CN105497712A - Manufacturing method of cough and asthma treating preparation - Google Patents
Manufacturing method of cough and asthma treating preparation Download PDFInfo
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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Abstract
The invention discloses a manufacturing method of a cough and asthma treating preparation. The cough and asthma treating preparation is mainly prepared from balloon flowers, gypsum, pericarpium papaveris, liquorice roots, herbal ephedrae, stemona japonica, bitter apricot seeds and auxiliary materials. The specific manufacturing process and parameters of the cough and asthma treating preparation are improved according to the properties of all medicines in the cough and asthma treating preparation composition and the effects of the medicines in the composition, the effective constituent ephedrine of herbal ephedrae can be easily measured, and the content of the measured effective constituent of herbal ephedrae is high. The medicine can be more refined, the efficacy is more remarkable, and the clinical treatment effect is good.
Description
Technical field
The invention belongs to the field of Chinese medicines, be specifically related to a kind of manufacture method of tetrahydro-isoquinolin preparation.
Background technology
Chinese medicine extraction is a kind of method conventional in herbal pharmaceutical, and chemical composition of Chinese materia medica is extremely complicated, need extract the effective active ingredient of Chinese herbs of human body from the mixture of complexity.To improve drug effect.
Tetrahydro-isoquinolin is made primarily of Radix Platycodonis, Gypsum Fibrosum, Pericarpium Papaveris, Radix Glycyrrhizae, Herba Ephedrae, the Radix Stemonae and Semen Armeniacae Amarum.The tetrahydro-isoquinolin made has should lead to lung qi, effect of relieving cough and asthma.For bronchial asthma, cough, old productive cough.
In prior art, tetrahydro-isoquinolin makes like this: Radix Platycodonis, Gypsum Fibrosum are ground into fine powder respectively, and Pericarpium Papaveris, Radix Glycyrrhizae, Herba Ephedrae decoct with water secondary, each 3 hours, collecting decoction, and filter, filtrate is condensed into cream; The Radix Stemonae 60% alcohol heating reflux extracts, Semen Armeniacae Amarum (deoiling) more than 85% alcohol heating reflux extracts secondary, merge above ethanol extract, reclaim ethanol and be condensed into cream, merge with above-mentioned water condensed cream, add the fine powders such as Radix Platycodonis and right amount of auxiliary materials mixing, make granule, dry, tabletting, to obtain final product.But inventor finds in research process, adopt existing extraction process to make in tetrahydro-isoquinolin, the effective ingredient ephedrine of Herba Ephedrae is not easily measured.Make the clinical efficacy of tetrahydro-isoquinolin desirable not enough.
Summary of the invention
The invention provides a kind of manufacture method of tetrahydro-isoquinolin preparation.The present invention is according to the character of medicine each in tetrahydro-isoquinolin preparation recipe, and this medicine role in prescription, the concrete processing technology of tetrahydro-isoquinolin preparation and parameter are improved, the effective ingredient ephedrine of Herba Ephedrae is easily measured, and it is high to measure Content of Ephedrine With.Make the refine more of this medicine, drug effect is more remarkable, and clinical efficacy is good.
To achieve these goals, the invention provides following technical scheme: a kind of manufacture method of tetrahydro-isoquinolin preparation, described tetrahydro-isoquinolin preparation calculates by weight, makes primarily of Radix Platycodonis 10-30 part, Gypsum Fibrosum 10-30 part, Pericarpium Papaveris 10-30 part, Radix Glycyrrhizae 30-50 part, Herba Ephedrae 30-50 part, Radix Stemonae 10-30 part and Semen Armeniacae Amarum 30-50 part; The manufacture method of described tetrahydro-isoquinolin preparation is: get Herba Ephedrae, adds alcoholic solution reflux, extract, 2-4 time of 70%-90%, filters, merging filtrate, reclaims ethanol, obtains alcohol extract, for subsequent use; Filtering residue adds water extraction 2-3 time again, and filter, merging filtrate, after being condensed into concentrated solution, merging with above-mentioned alcohol extract, be condensed into extractum, obtain Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, decoct with water, filter, filtrate reduced in volume, to clear paste, adds ethanol and makes alcohol content reach 55%-85%, stir, leave standstill 12-48 hour, filter, decompression filtrate recycling ethanol is also condensed into extractum, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, add Platycodon Root, gypsum powder and adjuvant, mixing, makes pharmaceutical preparation.
