CN105395956A - Traditional Chinese medicine composition for treating anemopyretic cold and preparing method and quality control method thereof - Google Patents
Traditional Chinese medicine composition for treating anemopyretic cold and preparing method and quality control method thereof Download PDFInfo
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Abstract
The invention provides a traditional Chinese medicine composition for treating anemopyretic cold and a preparing method and quality control method thereof. The traditional Chinese medicine composition is prepared from honeysuckle, fructus forsythia, saposhnicovia divaricata, platycodon grandiflorum, scutellaria baicalensis, rhizoma phragmitis and liquorice. The traditional Chinese medicine composition can clear away heat, relieve exterior syndrome, relieve sore-throat and diminish swelling, and can be used for treating flu or fever, headache, swollen sore throat and other symptoms clinically.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof, particularly a kind of Chinese medicine composition, its preparation method and method of quality control thereof for the treatment of anemopyretic cold.
Background technology
Caused by anemopyretic cold is the evil criminal table of wind heat, lung qi is become estranged.Symptoms is heating weight, micro evil wind, distending pain in the head, have antiperspirant, red swelling and pain of throat, cough, expectorant are sticky or yellow, yellow thick nasal discharge of having a stuffy nose, thirst and liking drink, the tip of the tongue limit are red, the micro-Huang of white and thin fur.The traditional Chinese medical science is thought, caused by anemopyretic cold is the evil criminal table of wind heat, lung qi is become estranged.Method for the treatment of should based on relieving the exterior syndrome with drugs of pungent in flavor and cool in nature.Often select Flos Chrysanthemi, Herba Menthae, Folium Mori etc.Represent prescription for " Lonicerae and Forsythiae Powder ", " SANGJU YIN ".
Summary of the invention
The object of the present invention is to provide a kind of Chinese medicine composition for the treatment of anemopyretic cold and preparation method thereof.The crude drug of described Chinese medicine composition is by Flos Lonicerae, and Fructus Forsythiae, Radix Saposhnikoviae, Radix Platycodonis, the seven flavor medicine material such as Radix Scutellariae, Rhizoma Phragmitis, Radix Glycyrrhizae forms, and has heat clearing away, induces sweat, effect of relieving sore throat and diminishing swelling, be used for the treatment of cold, fever clinically, headache, the diseases such as laryngopharynx swelling and pain.In side, Flos Lonicerae, Fructus Forsythiae are monarch drug; have heat-clearing and toxic substances removing, effect of wind-heat dissipating, Radix Saposhnikoviae can help the heresy of Flos Lonicerae, Fructus Forsythiae expelling pathogenic factors from muscles table; to dispel the wind again diaphoresis pain relieving; Radix Platycodonis lung qi dispersing eliminates the phlegm, clearing throat, Radix Scutellariae pathogenic fire purging cold in nature, clearing interior heat, and Rhizoma Phragmitis does cool clear profit, promoting the production of body fluid to quench thirst; Radix Glycyrrhizae both can coordinating the actions of various ingredients in a prescription; protect stomach regulating the spleen and stomach, also have relieving cough and expelling phlegm anti-inflammatory efficacy simultaneously, throat and the tunica mucosa tracheae of inflammation can be protected.All medicines share, and play dispelling wind and heat pathogens altogether, clearing away lung-heat to relieve cough, effect that antiinflammatory profit is swollen.
The crude drug that the present invention treats the Chinese medicine composition of anemopyretic cold consists of: Flos Lonicerae 320-360 weight portion, Fructus Forsythiae 320-360 weight portion, Radix Saposhnikoviae 320-360 weight portion, Radix Platycodonis 320-360 weight portion, Radix Scutellariae 220-270 weight portion, Rhizoma Phragmitis 180-220 weight portion, Radix Glycyrrhizae 160-180 weight portion.
The preferred Chinese medicine composition of the present invention, is characterized in that it is made up of following raw material medicaments: Flos Lonicerae 345 weight portion, Fructus Forsythiae 345 weight portion, Radix Saposhnikoviae 345 weight portion, Radix Platycodonis 345 weight portion, Radix Scutellariae 250 weight portion, Rhizoma Phragmitis 200 weight portion, Radix Glycyrrhizae 170 weight portion.
The Chinese medicine composition for the treatment of anemopyretic cold of the present invention can add various customary adjuvant required when preparing different dosage forms, such as disintegrating agent, lubricant, filler etc. are prepared into multiple conventional oral formulations with the method for Chinese medicinal of routine, such as pill, capsule, tablet, granule or oral liquid etc., preferred particulates agent.
The preparation technology of the Chinese medicine composition for the treatment of anemopyretic cold of the present invention, comprises the steps: by recipe quantity, the seven flavor medicine materials such as extracting honeysuckle, decoct with water twice, collecting decoction, filter, filter vacuum concentrating under reduced pressure, add ethanol, stir evenly, leave standstill, filter, filtrate recycling ethanol, vacuum-concentrcted is extractum, adds different auxiliary material make preparation according to the process requirements making different dosage form.Method for optimizing comprises the steps: by recipe quantity, the seven flavor medicine materials such as extracting honeysuckle, decoct with water twice, add water 12 times amount for the first time, decocts 3 hours, and add water 9 times amount for the second time, decoct 2 hours, collecting decoction, filter, filter vacuum is evaporated to about 1000ml, relative density about 1.15 ~ 1.25 (60 DEG C), be incorporated as the ethanol of concentrated solution 1.5 times of volumes, stir evenly, leave standstill 12 hours, filter, filtrate recycling ethanol, vacuum-concentrcted is extractum, adds different auxiliary material make preparation according to the process requirements making different dosage form.
