CN100515476C - Compound capsule with pseudo-ginseng and Chinese fanpalm seed, its preparation process and quality control method - Google Patents
Compound capsule with pseudo-ginseng and Chinese fanpalm seed, its preparation process and quality control method Download PDFInfo
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- CN100515476C CN100515476C CNB2006100404034A CN200610040403A CN100515476C CN 100515476 C CN100515476 C CN 100515476C CN B2006100404034 A CNB2006100404034 A CN B2006100404034A CN 200610040403 A CN200610040403 A CN 200610040403A CN 100515476 C CN100515476 C CN 100515476C
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Abstract
The invention relates to a compound capsule, process for preparation and quality control method, wherein the raw materials include malva seed, Bupleurum root, zedoary, root of red rooted saliva, gynostemma pentaphylla, astragalus root, ligustrum japonicum and spirulina. The preparing process consists of the steps of disintegrating raw materials, extracting by ethanol backflow, filtrating, concentrating the filtrate into grease, chopping raw materials, watering and boiling, filtrating, concentrating the filtrate into clear grease, charging ethanol, homogenizing, stewing till the second day, filtrating, concentrating the filtrate into clear grease, merging the clear grease, decompressing for reclaiming ethanol, drying into dried grease, disintegrating, sieving, mixing homogenously, palletizing, and packing capsules.
Description
Technical field
The present invention relates to a kind of new Chinese medicine, be specifically related to the Preparation method and its quality control technique of Chinese medicine compound capsule with pseudo-ginseng and Chinese fanpalm seed.
Background technology
" compound recipe gold Pu sheet " is that office of National Drug Administration issues standard country standard for traditional Chinese medicines compilation (Chinese patent medicine provincial standard rising national standard part) department of pediatrics department of stomatology oncology fascicle and records kind, the former disintegration of tablet time is long, bioavailability is relatively poor, the present invention carries out secondary development research with novel form, new preparation process, new quality standard to this kind, the selection dosage form is a capsule, capsule is easier to disintegrate, and attractive in appearance, swallow easily, and increased patient's selectivity and compliance.
Summary of the invention
The objective of the invention is Chinese medicine compound gold Pu sheet is carried out novel form and new technology research and new quality standard thereof, compound capsule with pseudo-ginseng and Chinese fanpalm seed and preparation method thereof and Quality Control Technology are provided.The compound capsule with pseudo-ginseng and Chinese fanpalm seed of the present invention's research has blood circulation promoting and blood stasis dispelling, the effect of promoting the circulation of QI to relieve pain.The auxiliary treatment that is used for the hepatocarcinoma of syndrome of qi stagnation and blood stasis.
Technical scheme of the present invention is as follows:
Compound capsule with pseudo-ginseng and Chinese fanpalm seed, crude drug is made up of Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Chinese fanpalm seed, Radix Bupleuri, Rhizoma Curcumae, Radix Salviae Miltiorrhizae, Herb Gynostemmae Pentaphylli, the Radix Astragali, Fructus Ligustri Lucidi, spirulina, it is characterized in that:
(1) the formulation weight ratio is:
Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 450 Chinese fanpalm seeds 450 Radix Bupleuri 350
Rhizoma Curcumae 350 Radix Salviae Miltiorrhizaes 100 strands 100
The Radix Astragali 100 Fructus Ligustri Lucidi 100 spirulinas 14
(2) adjuvant comprises:
Microcrystalline Cellulose, Pulvis Talci, starch, calcium hydrogen phosphate, carboxymethyl starch sodium, magnesium stearate etc.