In the manufacture method of aforesaid tetrahydro-isoquinolin preparation, described tetrahydro-isoquinolin preparation calculates by weight, makes primarily of Radix Platycodonis 20 parts, 20 parts, Gypsum Fibrosum, Pericarpium Papaveris 20 parts, 40 parts, Radix Glycyrrhizae, 40 parts, Herba Ephedrae, the Radix Stemonae 20 parts and Semen Armeniacae Amarum 40 parts.
In the manufacture method of aforesaid tetrahydro-isoquinolin preparation, the manufacture method of described tetrahydro-isoquinolin preparation is: get Herba Ephedrae, adds alcoholic solution reflux, extract, 2-4 time of 8-12 times amount 70%-90%, each 2-3h, filters, merging filtrate, reclaims ethanol, obtains alcohol extract, for subsequent use; Filtering residue adds 6-10 times amount water extraction 2-3 time again, each 1-3 hour, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and being concentrated into relative density at 50-60 DEG C is the extractum of 1.1-1.2, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 7-12 times of soak by water 2-4 time, each 0.5-3 hour, filter, merging filtrate, concentrating under reduced pressure becomes clear paste, adding ethanol makes alcohol content reach 55%-85%, stirs, and leaves standstill 12-48 hour, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, add Platycodon Root, gypsum powder and adjuvant, mixing, makes pharmaceutical preparation.
In the manufacture method of aforesaid tetrahydro-isoquinolin preparation, the manufacture method of described tetrahydro-isoquinolin preparation is: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaims ethanol, obtains alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, add Platycodon Root, gypsum powder and adjuvant, mixing, makes pharmaceutical preparation.
In the manufacture method of aforesaid tetrahydro-isoquinolin preparation, described pharmaceutical preparation is oral formulations.
In the manufacture method of aforesaid tetrahydro-isoquinolin preparation, described oral formulations is tablet, granule, capsule or pill.
In the manufacture method of aforesaid tetrahydro-isoquinolin preparation, described tablet makes like this: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaims ethanol, obtains alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, add Platycodon Root, gypsum powder, and the dextrine powder mixing of the amount of making 10-20%, with alcohol granulation, dry, tabletting, to obtain final product.
In the manufacture method of aforesaid tetrahydro-isoquinolin preparation, described granule makes like this: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaims ethanol, obtains alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, add Radix Platycodonis, gypsum powder, the dextrine powder of the amount of making 10-20% and the cane sugar powder mixing of the amount of making 10-20%, with alcohol granulation, to obtain final product.
In the manufacture method of aforesaid tetrahydro-isoquinolin preparation, described capsule makes like this: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaims ethanol, obtains alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, and add the starch mixing of Platycodon Root, gypsum powder, 10-20%, granulate, incapsulate, to obtain final product.
In the manufacture method of aforesaid tetrahydro-isoquinolin preparation, described pill makes like this: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaims ethanol, obtains alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, dry, pulverize, obtains Herba Ephedrae extract, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into cream, for subsequent use; The Radix Stemonae 60% alcohol heating reflux extracts, extract secondary with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream merge, dry, pulverize into powder, then mix with above-mentioned Herba Ephedrae extract, Platycodon Root and gypsum powder, add the refined honey of medicated powder amount 25%-40%, water-honeyed pill is made by suitable quantity of water, dry, to obtain final product.
