CN1493308A - Preparation technology of sugarless small radix bupleuri granular agent - Google Patents
Preparation technology of sugarless small radix bupleuri granular agent Download PDFInfo
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- CN1493308A CN1493308A CNA021258058A CN02125805A CN1493308A CN 1493308 A CN1493308 A CN 1493308A CN A021258058 A CNA021258058 A CN A021258058A CN 02125805 A CN02125805 A CN 02125805A CN 1493308 A CN1493308 A CN 1493308A
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Abstract
A concentrated non-sugar bupleurum root particles, its preparing process, and the method for testing its content and disclosed. The particle has full effect, stable and controllable quality.
Description
Technical field
The present invention relates to the new preparation process of small radix bupleuri granular agent, belong to field of traditional Chinese.
Background technology
Herba Sidae Rhombifoliae soup comes from the classic doctor of traditional Chinese medical science nationality treatise on Febrile Diseases, is made up of Radix Bupleuri, Radix Codonopsis, Fructus Jujubae, the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Zingiberis Recens, Radix Glycyrrhizae, is used for the treatment of alternate attack of chill and fever, and costa sternales is bitter full, and vexed happiness is told, diseases such as bitter taste in the mouth and dry throat.General dosage form has oral liquid, granule, tablet etc. at present.Little bupleurum particles (electuary) promptly is to be prepared from modern crafts on the Herba Sidae Rhombifoliae soup basis, now record in the 8th of the Sanitation Ministry medicine standard, but add a large amount of cane sugar powders in its technology, modern study shows, sucrose can produce harmful substance with composition generation chemical reactions such as some Chinese medicine protein, tannins, can decompose the some drugs effective ingredient, disturb some drugs to absorb, influence the final curative effect of medicine; While preparation sugar content height, big, the easy moisture absorption of volume makes troubles, and has increased the producing and selling cost for production, accumulating; This external preparation sugar content height is unsuitable for using with the patient of diseases such as diabetes, hypertension, obesity, thereby has retrained the clinical practice of little bupleurum particles (electuary).The little bupleurum particles of sugar-free concentrated type of the present invention (electuary) is at the problems referred to above, done innovation at process aspect, remove cane sugar powders a large amount of in the former technology, use an amount of dextrin instead and replace, granulate after mixing soft material, so both reduced medicine viscosity, be beneficial to granulation, make the grain graininess of making good again, color and luster is even, and melting is good.We add an amount of not containing heat, have no side effect in addition, and safe and reliable stevioside with the antidote hardship, is easy to inlet as correctives.
Technology contents
The object of the invention provides a kind of good stability, curative effect height, can enlarge the medication object the new preparation process of small radix bupleuri granular agent; The object of the invention also is to provide a kind of quality determining method of small radix bupleuri granular agent.
The present invention seeks to be achieved through the following technical solutions:
Radix Bupleuri 500-1000 weight portion Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) 200-400 weight portion
Radix Scutellariae 200-400 weight portion Radix Codonopsis 200-400 weight portion
Radix Glycyrrhizae 200-400 weight portion Rhizoma Zingiberis Recens 200-400 weight portion
Fructus Jujubae 200-400 weight portion
More than seven flavors, Radix Bupleuri, Radix Scutellariae, Radix Codonopsis, Radix Glycyrrhizae and Fructus Jujubae decoct with water 2-4 time, each 1-2 hour, collecting decoction, filtration, filtrate is concentrated in right amount.Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens), Rhizoma Zingiberis Recens shine the percolation of fluid extract and extractum item-F, make solvent with 60-80% ethanol, flood after 12-36 hour, percolation slowly, collect percolate, reclaim ethanol, merge with above-mentioned concentrated solution, be concentrated into clear paste, it is an amount of to add dextrin, stevioside and ethanol, and mixing is made granule, drying, promptly.
Medicine of the present invention is that pale brown color is to tan granule; Sweet, little hardship of distinguishing the flavor of.
The discrimination method of medicine of the present invention is: get medicine 1g of the present invention, add methanol 10ml, supersound process 20 minutes filters, and filtrate is as need testing solution.Other gets the baicalin reference substance, adds Diluted Alcohol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution.According to the thin layer chromatography test, draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with acetic acid, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Get medicine 10g of the present invention, porphyrize adds 5mol/L hydrochloric acid 30ml and chloroform 30ml, and reflux 1 hour is put coldly, divides and to get chloroform solution, and evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance in addition, add dehydrated alcohol and make the solution that contains 1mg among every 1ml, product solution in contrast, test according to thin layer chromatography, draw each 3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 20: 7: 2 benzene-ethyl acetate-glacial acetic acid was developing solvent, launched, and took out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 105 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Content of drug assay method of the present invention is: according to high performance liquid chromatography, chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 47: 53: 0.2 methanol-water-phosphoric acid are mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the baicalin peak should be not less than 2500; Precision takes by weighing at 4 hours baicalin reference substance of 60 ℃ of drying under reduced pressure an amount of, adds methanol and makes the solution that contains 60 μ g among every 1ml, promptly gets reference substance solution; Get the medicine of the present invention under the content uniformity item, porphyrize is got about 1g, the accurate title, decide, and adds 70% ethanol 80ml, reflux 3 hours, put coldly, filter, filtrate is put in the 100ml measuring bottle, with 70% ethanol gradation washing container and residue, washing liquid is filtered in the same measuring bottle, adds 70% ethanol to scale, shake up, promptly get need testing solution, accurate respectively reference substance solution and each 10-20 μ l injection chromatograph of liquid of need testing solution drawn, measure, promptly.