The preparation method of described compound capsule with pseudo-ginseng and Chinese fanpalm seed is characterized in that:
Preparation method is 1.: above nine flavor medical materials, and Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Salviae Miltiorrhizae powder are broken into coarse powder or coarse grain, add alcohol reflux, merge alcohol extract, filter, and filtrate is condensed into clear paste; Radix Bupleuri, Rhizoma Curcumae, the Radix Astragali, Herb Gynostemmae Pentaphylli cutting, Chinese fanpalm seed, Fructus Ligustri Lucidi are smashed to pieces, merge with above-mentioned medicinal residues, decoct with water, collecting decoction filters, and filtrate is condensed into clear paste, adds ethanol and makes and contain the alcohol amount and reach 55～75%, stir evenly, standing over night filters, and filtrate is condensed into clear paste, merge with above-mentioned clear paste, decompression recycling ethanol is dried to dried cream, pulverizes, sieve, add spirulina, microcrystalline Cellulose, mixing, granulate, encapsulated, promptly;
Preparation method is 2.: above nine flavor medical materials, and Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Salviae Miltiorrhizae powder are broken into coarse powder or coarse grain; Radix Bupleuri, Rhizoma Curcumae, the Radix Astragali, Herb Gynostemmae Pentaphylli cutting; Chinese fanpalm seed, Fructus Ligustri Lucidi are smashed to pieces, and nine flavor medical materials add alcohol reflux, reflux 1～3 hour jointly, merge alcohol extract, filter, filtrate is condensed into clear paste, be dried to dried cream, pulverize, sieve, add spirulina, microcrystalline Cellulose, Pulvis Talci, mixing is granulated, and adds magnesium stearate, encapsulated, promptly;
Preparation method is 3.: above nine flavor medical materials, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Salviae Miltiorrhizae powder are broken into coarse powder, and Chinese fanpalm seed, Fructus Ligustri Lucidi are smashed to pieces, add alcohol reflux, and reflux 1～3 hour merges alcohol extract, filters, and filtrate is condensed into clear paste; Radix Bupleuri, Rhizoma Curcumae, immersion 1～3 hour, steam distillation extracts volatile oil, and volatile oil device is in addition stored, and decocting liquid is continued to employ; The Radix Astragali, Herb Gynostemmae Pentaphylli cutting merge with above-mentioned two parts of medicinal residues, decoct with water collecting decoction, filter, filtrate is condensed into clear paste, adds ethanol and makes and contain the alcohol amount and reach 60～75%, stirs evenly, standing over night filters, and filtrate is condensed into clear paste, merges with above-mentioned clear paste, be dried to dried cream, pulverize, sieve, add spirulina, starch, calcium hydrogen phosphate, carboxymethyl starch sodium, mixing is granulated, spray into volatile oil, encapsulated, promptly.
Described preparation method is characterized in that its concrete steps are respectively:
Preparation method 1. concrete steps is: above nine flavor medical materials, and Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Salviae Miltiorrhizae powder are broken into coarse powder, add 6 times of amount 70% alcoholic solution reflux, extract, three times, each time is 1 hour, merge alcohol extract, filter, filtrate is concentrated into the clear paste that relative density is 1.10～1.13 (60 ℃); Radix Bupleuri, Rhizoma Curcumae, the Radix Astragali, Herb Gynostemmae Pentaphylli cutting, Chinese fanpalm seed, Fructus Ligustri Lucidi are smashed to pieces, merge with above-mentioned medicinal residues, decoct with water three times, add 12 times of amounts of water at every turn, decocted 2 hours, collecting decoction filters, and filtrate is concentrated into the clear paste that relative density is 1.15 (60 ℃), add ethanol and make and contain the alcohol amount and reach 65%, stir evenly standing over night, filter, filtrate is concentrated into the clear paste that relative density is 1.13～1.15 (60 ℃), merges decompression recycling ethanol with above-mentioned clear paste, be dried to dried cream, pulverize, sieve, add spirulina, microcrystalline Cellulose, mixing, granulate, encapsulated, promptly;
Preparation method 2. concrete steps is: above nine flavor medical materials, and Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Salviae Miltiorrhizae powder are broken into coarse powder; Radix Bupleuri, Rhizoma Curcumae, the Radix Astragali, Herb Gynostemmae Pentaphylli cutting; Chinese fanpalm seed, Fructus Ligustri Lucidi are smashed to pieces, and this nine flavors medical material adds 70% alcoholic solution reflux, extract, three times jointly, each 8 times of amounts 1 hour, merge alcohol extract, filter, filtrate is concentrated into the clear paste that relative density is 1.13～1.15 (60 ℃), be dried to dried cream, pulverize, sieve, add spirulina, microcrystalline Cellulose, Pulvis Talci, mixing is granulated, and adds magnesium stearate, encapsulated, promptly;