The present invention adopts Radix Platycodonis, Gypsum Fibrosum, Pericarpium Papaveris, Radix Glycyrrhizae, Herba Ephedrae, the Radix Stemonae and Semen Armeniacae Amarum to make medicine, i.e. tetrahydro-isoquinolin preparation, and each raw material has good synergism, and the preparation made has and should lead to lung qi, effect of relieving cough and asthma.For bronchial asthma, cough, the diseases such as old productive cough.
The manufacture method method of existing production tetrahydro-isoquinolin preparation is: Radix Platycodonis, Gypsum Fibrosum are ground into fine powder respectively, and Pericarpium Papaveris, Radix Glycyrrhizae, Herba Ephedrae decoct with water secondary, each 3 hours, collecting decoction, and filter, filtrate is condensed into cream; The Radix Stemonae 60% alcohol heating reflux extracts, Semen Armeniacae Amarum (deoiling) more than 85% alcohol heating reflux extracts secondary, merge above ethanol extract, reclaim ethanol and be condensed into cream, merge with above-mentioned water condensed cream, add the fine powders such as Radix Platycodonis and right amount of auxiliary materials mixing, make granule, dry, tabletting, to obtain final product.But inventor finds in research process, adopt and make in tetrahydro-isoquinolin in this way, the effective ingredient of Herba Ephedrae is not easily measured.Make the clinical efficacy of tetrahydro-isoquinolin desirable not enough.Inventor also finds in technical study, and adopt the inventive method Herba Ephedrae and Radix Platycodonis to be extracted separately, in the tetrahydro-isoquinolin preparation made, the effective ingredient ephedrine of Herba Ephedrae is easily measured, and the effective ingredient Content of Ephedrine With of the Herba Ephedrae of measuring is high.This just makes the refine more of this medicine, and drug effect is more remarkable, and clinical efficacy is good.Therefore this technique facilitates the dissolution rate of the dissolution rate of effective ingredient in Herba Ephedrae, particularly ephedrine, and ephedrine is active component important in Herba Ephedrae, has very strong pharmacologically active, after the dissolution rate raising of ephedrine, effectively can improve the drug effect of tetrahydro-isoquinolin preparation.
Compared with prior art, in the tetrahydro-isoquinolin preparation that the method for the invention makes, the effective ingredient in Herba Ephedrae is easily measured, and the Content of Ephedrine With measured is high.Effectively can improve the drug effect of tetrahydro-isoquinolin preparation.
Invention has been a large amount of experimentatioies, is below the result of experimentation of the present invention:
Experimental example 1: Content of Ephedrine With is investigated
1 raw material
Send out tetrahydro-isoquinolin, make by the method for embodiment 1 for 1.1.
1.2 existing tetrahydro-isoquinolin: make by following technique:
Prescription: Radix Platycodonis 200g, Gypsum Fibrosum 200g, Pericarpium Papaveris 200g, Radix Glycyrrhizae 400g, Herba Ephedrae 400g, Radix Stemonae 200g and Semen Armeniacae Amarum 400g and adjuvant.
Technique: Radix Platycodonis, Gypsum Fibrosum are ground into fine powder respectively, Pericarpium Papaveris, Radix Glycyrrhizae, Herba Ephedrae decoct with water secondary, each 3 hours, collecting decoction, and filter, filtrate is condensed into cream; The Radix Stemonae 60% alcohol heating reflux extracts, Semen Armeniacae Amarum (deoiling) more than 85% alcohol heating reflux extracts secondary, merge above ethanol extract, reclaim ethanol and be condensed into cream, merge with above-mentioned water condensed cream, add the fine powders such as Radix Platycodonis and right amount of auxiliary materials mixing, make granule, dry, tabletting, to obtain final product.
1.4Waters1525HPLC; Chromatographic column Merck-C
18(5um, 150mm × 4.6mm).Negative controls self-control ephedrine reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 171241-200506, for assay); Methanol is chromatographically pure, and water is double distilled water, and other reagent is analytical pure.