Medicine of the present invention contains Radix Scutellariae with baicalin (C for every bag
21H
18O
11) meter, must not be less than 20.0mg.Every packed 3g, an oral 3g, 3 times on the one.
Granule of the present invention, the institute that has Herba Sidae Rhombifoliae soup through the scientific experiments confirmation is powerful, stable and controllable for quality.
Embodiment
Radix Bupleuri 848g Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) 318g Radix Scutellariae 318g Radix Codonopsis 318g
Radix Glycyrrhizae 318g Rhizoma Zingiberis Recens 318g Fructus Jujubae 318g
More than seven flavors, Radix Bupleuri, Radix Scutellariae, Radix Codonopsis, Radix Glycyrrhizae and Fructus Jujubae decoct with water secondary, each 1.5 hours, collecting decoction filtered, filtrate is concentrated in right amount.Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens), Rhizoma Zingiberis Recens shine the percolation of fluid extract and extractum item-F, make solvent with 70% ethanol, flood after 24 hours, with the speed of per minute 1-3ml percolation slowly, collect the about 3180ml of percolate, recovery ethanol, merge with above-mentioned concentrated solution, being concentrated into relative density is the clear paste of 1.32-1.35 (75～80 ℃), and it is an amount of to add dextrin, stevioside and ethanol, mixing, make granule, drying is made 1000g, promptly.
Claims (4)
1, a kind of preparation method of sugar-free concentrated type small radix bupleuri granular agent is characterized in that this method is:
Radix Bupleuri 500-1000 weight portion Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) 200-400 weight portion
Radix Scutellariae 200-400 weight portion Radix Codonopsis 200-400 weight portion
Radix Glycyrrhizae 200-400 weight portion Rhizoma Zingiberis Recens 200-400 weight portion
Fructus Jujubae 200-400 weight portion
More than seven flavors, Radix Bupleuri, Radix Scutellariae, Radix Codonopsis, Radix Glycyrrhizae and Fructus Jujubae decoct with water 2-4 time, each 1-2 hour, collecting decoction, filtration, filtrate is concentrated in right amount.Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens), Rhizoma Zingiberis Recens shine the percolation of fluid extract and extractum item-F, make solvent with 60-80% ethanol, flood after 12-36 hour, slowly percolation, collect percolate, reclaim ethanol, merge, be concentrated into clear paste with above-mentioned concentrated solution, it is an amount of to add dextrin, stevioside and ethanol, mixing is made granule, promptly.
2, the preparation method of a kind of sugar-free concentrated type small radix bupleuri granular agent as claimed in claim 1 is characterized in that this method is:
Radix Bupleuri 848 weight portion Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens)s 318 weight portion Radix Scutellariaes 318 weight portions
Radix Codonopsis 318 weight portion Radix Glycyrrhizaes 318 weight portion Rhizoma Zingiberis Recenss 318 weight portions
Fructus Jujubae 318 weight portions
More than seven flavors, Radix Bupleuri, Radix Scutellariae, Radix Codonopsis, Radix Glycyrrhizae and Fructus Jujubae decoct with water secondary, each 1.5 hours, collecting decoction filtered, filtrate is concentrated in right amount.Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens), Rhizoma Zingiberis Recens shine the percolation of fluid extract and extractum item-F, make solvent with 70% ethanol, flood after 24 hours, with the speed of per minute 1-3ml percolation slowly, collect the about 3180ml of percolate, reclaim ethanol, merge with above-mentioned concentrated solution, being concentrated into relative density is the clear paste of 1.32-1.35 (75～80 ℃), it is an amount of to add dextrin, stevioside and ethanol, mixing is made granule, promptly.