Preparation method 3. concrete steps is: above nine flavor medical materials, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Salviae Miltiorrhizae powder are broken into coarse powder, Chinese fanpalm seed, Fructus Ligustri Lucidi are smashed to pieces, adding 6 times of amount 70% alcoholic solution refluxes, extract three times, each 1 hour, merge alcohol extract, filter, filtrate is concentrated into the clear paste that relative density is 1.10～1.13 (60 ℃); Radix Bupleuri, Rhizoma Curcumae, immersion 2 hours, steam distillation extracted volatile oil 6 hours, and volatile oil device is in addition stored, and decocting liquid is continued to employ; The Radix Astragali, Herb Gynostemmae Pentaphylli cutting merge with above-mentioned two minutes medicinal residues, decoct with water three times, add 12 times of amounts of water at every turn, decocted collecting decoction 2 hours, filter, filtrate is concentrated into the clear paste that relative density is 1.15 (60 ℃), adds ethanol and makes and contain the alcohol amount and reach 65%, stir evenly, standing over night filters, and filtrate is concentrated into the clear paste that relative density is 1.13～1.15 (60 ℃), merge with above-mentioned clear paste, be dried to dried cream, pulverize, sieve, add spirulina, starch, calcium hydrogen phosphate, carboxymethyl starch sodium, mixing is granulated, and sprays into volatile oil, encapsulated, promptly.
The method of quality control of compound capsule with pseudo-ginseng and Chinese fanpalm seed is characterized in that differentiating and measuring by following steps:
(1) qualitative identification
A, get compound capsule with pseudo-ginseng and Chinese fanpalm seed content 2g, porphyrize adds ethanol 10ml, and supersound process 30 minutes filters, and filtrate is as need testing solution; Other gets the rotundine hydrochloride reference substance, adds ethanol 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 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with normal hexane-chloroform-methanol (15: 5: 2), launches, take out, dry, put in the iodine vapor and smoked 30 seconds, take out, wave the iodine that adsorbs on the most plate, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
B, get compound capsule with pseudo-ginseng and Chinese fanpalm seed 8g, porphyrize adds methanol solution 50ml, supersound process 30 minutes filters, and filtrate is put evaporate to dryness in the water-bath, residue adds water 30ml makes dissolving, extract 3 times with the ether jolting, each 40ml discards ether solution, D101 macroporous adsorptive resins (the internal diameter 1.5cm of water liquid by having handled well, the high 12cm of post) on,, discards eluent with 1% sodium hydroxide solution 100ml eluting; Continue with 40% ethanol 100ml 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 water saturated n-butyl alcohol 20ml makes dissolving, and with ammonia solution 10ml washing, branch is got n-butyl alcohol liquid and put evaporate to dryness in the water-bath, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Radix Bupleuri control medicinal material 3g, adds water 100ml, decocts 1 hour, filters, and filtrate is risen from " with ether jolting 3 times, each 40ml ", shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing 12 hours below 10 ℃ with chloroform-methanol-water (65: 35: 10) is developing solvent, launch, take out, dry, spray is with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;
C, get the astragaloside reference substance, add methanol and make 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 2005 B), draw each the 10 μ l of need testing solution under the item of above-mentioned reference substance solution and [discriminating] (2), put respectively on same silica gel g thin-layer plate, lower floor's solution of placing 12 hours below 10 ℃ with chloroform-methanol-water (65: 35: 10) is developing solvent, launch 15cm, take out, dry up, spray is with 10% ethanol solution of sulfuric acid of 1% pair of dimethylbenzaldehyde, and hot blast blows to clear to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
D, get compound capsule with pseudo-ginseng and Chinese fanpalm seed content 5g, porphyrize, the 30ml that adds diethyl ether, supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets the tanshinone reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to thin layer chromatography (appendix VI B) test, draw each 5 μ l of above-mentioned three kinds of solution, on the same silica gel g thin-layer plate of idea, be developing solvent respectively with benzene-ethyl acetate (19: 1), launch, take out, dry; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical kermesinus speckle;
(2) quantitative assay
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (75: 25) is a mobile phase; The detection wavelength is 270nm; Number of theoretical plate calculates by Tanshinone I I A peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the tanshinone reference substance, adds methanol and make the solution that every 1ml contains 10 μ g, promptly;
The content under the content uniformity item is got in the preparation of need testing solution, and porphyrize is got about 1.0g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 25ml that adds, close plug claims to decide weight, supersound extraction (power 100W, frequency 50kHz) 30 minutes, put cold, close plug, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 10ml, by neutral alumina post (100～200 orders of having handled well, 3g, internal diameter 8～10mm), reuse methanol 40ml eluting, merge eluent, evaporate to dryness, residue add methanol make the dissolving and move in the brown measuring bottle of 10ml, add methanol to scale, shake 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;
Every of compound capsule with pseudo-ginseng and Chinese fanpalm seed contains Radix Salviae Miltiorrhizae in tanshinone (C19H18O3), must not be less than 50 μ g.