2 experimental techniques and result
2.1 chromatographic condition
Mobile phase: methanol-water (80:20), determined wavelength: 245nm, flow velocity 0.8ml/min, sample size: 20ul.Column temperature: 30 DEG C.
The preparation of 2.2 reference substance solution
Precision takes ephedrine reference substance 12.5mg, put in 100ml measuring bottle, is diluted to scale with water dissolution, shake up, precision measures 10ml, is placed in 25ml measuring bottle, add periodic acid solution, 1ml, 0.25mol/l sodium hydroxide solution 2.5ml, shakes up, and places 30min, regulate pH to neutral with 0.5mol/l hydrochloric acid solution, add methanol to scale, shake up, obtain (containing ephedrine 50 μ g in every 1ml).
The preparation of 2.3 need testing solutions
The preparation of need testing solution 1: get tetrahydro-isoquinolin of the present invention, porphyrize, precision takes fine powder 4g, adds 5mol/l sodium hydroxide solution 120ml, shakes loose, add sodium chloride 7.5g, supersound process 10min, distillation, collects the nearly 190ml of distillate with the 200ml measuring bottle filling 0.5mol/l hydrochloric acid solution 10ml in advance, add water to scale, shake up.Precision measures 10ml, puts in 25ml measuring bottle, and the method under Zhao's reference substance solution preparation, from " adding periodic acid solution ", operates in accordance with the law, to obtain final product.
The preparation of need testing solution 2: enchashment has tetrahydro-isoquinolin, porphyrize, precision takes fine powder 4g, adds 5mol/l sodium hydroxide solution 120ml, shakes loose, add sodium chloride 7.5g, supersound process 10min, distillation, collects the nearly 190ml of distillate with the 200ml measuring bottle filling 0.5mol/l hydrochloric acid solution 10ml in advance, add water to scale, shake up.Precision measures 10ml, puts in 25ml measuring bottle, and the method under Zhao's reference substance solution preparation, from " adding periodic acid solution ", operates in accordance with the law, to obtain final product.
2.4 determined wavelength are selected
The determination of determined wavelength: get ephedrine reference substance solution, in the interscan of 200-400nm wave-length coverage, ephedrine has absorption maximum at 254nm place, therefore selects 254nm to be determined wavelength.
2.5 Specification Curve of Increasing
Precision takes the ephedrine reference substance 25.05mg being dried to permanent quality, be placed in 100ml measuring bottle, is diluted to scale, shakes up with water dissolution, measure 1 respectively, 2,4,6,8,10ml, is placed in 25ml measuring bottle, adds periodic acid solution 1ml, 0.25mol/l sodium hydroxide solution 2.5ml, shakes up, and places 30min, regulates pH to neutral with 0.5mol/l dissolving with hydrochloric acid, add methanol to scale, shake up, obtain 1ml containing 10.02,20.04,40.08, the solution of 60.12,80.16,100.2 μ g ephedrines.Get above-mentioned solution sample introduction 20 μ l respectively, with sample size X for abscissa, integrating peak areas value Y is vertical coordinate, drawing standard curve obtains A=78152.46C-170815, r=0.9999. result shows, ephedrine is within the scope of 0.2004-2.0040 μ g/ml, and sample size and peak area are good linear relationship.
2.6 precision test
Get need testing solution 20 microlitre, injection liquid chromatography, record chromatogram, continuous sample introduction 5 times, RSD is 1.2%.Test shows, precision is good.
The mensuration of 2.7 need testing solution stability
2.7.1 the mensuration of need testing solution 1 stability: respectively at the the the 0th, 1,2,4,6,8h draws need testing solution 1, and uptake is 20 microlitres, injection liquid chromatography, record chromatogram, result RSD is 1.36%, and result shows, need testing solution 1 is stable in 4h, can meet the needs of mensuration.