3, the discrimination method of the small radix bupleuri granular agent made of preparation method is as claimed in claim 1 or 2: get medicine 1g of the present invention, add methanol 10ml, supersound process 20 minutes filters, and filtrate is as need testing solution.Other gets the baicalin reference substance, adds Diluted Alcohol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution.According to the thin layer chromatography test, draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with acetic acid, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Get medicine 10g of the present invention, porphyrize adds 5mol/L hydrochloric acid 30ml and chloroform 30ml, and reflux 1 hour is put coldly, divides and to get chloroform solution, and evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Extracting liquorice subacid reference substance in addition, add dehydrated alcohol and make the solution that contains 1mg among every 1ml, product solution in contrast, test according to thin layer chromatography, draw each 3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 20: 7: 2 benzene-ethyl acetate-glacial acetic acid was developing solvent, launched, and took out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 105 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
4, the content assaying method of the small radix bupleuri granular agent made of preparation method is as claimed in claim 1 or 2: according to high performance liquid chromatography, it is filler that chromatographic condition is tested with octadecylsilane chemically bonded silica with system suitability; 47: 53: 0.2 methanol-water-phosphoric acid are mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the baicalin peak should be not less than 2500; Precision takes by weighing at 4 hours baicalin reference substance of 60 ℃ of drying under reduced pressure an amount of, adds methanol and makes the solution that contains 60 μ g among every 1ml, promptly gets reference substance solution; Get the medicine of the present invention under the content uniformity item, porphyrize, get about 1g, the accurate title, decide, and adds 70% ethanol 80ml, reflux 3 hours, put cold, filter, filtrate is put in the 100ml measuring bottle, with 70% ethanol gradation washing container and residue, washing liquid is filtered in the same measuring bottle, add 70% ethanol to scale, shake up, promptly get need testing solution, accurate respectively reference substance solution and each 10-20 μ l injection chromatograph of liquid of need testing solution drawn, measure, every bag of 3g dress small radix bupleuri granular agent contains Radix Scutellariae in baicalin, must not be less than 20.0mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02125805 CN1244813C (en) | 2002-07-17 | 2002-07-17 | Preparation technology of sugarless small radix bupleuri granular agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02125805 CN1244813C (en) | 2002-07-17 | 2002-07-17 | Preparation technology of sugarless small radix bupleuri granular agent |
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| Publication Number | Publication Date |
|---|---|
| CN1493308A true CN1493308A (en) | 2004-05-05 |
| CN1244813C CN1244813C (en) | 2006-03-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02125805 Expired - Lifetime CN1244813C (en) | 2002-07-17 | 2002-07-17 | Preparation technology of sugarless small radix bupleuri granular agent |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102526391A (en) * | 2010-12-16 | 2012-07-04 | 天津中敖生物科技有限公司 | Livestock Chinese medicinal composition with refrigerating function and preparation method thereof |
| CN103784923A (en) * | 2014-01-27 | 2014-05-14 | 海南葫芦娃制药有限公司 | Bupleurum tenue granules and preparation method thereof |
| CN103961665A (en) * | 2014-05-07 | 2014-08-06 | 江西百神药业股份有限公司 | Preparation method of common goldenrop granules |
| CN104225530A (en) * | 2014-09-11 | 2014-12-24 | 江西九华药业有限公司 | Preparation method of common goldenrop particles |
| CN105902979A (en) * | 2016-05-17 | 2016-08-31 | 海南中宝制药股份有限公司 | Preparation method of minor radix bupleuri granules |
| CN106353422A (en) * | 2016-08-30 | 2017-01-25 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Content measuring method for refreshing and pressure reducing pills |
| CN107496884A (en) * | 2017-09-28 | 2017-12-22 | 安徽协和成制药有限公司 | Xiao Chai Hu granules composition and preparation method thereof |
| CN110960663A (en) * | 2019-12-21 | 2020-04-07 | 江西济民可信金水宝制药有限公司 | Preparation method of Xiaochaihu granules |
| CN113599404A (en) * | 2021-09-23 | 2021-11-05 | 四川省中医药科学院 | Preparation method of bupleurum extract and bupleurum tenue granules |
-
2002
- 2002-07-17 CN CN 02125805 patent/CN1244813C/en not_active Expired - Lifetime
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102526391A (en) * | 2010-12-16 | 2012-07-04 | 天津中敖生物科技有限公司 | Livestock Chinese medicinal composition with refrigerating function and preparation method thereof |
| CN103784923A (en) * | 2014-01-27 | 2014-05-14 | 海南葫芦娃制药有限公司 | Bupleurum tenue granules and preparation method thereof |
| CN103784923B (en) * | 2014-01-27 | 2016-09-07 | 海南葫芦娃药业集团股份有限公司 | Xiao Chai Hu granules and preparation method thereof |
| CN103961665A (en) * | 2014-05-07 | 2014-08-06 | 江西百神药业股份有限公司 | Preparation method of common goldenrop granules |
| CN103961665B (en) * | 2014-05-07 | 2017-09-01 | 江西百神药业股份有限公司 | A kind of preparation method of Xiao Chai Hu granules |
| CN104225530A (en) * | 2014-09-11 | 2014-12-24 | 江西九华药业有限公司 | Preparation method of common goldenrop particles |
| CN105902979A (en) * | 2016-05-17 | 2016-08-31 | 海南中宝制药股份有限公司 | Preparation method of minor radix bupleuri granules |
| CN106353422A (en) * | 2016-08-30 | 2017-01-25 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Content measuring method for refreshing and pressure reducing pills |
| CN107496884A (en) * | 2017-09-28 | 2017-12-22 | 安徽协和成制药有限公司 | Xiao Chai Hu granules composition and preparation method thereof |
| CN110960663A (en) * | 2019-12-21 | 2020-04-07 | 江西济民可信金水宝制药有限公司 | Preparation method of Xiaochaihu granules |
| CN113599404A (en) * | 2021-09-23 | 2021-11-05 | 四川省中医药科学院 | Preparation method of bupleurum extract and bupleurum tenue granules |
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| Publication number | Publication date |
|---|---|
| CN1244813C (en) | 2006-03-08 |
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