The present invention carries out secondary development research with novel form, new preparation process, new quality standard to this kind, and the selection dosage form is a capsule, and capsule is easier to disintegrate, and attractive in appearance, swallow easily, and increased patient's selectivity and compliance.
The specific embodiment
Embodiment 1:
(1) prescription: Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 450g Chinese fanpalm seed 450g Radix Bupleuri 350g
Rhizoma Curcumae 350g Radix Salviae Miltiorrhizae 100g Herb Gynostemmae Pentaphylli 100g
Radix Astragali 100g Fructus Ligustri Lucidi 100g spirulina 14g
Microcrystalline Cellulose 150g
More than make 1000
(2) method for making:
More than nine flavor medical materials, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Salviae Miltiorrhizae powder are broken into coarse powder, add 70% alcoholic solution reflux, extract, three times, each 6 times of amounts 1 hour merge alcohol extract, filter, filtrate is concentrated into the clear paste that relative density is 1.10～1.13 (60 ℃); Radix Bupleuri, Rhizoma Curcumae, the Radix Astragali, the Herb Gynostemmae Pentaphylli cutting, Chinese fanpalm seed, Fructus Ligustri Lucidi is smashed to pieces, merges with above-mentioned medicinal residues, decoct with water three times, add 12 times of amounts of water at every turn, decocted 2 hours, collecting decoction filters, and filtrate is concentrated into the clear paste that relative density is 1.15 (60 ℃), add ethanol and make and contain the alcohol amount and reach 65%, stir evenly standing over night, filter, filtrate is concentrated into the clear paste that relative density is 1.13～1.15 (60 ℃), merges with above-mentioned clear paste, decompression recycling ethanol, be dried to dried cream, pulverize, sieve, add spirulina, microcrystalline Cellulose, mixing is granulated, and is encapsulated, make 1000, promptly.
" doubly amount " speech is defined as among the present invention: Chinese crude drug weight and the volume ratio of extracting with liquid, unit is: g/ml.(3) the clear paste baking temperature is investigated
● sample treatment takes by weighing three parts of medical material Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 45g, Chinese fanpalm seed 45g, Radix Bupleuri 35g, Rhizoma Curcumae 35g, Radix Salviae Miltiorrhizae 10g, Herb Gynostemmae Pentaphylli 10g, Radix Astragali 10g, Fructus Ligustri Lucidi 10g, spirulina 1.4g, extraction process by former dosage form is extracted into clear paste, be tiled in little porcelain dish respectively, respectively at 60 ℃, 80 ℃, 100 ℃ drying under reduced pressure, with drying time, character (whether breeze is arranged), tanshinone content the results are shown in Table 1 for investigating index in the dried cream.
● content assaying method is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (75: 25) is a mobile phase; The detection wavelength is 270nm.Number of theoretical plate calculates by the tanshinone peak should be not less than 2000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the tanshinone reference substance, adds methanol and make the solution that every 1ml contains 10 μ g, promptly.
Extractum is got in the preparation of need testing solution, and porphyrize is got about 0.6g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 25ml that adds, close plug claims to decide weight, supersound extraction (power 100W, frequency 50kHz) 30 minutes, put cold, close plug, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 10ml, by neutral alumina post (100～200 orders of having handled well, 3g, internal diameter 8～10mm), reuse methanol 40ml eluting, merge eluent, evaporate to dryness, residue add methanol make the dissolving and move in the brown measuring bottle of 10ml, add methanol to scale, shake 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.