2.7.2 the mensuration of need testing solution 2 stability: respectively at the the the 0th, 1,2,4,6,8h draws need testing solution 2, and uptake is 20 microlitres, injection liquid chromatography, record chromatogram, result RSD is 1.36%, and result shows, need testing solution 2 is stable in 4h, can meet the needs of mensuration.
2.8 repeatability tests
Get with batch tetrahydro-isoquinolin of the present invention and existing tetrahydro-isoquinolin respectively, detect 5 times respectively, result RSD is 1.21% and 1.23%, shows that this method repeatability is good in accordance with the law.
2.9 application of sample recovery tests
Precision takes the tetrahydro-isoquinolin of the present invention of known content and existing tetrahydro-isoquinolin respectively, each about 1g, accurately weighed, add ephedrine reference substance solution (1.02mg/ml) 4,5,6ml respectively, by above-mentioned need testing solution 1 and need testing solution 2 preparation method and chromatographic condition, prepare application of sample and reclaim need testing solution 1 and need testing solution 2, and inject high performance liquid chromatograph, the following column count formulae discovery response rate.Calculate average recovery rate be 100.52% and 99.99%, RSD be 1.27% and 1.28%.Result shows, assay method is feasible, meets assay requirement.
2.10 sample determination
Measure tetrahydro-isoquinolin of the present invention and existing tetrahydro-isoquinolin respectively, by need testing solution 1 and the preparation of need testing solution 2 preparation method, parallelly measure 6 parts, draw 20 microlitres for every part, inject high performance liquid chromatograph, record chromatographic peak area, external standard method calculates, and Content of Ephedrine With, the results are shown in 1.
The assay result of table 1 ephedrine
As known from Table 1, the average content of tetrahydro-isoquinolin Ephedrine of the present invention is 3.85mg/g, and the average content of existing tetrahydro-isoquinolin Ephedrine is 3.22mg/g.
Conclusion: compared with existing tetrahydro-isoquinolin, the content of the effective ingredient ephedrine of tetrahydro-isoquinolin epheday intermedia of the present invention is higher.In like manner, the preparation of other dosage forms made according to extracting method of the present invention, the active constituent content of Herba Ephedrae also should increase.
Experimental example 2: Effect tests
1 experiment material
1.1 medicine
1.1.1 tetrahydro-isoquinolin of the present invention, with embodiment 1.
1.1.2 existing tetrahydro-isoquinolin, with experimental example 1.
1.2 laboratory animal ICR mices and DPH Cavia porcellus, be male, provided by Zhejiang Province's Experimental Animal Center, and the quality certification number is 96 (002) numbers.
2 experimental techniques and result
2.1 mouse lung phenol red excretion tests
ICR mice 30, body weight 18-22g, be divided into 3 groups at random, namely of the present invention group, matched group, existing tetrahydro-isoquinolin group, often organize 10, of the present invention group of gavage tetrahydro-isoquinolin of the present invention, dosage is 20g/kg, existing tetrahydro-isoquinolin group, the existing tetrahydro-isoquinolin of gavage, given low is 20g/kg, equal administration 1 time, the normal saline of Normal group gavage same dose, the phenol red solution 0.5ml of every mouse peritoneal injection 0.25% after 30min, and mice is put to death after 30min, back of the body position is fixed, isolate trachea, insert plastic tube, the sodium bicarbonate solution 0.4ml at every turn drawing 5% with the syringe of 1ml rinses, 3 times like this, the washing liquid of 3 times is merged, add isopyknic dehydrated alcohol, the centrifugal 15min of 100rpm, get supernatant, compare with standard pipe in 546nm colorimetric, calculate the phenol red concentration of eluate, the results are shown in Table 2.
Table 2 is on the impact of Intestinal propulsive rate
Note: compare with matched group
+p<0.05,
++p<0.01; * P<0.05 is compared with existing tetrahydro-isoquinolin group.
