＞9, and remainder is made control medicinal material solution from " add diethyl ether and extract 3 times " with the need testing solution preparation method; Draw need testing solution, each 10 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with volume ratio is that benzene-methanol-glacial acetic acid of 30: 3: 1 is developing solvent, launch, take out, dry, it is clear that spray with the volume ratio of new preparation is that 1: 1 ferric chloride and potassium ferricyanide mixed solution to speckle develops the color; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
(2), quantitative assay
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With 99: 400 acetonitriles-0.05% phosphoric acid solution is mobile phase; The detection wavelength is 203nm.Number of theoretical plate calculates by the ginsenoside Re peak should be not less than 2500; The preparation of reference substance solution: precision takes by weighing the ginsenoside Rg
1Reference substance, ginsenoside Re's reference substance are an amount of, add methanol and make every 1ml respectively and contain the ginsenoside Rg
10.125mg, the solution of ginsenoside Re 0.1mg, promptly; The preparation of need testing solution: get this product Chinese medicine content 2.0g, the accurate title, decide, and puts in the apparatus,Soxhlet's, adding an amount of cocurrent flow of chloroform, to be extracted into extracting solution closely colourless, discards chloroform solution, and medicinal residues are flung to chloroform, move in the tool plug conical flask together with filtration paper cylinder, it is an amount of to add water saturated n-butyl alcohol, close plug, placement is spent the night, and supersound extraction filters, filter paper, filtering residue adds an amount of supersound extraction of water saturated n-butyl alcohol, filters, and filtrate merges, put in the water-bath and concentrate, put coldly, be transferred in the separatory funnel, add the saturated ammonia solution washing of n-butyl alcohol 1～5 time, each 5～25ml, add an amount of washing of the saturated water of n-butyl alcohol 1～3 time again, get n-butyl alcohol liquid, put evaporate to dryness in the water-bath, residue adds an amount of gradation of methanol makes dissolving, and quantitatively move in the 5ml measuring bottle, solubilizer is diluted to scale again, close plug, shake up, promptly; Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get the every 4g of this product Chinese medicine and contain Radix Ginseng with the ginsenoside Rg
1-C
42H
72O
14And ginsenoside Re-C
48H
82O
18Total amount must not be less than 1.2mg.
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| CN1325072C true CN1325072C (en) | 2007-07-11 |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1814170B (en) * | 2005-12-15 | 2011-01-19 | 贵州信邦制药股份有限公司 | Medicinal drop pills for treating cardiovascular disease and preparing method |
| CN100464773C (en) * | 2006-03-01 | 2009-03-04 | 贵州信邦远东药业有限公司 | Yixinshu Injecta for retaliation of Qi and pulse and promotion of blood circulation and removing of blood stasis, and preparing method therefor |
| CN101036748B (en) * | 2007-04-18 | 2011-09-28 | 贵州信邦制药股份有限公司 | Detection method of the Yixinshu Chinese traditional medicine for supplementing qi and for promoting blood circulation by removing blood stasis |
| CN101804150A (en) * | 2010-03-22 | 2010-08-18 | 贵州信邦制药股份有限公司 | Traditional Chinese medicine composite used for treating left ventricular diastolic dysfunction |
| CN102552465B (en) * | 2010-12-29 | 2013-11-13 | 四川科伦药物研究有限公司 | Quality test method for hawthorn leaf medicine, hawthorn leaf extractives or products |
| CN104547506A (en) * | 2013-10-14 | 2015-04-29 | 山东中泰药业有限公司 | Traditional Chinese medicine preparation containing ginseng ultrafine powder and preparation method of traditional Chinese medicine preparation |
| CN103604898B (en) * | 2013-11-12 | 2015-09-09 | 贵州信邦制药股份有限公司 | The benefit heart relaxes the fingerprint atlas detection method of preparation |
| CN104330511B (en) * | 2014-10-22 | 2019-02-15 | 贵州信邦制药股份有限公司 | A kind of invigorating heart is relaxed the content assaying method of ginsenoside in preparation |
| CN105116067A (en) * | 2015-08-03 | 2015-12-02 | 黑龙江省食品药品检验检测所 | Identification method for ginseng and compound preparation containing raw powder thereof |
| CN109432293A (en) * | 2019-01-09 | 2019-03-08 | 山东中泰药业有限公司 | A kind of Chinese medicinal granule and preparation method thereof for treating cardiovascular and cerebrovascular disease |
| CN111388594A (en) * | 2020-04-21 | 2020-07-10 | 广东先通药业有限公司 | Extraction and quality identification method of effective components of Yixinshu tablet composition |
| CN112741809A (en) * | 2021-02-08 | 2021-05-04 | 海南海力制药有限公司 | Preparation method of Yixinshu granules |
| CN112891453A (en) * | 2021-04-09 | 2021-06-04 | 海南海力制药有限公司 | Preparation method of Yixinshu granules |
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2005
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