Table 1 drying under reduced pressure temperature is investigated the result
The result shows: 60 ℃, 80 ℃ drying under reduced pressure, and tanshinone content difference is little, and 60 ℃, 80 ℃ dry character meet the requirements, but 60 ℃ of drying times are oversize, and 100 ℃ of drying under reduced pressure have a small amount of breeze, from producing actual consideration, select 80 ℃ of drying under reduced pressure.
Embodiment 2:
(1) prescription: Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 450g Chinese fanpalm seed 450g Radix Bupleuri 350g
Rhizoma Curcumae 350g Radix Salviae Miltiorrhizae 100g Herb Gynostemmae Pentaphylli 100g
Radix Astragali 100g Fructus Ligustri Lucidi 100g spirulina 14g
Microcrystalline Cellulose 80g Pulvis Talci 30g magnesium stearate 15g
More than make 1000
(2) method for making:
More than nine flavor medical materials, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Salviae Miltiorrhizae powder are broken into coarse powder; Radix Bupleuri, Rhizoma Curcumae, the Radix Astragali, Herb Gynostemmae Pentaphylli cutting; Chinese fanpalm seed, Fructus Ligustri Lucidi are smashed to pieces and are added 70% alcohol reflux three times, and each 8 times of amounts 1 hour merge alcohol extract, filter, filtrate is concentrated into the clear paste that relative density is 1.13～1.15 (60 ℃), is dried to dried cream, pulverize, sieve, add spirulina, microcrystalline Cellulose, Pulvis Talci, mixing, granulate, add magnesium stearate, encapsulated, make 1000, promptly.
Embodiment 3:
(1) prescription: Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 450g Chinese fanpalm seed 450g Radix Bupleuri 350g
Rhizoma Curcumae 350g Radix Salviae Miltiorrhizae 100g Herb Gynostemmae Pentaphylli 100g
Radix Astragali 100g Fructus Ligustri Lucidi 100g spirulina 14g
Starch 60g calcium hydrogen phosphate 20g carboxymethyl starch sodium 20g
More than make 1000
(2) method for making:
More than nine flavor medical materials, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Salviae Miltiorrhizae powder are broken into coarse powder, Chinese fanpalm seed, Fructus Ligustri Lucidi are smashed to pieces, add 70% alcohol reflux three times, each 6 times of amounts 1 hour merge alcohol extract, filter, filtrate is concentrated into the clear paste that relative density is 1.10～1.13 (60 ℃); Radix Bupleuri, Rhizoma Curcumae, immersion 2 hours, steam distillation extracted volatile oil 6 hours, and volatile oil device is in addition stored, and decocting liquid is continued to employ; The Radix Astragali, Herb Gynostemmae Pentaphylli cutting merge with above-mentioned two minutes medicinal residues, decoct with water three times, add 12 times of amounts of water at every turn, decocted collecting decoction 2 hours, filter, filtrate is concentrated into the clear paste that relative density is 1.15 (60 ℃), adds ethanol and makes and contain the alcohol amount and reach 65%, stir evenly, standing over night filters, filtrate is concentrated into the clear paste that relative density is 1.13～1.15 (60 ℃), merge with above-mentioned clear paste, be dried to dried cream, pulverize, sieve, add spirulina, starch, calcium hydrogen phosphate, carboxymethyl starch sodium, mixing is granulated, spray into volatile oil, encapsulated, make 1000, promptly.
Quality control
[character] compound capsule with pseudo-ginseng and Chinese fanpalm seed is a hard capsule, and content is that pale brown color is to tan granule and powder; Feeble QI perfume (or spice), mildly bitter flavor.