2.2 Cavia porcellus citric acid draw coughs test
DHP Cavia porcellus, male, body weight 195-205g.Just Cavia porcellus is placed in the glass bell jar of 3L volume, with 402 type ultrasonic atomizatios the citric acid of 17.5% be atomized and spray in glass bell jar, stop after spraying 1min, the cough latent period of observed and recorded Cavia porcellus, choose the Cavia porcellus 30 being less than 120 seconds incubation period, 3 groups are divided into according to body weight and cough latent period collocation, often organize 10, namely of the present invention group, matched group, existing tetrahydro-isoquinolin group, often organize 10, of the present invention group of gavage tetrahydro-isoquinolin of the present invention, dosage is 20g/kg, existing tetrahydro-isoquinolin group, the existing tetrahydro-isoquinolin of gavage, given low is 20g/kg, the normal saline of Normal group gavage same dose, administration every day 1 time, continuous 6d.1h after last administration, carries out drawing coughing test as stated above, observes the cough number of times in guinea pig cough's incubation period and 3min, the results are shown in Table 3.
Table 3 to Cavia porcellus antitussive effect (
n=10)
Note: compare with matched group,
*p<0.05,
*p<0.01; Compare with existing tetrahydro-isoquinolin group
+p<0.05.
2.3 pairs of Cavia porcellus acetylcholine draw breathes heavily antiasthmatic effect
DHP Cavia porcellus 30, body weight 200-250g, be divided into 3 groups at random, often organize 10, namely of the present invention group, existing tetrahydro-isoquinolin group, dosage and administration time the same, every day gavage 1 time, continuous gavage 6 days, last administration 1 as a child, Cavia porcellus is put into airtight glass bell jar, after animal peace and quiet, start the split type nebulizer of water power, regulate certain atomization quantity, atomizing particle diameter is made to be 4 microns, spray into mass fraction be respectively 2% acetylcholine and 4% histamine equivalent mixed liquor to animal overturning, the time (asthmatic latent period) that record spraying starts to move thing overturning organize between statistical procedures, the results are shown in Table 4.
Table 4 on Cavia porcellus acetylcholine draw breathe heavily impact (
n=10)
Note: compare with matched group,
*p<0.05,
*p<0.01; Compare with existing tetrahydro-isoquinolin group
+p<0.05.
Conclusion, tetrahydro-isoquinolin of the present invention and existing tetrahydro-isoquinolin all have analgesia, cough-relieving, the effect of relievining asthma, and guinea pig cough is obviously extended incubation period, and number of times of coughing reduces.And having of tetrahydro-isoquinolin of the present invention is better than existing tetrahydro-isoquinolin.
Detailed description of the invention:
Embodiment 1:
Formula: Radix Platycodonis 200g, Gypsum Fibrosum 200g, Pericarpium Papaveris 200g, Radix Glycyrrhizae 400g, Herba Ephedrae 400g, Radix Stemonae 200g and Semen Armeniacae Amarum 400g and adjuvant.
Technique: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaims ethanol, obtains alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, and add Platycodon Root, gypsum powder, and the dextrine powder mixing of the amount of making 10-20%, with alcohol granulation, dry, obtain tablet.
Usage and dosage: oral, a 2-4 sheet, 2 times on the one.
Specification: 0.6g/ sheet.
Embodiment 2:
Formula: Radix Platycodonis 200g, Gypsum Fibrosum 200g, Pericarpium Papaveris 200g, Radix Glycyrrhizae 400g, Herba Ephedrae 400g, Radix Stemonae 200g and Semen Armeniacae Amarum 400g and adjuvant.
Technique: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaims ethanol, obtains alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, add Radix Platycodonis, gypsum powder, the dextrine powder of the amount of making 10-20% and the cane sugar powder mixing of the amount of making 10-20%, with alcohol granulation, obtain granule.