The preferred marumerization of moulding process of Chinese medicinal composition granules preparation of the present invention, the method is the result of spray technique and fluid bed integrated use, traditional mixing, granulation, drying are once completed in same closed container, realize one-step method to granulate, material powder sets up fluidization in bed, simultaneously by binding agent droplet to fluidisation interface granulating, drying volatilization moisture take out of outside machine with air draft.The mixture of preferably sucrose powder and starch is as adjuvant, and starch consumption is 1% (weight), and fluid extract is given money as a gift in 70% (weight), and residue adjuvant is Icing Sugar (weight).Preferred one-step palletizing technique is: take cane sugar powder and starch according to the above ratio; put mix homogeneously in one-step-granulating method; the fluid extract relative density that the seven flavor medicine materials such as Flos Lonicerae extract is 1.20 ~ 1.30 (60 DEG C); spray into; one-step palletizing; inlet temperature 80 ~ 100 DEG C, during charging rate 30 ~ 50g/min, temperature of charge 50 ~ 70 DEG C.
The invention provides a kind of method of quality control of Chinese medicine composition of above-mentioned treatment anemopyretic cold, it is characterized in that using chromatograph of liquid to detect Chinese medicine composition Content of Chlorogenic Acid of the present invention, wherein chromatographic column filler is octadecyl silane, take acetonitrile as mobile phase A, with 0.4% phosphoric acid solution for Mobile phase B, carry out gradient elution, determined wavelength is 327nm, sampling volume 10 μ l, the preparation method detecting sample is: get testing sample 1.0g, porphyrize, accurately weighed, put 50ml measuring bottle, add 50% methanol and be about 40ml, airtight, supersound process 30 minutes, let cool, by 50% methanol constant volume to scale, shake up, filter and get final product.Chinese medicinal granule every gram of the present invention must not be less than 1.2mg containing Flos Lonicerae in chlorogenic acid (C16H18O9).
The Chinese medicine composition of the present invention to obtained treatment anemopyretic cold has carried out clinical efficacy and safety testing thereof.Method adopts Method of Random Test, observes the clinical efficacy that compositions of the present invention treats 160 routine anemopyretic cold patients.After treatment in 3 days, result is treatment group clinical recovery rate is 33%, and obvious effective rate is 12%, and effective percentage is 34%.The above results shows that compositions of the present invention has obvious curative effects for treatment anemopyretic cold.Safety testing does not find untoward reaction.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, can better understand the present invention and can be implemented, but illustrated embodiment is not as a limitation of the invention to make those skilled in the art.
The preparation of embodiment 1 extractum
Extracting honeysuckle 345g, Fructus Forsythiae 345g, Radix Saposhnikoviae 345g, Radix Platycodonis 345g, Radix Scutellariae 250g, Rhizoma Phragmitis 200g, Radix Glycyrrhizae 170g, decocts with water twice, and add water 12 times amount for the first time, decoct 3 hours, add water 9 times amount for the second time, decocts 2 hours, collecting decoction, filter, filter vacuum is evaporated to about 1000ml, and relative density about 1.15 ~ 1.25 (60 DEG C), is incorporated as the ethanol of concentrated solution 1.5 times of volumes, stir evenly, leave standstill 12 hours, filter, filtrate recycling ethanol, vacuum-concentrcted is extractum, measures chlorogenic acid content.
The preparation of embodiment 2 Chinese medicinal composition granules
Extracting honeysuckle 345g, Fructus Forsythiae 345g, Radix Saposhnikoviae 345g, Radix Platycodonis 345g, Radix Scutellariae 250g, Rhizoma Phragmitis 200g, Radix Glycyrrhizae 170g, decoct with water secondary, add water 12 times amount for the first time, decoct 3 hours, add water 9 times amount for the second time, decoct 2 hours, collecting decoction, filter, filtrate 80 DEG C is evaporated to about 1000ml, relative density about 1.15 ~ 1.25 (60 DEG C), be incorporated as the ethanol of concentrated solution 1.5 times of volumes, stir evenly, leave standstill 12 hours, filter, filtrate recycling ethanol, be evaporated to the fluid extract of relative density 1.20 ~ 1.30 (60 DEG C), slightly cold, get Icing Sugar and starch mixes in right amount, spray into fluid extract, one-step palletizing, 1000g is made in drying, obtain.
The confirmation of supplementary product consumption
According to drafting extraction process, preparing extractum with recipe quantity, take sucrose as major auxiliary burden, and adopt the consumption of single factor test screening starch, and grope preparation process, screen, one-step palletizing all makes 1000g.Dry cream rate according to each batch experiment gained extractum calculates adjuvant inventory, confirms supplementary product consumption by pelletizing forming situation and granule melting.