Compound capsule with pseudo-ginseng and Chinese fanpalm seed content 2g is got in [discriminating] (1), and porphyrize adds ethanol 10ml, and supersound process 30 minutes filters, and filtrate is as need testing solution.Other gets the rotundine hydrochloride reference substance, adds ethanol 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 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with normal hexane-chloroform-methanol (15: 5: 2), launches, take out, dry, put in the iodine vapor and smoked 30 seconds, take out, wave the iodine that adsorbs on the most plate, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(2) get compound capsule with pseudo-ginseng and Chinese fanpalm seed 8g, porphyrize adds methanol solution 50ml, supersound process 30 minutes filters, and filtrate is put evaporate to dryness in the water-bath, residue adds water 30ml makes dissolving, with ether extraction 3 times, each 40ml discards ether solution, D101 macroporous adsorptive resins (the internal diameter 1.5cm of water liquid by having handled well, the high 12cm of post) on,, discards eluent with 1% sodium hydroxide solution 100ml eluting; Continue with 40% ethanol 100ml 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 water saturated n-butyl alcohol 20ml makes dissolving, and with ammonia solution 10ml washing, branch is got n-butyl alcohol liquid and put evaporate to dryness in the water-bath, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Bupleuri control medicinal material 3g, adds water 100ml, decocts 1 hour, filters, and filtrate is risen from " with ether jolting 3 times, each 40ml ", shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing 12 hours below 10 ℃ with chloroform-methanol-water (65: 35: 10) is developing solvent, launch, take out, dry, spray is with 40% ethanol solution of sulfuric acid of 2% paradime thylaminobenzaldehyde, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color.
(3) get the astragaloside reference substance, add methanol and make 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 2005 B), draw each the 10 μ l of need testing solution under the item of above-mentioned reference substance solution and [discriminating] (2), put respectively on same silica gel g thin-layer plate, lower floor's solution of placing 12 hours below 10 ℃ with chloroform-methanol-water (65: 35: 10) is developing solvent, launch 15cm, take out, dry up, spray is with 10% ethanol solution of sulfuric acid of 1% pair of dimethylbenzaldehyde, and hot blast blows to clear to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(4) get compound capsule with pseudo-ginseng and Chinese fanpalm seed content 5g, porphyrize, the 30ml that adds diethyl ether, supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.Other gets the tanshinone reference substance, adds methanol and makes the solution that every 1ml contains 2mg, in contrast product solution.According to thin layer chromatography (appendix VI B) test, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with benzene-ethyl acetate (19: 1), launch, take out, dry.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical kermesinus speckle.
[inspection] should meet every regulation relevant under the capsule item (an appendix I of Chinese Pharmacopoeia version in 2005 L).
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (75: 25) is a mobile phase; The detection wavelength is 270nm.Number of theoretical plate calculates by Tanshinone I I A peak should be not less than 2000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the tanshinone reference substance, adds methanol and make the solution that every 1ml contains 10 μ g, promptly.
The content under the content uniformity item is got in the preparation of need testing solution, and porphyrize is got about 1.0g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 25ml that adds, close plug claims to decide weight, supersound extraction (power 100W, frequency 50kHz) 30 minutes, put cold, close plug, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 10ml, by neutral alumina post (100～200 orders of having handled well, 3g, internal diameter 8～10mm), reuse methanol 40ml eluting, merge eluent, evaporate to dryness, residue add methanol make the dissolving and move in the brown measuring bottle of 10ml, add methanol to scale, shake 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.
Every of compound capsule with pseudo-ginseng and Chinese fanpalm seed contains Radix Salviae Miltiorrhizae in tanshinone (C19H18O3), must not be less than 50 μ g.
[function cures mainly] blood circulation promoting and blood stasis dispelling, promoting the circulation of QI to relieve pain.The auxiliary treatment that is used for the hepatocarcinoma of syndrome of qi stagnation and blood stasis.