Usage and dosage: oral, a 5-10g, 2 times on the one.
Specification: 10g/ bag.
Embodiment 3:
Formula: Radix Platycodonis 200g, Gypsum Fibrosum 200g, Pericarpium Papaveris 200g, Radix Glycyrrhizae 400g, Herba Ephedrae 400g, Radix Stemonae 200g and Semen Armeniacae Amarum 400g and adjuvant.
Technique: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaims ethanol, obtains alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, and add the starch mixing of Platycodon Root, gypsum powder, 10-20%, granulate, incapsulate, obtain capsule.
Usage and dosage: oral, a 2-4 grain, 2 times on the one.
Specification: 0.6g/ grain.
Claims (10)
1. the manufacture method of a tetrahydro-isoquinolin preparation, it is characterized in that: described tetrahydro-isoquinolin preparation calculates by weight, make primarily of Radix Platycodonis 10-30 part, Gypsum Fibrosum 10-30 part, Pericarpium Papaveris 10-30 part, Radix Glycyrrhizae 30-50 part, Herba Ephedrae 30-50 part, Radix Stemonae 10-30 part and Semen Armeniacae Amarum 30-50 part; The manufacture method of described tetrahydro-isoquinolin preparation is: get Herba Ephedrae, adds alcoholic solution reflux, extract, 2-4 time of 70%-90%, filters, merging filtrate, reclaims ethanol, obtains alcohol extract, for subsequent use; Filtering residue adds water extraction 2-3 time again, and filter, merging filtrate, after being condensed into concentrated solution, merging with above-mentioned alcohol extract, be condensed into extractum, obtain Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, decoct with water, filter, filtrate reduced in volume, to clear paste, adds ethanol and makes alcohol content reach 55%-85%, stir, leave standstill 12-48 hour, filter, decompression filtrate recycling ethanol is also condensed into extractum, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, add Platycodon Root, gypsum powder and adjuvant, mixing, makes pharmaceutical preparation.
2. the manufacture method of tetrahydro-isoquinolin preparation as claimed in claim 1, it is characterized in that: described tetrahydro-isoquinolin preparation calculates by weight, make primarily of Radix Platycodonis 20 parts, 20 parts, Gypsum Fibrosum, Pericarpium Papaveris 20 parts, 40 parts, Radix Glycyrrhizae, 40 parts, Herba Ephedrae, the Radix Stemonae 20 parts and Semen Armeniacae Amarum 40 parts.
3. the manufacture method of tetrahydro-isoquinolin preparation as claimed in claim 1, it is characterized in that: the manufacture method of described tetrahydro-isoquinolin preparation is: get Herba Ephedrae, add alcoholic solution reflux, extract, 2-4 time of 8-12 times amount 70%-90%, each 2-3h, filter, merging filtrate, reclaim ethanol, obtain alcohol extract, for subsequent use; Filtering residue adds 6-10 times amount water extraction 2-3 time again, each 1-3 hour, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and being concentrated into relative density at 50-60 DEG C is the extractum of 1.1-1.2, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 7-12 times of soak by water 2-4 time, each 0.5-3 hour, filter, merging filtrate, concentrating under reduced pressure becomes clear paste, adding ethanol makes alcohol content reach 55%-85%, stirs, and leaves standstill 12-48 hour, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, add Platycodon Root, gypsum powder and adjuvant, mixing, makes pharmaceutical preparation.
4. the manufacture method of tetrahydro-isoquinolin preparation as claimed in claim 1, is characterized in that: the manufacture method of described tetrahydro-isoquinolin preparation is: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaim ethanol, obtain alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, add Platycodon Root, gypsum powder and adjuvant, mixing, makes pharmaceutical preparation.
5. the manufacture method of the tetrahydro-isoquinolin preparation according to any one of claim 1-4, is characterized in that: described pharmaceutical preparation is oral formulations.