Claims (2)
1, the preparation method of compound capsule with pseudo-ginseng and Chinese fanpalm seed, crude drug is made up of Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Chinese fanpalm seed, Radix Bupleuri, Rhizoma Curcumae, Radix Salviae Miltiorrhizae, Herb Gynostemmae Pentaphylli, the Radix Astragali, Fructus Ligustri Lucidi, spirulina, it is characterized in that:
(1) the formulation weight ratio is:
Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) 450 Chinese fanpalm seeds 450 Radix Bupleuri 350
Rhizoma Curcumae 350 Radix Salviae Miltiorrhizaes 100 Herb Gynostemmae Pentaphylli 100
The Radix Astragali 100 Fructus Ligustri Lucidi 100 spirulinas 14
(2) preparation method:
More than nine flavor medical materials, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Salviae Miltiorrhizae powder are broken into coarse powder, Chinese fanpalm seed, Fructus Ligustri Lucidi are smashed to pieces, add alcohol reflux, reflux 1～3 hour merges alcohol extract, filters, filtrate is condensed into clear paste; Radix Bupleuri, Rhizoma Curcumae, immersion 1～3 hour, steam distillation extracts volatile oil, and volatile oil device is in addition stored, and decocting liquid is continued to employ; The Radix Astragali, Herb Gynostemmae Pentaphylli cutting merge with above-mentioned two parts of medicinal residues, decoct with water collecting decoction, filter, filtrate is condensed into clear paste, adds ethanol and makes and contain the alcohol amount and reach 60～75%, stirs evenly, standing over night filters, and filtrate is condensed into clear paste, merges with above-mentioned clear paste, be dried to dried cream, pulverize, sieve, add spirulina, starch, calcium hydrogen phosphate, carboxymethyl starch sodium, mixing is granulated, spray into volatile oil, encapsulated, promptly.
2, preparation method according to claim 1 is characterized in that its concrete steps are:
More than nine flavor medical materials, Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae), Radix Salviae Miltiorrhizae powder are broken into coarse powder, Chinese fanpalm seed, Fructus Ligustri Lucidi are smashed to pieces, add 6 times of amount 70% alcoholic solution and reflux, extract each 1 hour three times, merge alcohol extract, filter, it is 1.10～1.13 clear paste that filtrate is concentrated into 60 ℃ of following relative densities; Radix Bupleuri, Rhizoma Curcumae, immersion 2 hours, steam distillation extracted volatile oil 6 hours, and volatile oil device is in addition stored, and decocting liquid is continued to employ; The Radix Astragali, Herb Gynostemmae Pentaphylli cutting merge with above-mentioned two minutes medicinal residues, decoct with water three times, add 12 times of amounts of water at every turn, decocted collecting decoction 2 hours, filter, it is 1.15 clear paste that filtrate is concentrated into 60 ℃ of following relative densities, adds ethanol and makes and contain the alcohol amount and reach 65%, stir evenly, standing over night filters, and it is 1.13～1.15 clear paste that filtrate is concentrated into 60 ℃ of following relative densities, merge with above-mentioned clear paste, be dried to dried cream, pulverize, sieve, add spirulina, starch, calcium hydrogen phosphate, carboxymethyl starch sodium, mixing is granulated, and sprays into volatile oil, encapsulated, promptly.
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| CNB2006100404034A CN100515476C (en) | 2006-05-06 | 2006-05-06 | Compound capsule with pseudo-ginseng and Chinese fanpalm seed, its preparation process and quality control method |
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| CNB2006100404034A CN100515476C (en) | 2006-05-06 | 2006-05-06 | Compound capsule with pseudo-ginseng and Chinese fanpalm seed, its preparation process and quality control method |
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| CN103816328A (en) * | 2014-03-12 | 2014-05-28 | 潘国栋 | Cancer-inhibiting and pain-relieving patch |
| CN104721730A (en) * | 2014-11-28 | 2015-06-24 | 悦康药业集团安徽天然制药有限公司 | Compound capsule of stephania sinica diels and fructus livistonae chinensis and preparation method thereof |
| CN114719947B (en) * | 2022-06-08 | 2022-08-09 | 潍坊市检验检测中心 | Soft capsule loading difference detection device for analysis and detection method thereof |
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Non-Patent Citations (4)
| Title |
|---|
| 中华人民共和国药典. 52. 2005 * |
| 中药药剂学. 范碧亭主编，348，上海科学技术出版社. 1997 * |
| 国家中成药标准汇编. 477－479，国家药品监督管理局. 2002 中华人民共和国药典. 52. 2005 中药药剂学. 范碧亭主编，348，上海科学技术出版社. 1997 |
| 国家中成药标准汇编. 477－479，国家药品监督管理局. 2002 * |
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