6. the manufacture method of tetrahydro-isoquinolin preparation as claimed in claim 5, is characterized in that: described oral formulations is tablet, granule, capsule or pill.
7. the manufacture method of tetrahydro-isoquinolin preparation as claimed in claim 6, is characterized in that: described tablet makes like this: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaim ethanol, obtain alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, add Platycodon Root, gypsum powder, and the dextrine powder mixing of the amount of making 10-20%, with alcohol granulation, dry, tabletting, to obtain final product.
8. the manufacture method of tetrahydro-isoquinolin preparation as claimed in claim 6, is characterized in that: described granule makes like this: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaim ethanol, obtain alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, add Radix Platycodonis, gypsum powder, the dextrine powder of the amount of making 10-20% and the cane sugar powder mixing of the amount of making 10-20%, with alcohol granulation, to obtain final product.
9. the manufacture method of tetrahydro-isoquinolin preparation as claimed in claim 6, is characterized in that: described capsule makes like this: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaim ethanol, obtain alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, obtains Herba Ephedrae extractum, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into condensed cream; The Radix Stemonae 60% alcohol heating reflux extracts, secondary is extracted with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream, Herba Ephedrae extractum merge, and add the starch mixing of Platycodon Root, gypsum powder, 10-20%, granulate, incapsulate, to obtain final product.
10. the manufacture method of tetrahydro-isoquinolin preparation as claimed in claim 6, is characterized in that: described pill makes like this: get Herba Ephedrae, adds the alcoholic solution reflux, extract, 3 times of 10 times amount 80%, each 2h, filters, merging filtrate, reclaim ethanol, obtain alcohol extract, for subsequent use; Filtering residue adds 8 times amount water extraction 2 times again, each 2 hours, and filter, merging filtrate, after being condensed into concentrated solution, merges with above-mentioned alcohol extract, and when being concentrated into 50-60 DEG C, relative density is the extractum of 1.10-1.20, dry, pulverize, obtains Herba Ephedrae extract, for subsequent use; Get Radix Platycodonis to pulverize, add 10 times of soak by water 3 times, each 2 hours, filter, merging filtrate, when being evaporated to 50 DEG C, relative density is the extractum of 1.05-1.10, adding ethanol makes alcohol content reach 65%, stirs, and leaves standstill 24 hours, filter, decompression filtrate recycling ethanol to be concentrated into relative density when relative density is 50 DEG C be the extractum of 1.15-1.20, dry, pulverize powdered, obtain Platycodon Root, for subsequent use; Get Gypsum Fibrosum powder and be broken into fine powder, obtain gypsum powder; Get Pericarpium Papaveris again and Radix Glycyrrhizae decocts with water secondary, each 3 hours, merge decoction liquor, filter, filtrate is condensed into cream, for subsequent use; The Radix Stemonae 60% alcohol heating reflux extracts, extract secondary with the alcohol heating reflux of more than 85% after Semen Armeniacae Amarum deoils, merge above ethanol extract, reclaim ethanol and be condensed into extractum, extractum and above-mentioned condensed cream merge, dry, pulverize into powder, then mix with above-mentioned Herba Ephedrae extract, Platycodon Root and gypsum powder, add the refined honey of medicated powder amount 25%-40%, water-honeyed pill is made by suitable quantity of water, dry, to obtain final product.
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| CN114699973A (en) * | 2022-05-06 | 2022-07-05 | 山东德聚仁合生物工程有限公司 | Preparation method of improved animal cough and asthma mixture |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114699973A (en) * | 2022-05-06 | 2022-07-05 | 山东德聚仁合生物工程有限公司 | Preparation method of improved animal cough and asthma mixture |
| CN114699973B (en) * | 2022-05-06 | 2024-03-08 | 山东德聚仁合生物工程有限公司 | Preparation method of improved animal cough and asthma mixture |
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