Six batches of test gained granular mass evaluation results are as follows:
Comprehensive above evaluation index, select preparations shaping starch consumption to be 1%, fluid extract is given money as a gift in 70%, and residue adjuvant is Icing Sugar, and one-step palletizing is more satisfactory.
The determination of fluid extract relative density
Cane sugar powder and starch is taken by recipe quantity; put mix homogeneously in one-step-granulating method; get the fluid extract that relative density is respectively 1.20,1.25,1.30, carry out one-step palletizing, in pelletization; regulate air quantity at any time; material is made to be fluidized state, charging rate 40g/min, inlet temperature 80 ~ 90 DEG C; temperature of charge 50 ~ 60 DEG C, observes granulating efficiency.
As seen from the above table, the fluid extract one-step palletizing of relative density 1.20 ~ 1.30 (60 DEG C) is comparatively smooth, and the granule of gained size of loosening is even.
The determination of charging rate
Cane sugar powder and starch is taken by recipe quantity; put mix homogeneously in one-step-granulating method; get the fluid extract that relative density is 1.24 (60 DEG C); carry out one-step palletizing, in pelletization, regulate air quantity at any time; material is made to be fluidized state; inlet temperature 80 ~ 90 DEG C, respectively charging rate be 30,40,50,60g/min granulates, and observes granulating efficiency.
As seen from the above table, time charging rate very fast (60g/min), humidity of materials is comparatively large, as drying easily causes particle from caking not in time, produces bulky grain.Charging rate controls when 30 ~ 50g/min, and shaping particles is better.
Granulating process lab scale checking research
Adopt one-step palletizing technique, with the technological parameter determined, manufacture experimently 5 batches of lab scales, often criticize grain amount 2000g, calculate the addition of cane sugar powder and starch according to grain amount and dry cream rate.
After measured, granule Content of Chlorogenic Acid total amount and medicinal material extract gained extractum Content of Chlorogenic Acid total amount are more or less the same, and illustrate that moulding process is substantially lossless.
The quality control of embodiment 3 Chinese medicine composition
Instrument high performance liquid chromatograph Shimadzu LabSolutionsEssentia work station, LC-16 type high pressure pump, SPD-16 type UV-detector, CBM-16 controller; (Shimadzu Corporation).
Reagent and reagent
Chlorogenic acid reference substance: provided by National Institute for Food and Drugs Control.
Negative control sample: self-control (not containing Flos Lonicerae)
Test sample: the Chinese medicinal composition granules of embodiment 2
Test sample treatment is: get this product under content uniformity item, porphyrize, get about 1.0g, accurately weighed, put 50ml measuring bottle, add 50% methanol and be about 40ml, airtight, supersound process (power 150W, frequency 40kHz) 30 minutes, lets cool, by 50% methanol constant volume to scale, shake up, filter, to obtain final product.
Methanol, acetonitrile are chromatographically pure, and phosphoric acid is AG, and water is dual distilled water.
Chromatographic condition octadecylsilane chemically bonded silica is filler; Take acetonitrile as mobile phase A, with 0.4% phosphoric acid solution for Mobile phase B, the regulation according to the form below carries out gradient elution; Determined wavelength is 327nm, sampling volume 10 μ l.Theoretical cam curve calculates should be not less than 2000 by chlorogenic acid peak.
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0～15 | 10→12 | 90→88 |
| 15～30 | 12→30 | 88→70 |
| 30～35 | 30 | 70 |
| 35～36 | 30→10 | 70→90 |
| 36～42 | 10 | 90 |
The selection of mobile phase is with reference to " Chinese Pharmacopoeia " 2010 editions Flos Lonicerae content assaying methods, with acetonitrile-0.4% phosphoric acid solution (13:87) for mobile phase, determined wavelength is 327nm, sampling volume 10 μ l, sample introduction measures, chlorogenic acid peak shape is better, but lab scale conceptual phase, strong reservation peak is often had to go out peak in sample analysis more late, disturb next sample needle eluting, complete elution analysis overlong time, analytic product quality fast and effectively when being unfavorable for actual production, effectively be separated within a certain period of time for making each composition in sample, we adopt gradient elution, mobile phase ratio is through repeatedly adjusting, determine to analyze with above-mentioned Gradient program, main peak and adjacent chromatographic peak separating degree better, all can be separated completely according to other similar features peaks in document and within 40 minutes basic eluting complete, chlorogenic acid retention time about about 20 minutes, theoretical cam curve 20656 is much larger than 2000, separating degree 18.098 is greater than 1.5, tailing factor 1.049, and the method specificity is better negative noiseless, therefore select above gradient elution program to carry out sample size analysis.
System suitability is with the above-mentioned separation condition determined, get reference substance solution continuous sample introduction 6 pin, need testing solution enters 2 pins, and sampling volume 10 μ l, carries out system suitability.The results are shown in following table:
Illustrate that the gradient elution method system suitability determined is good by above-mentioned data, meet statutory regulations.
System precision
Get same uniform sample solution or chlorogenic acid reference substance solution appropriate, accurately draw 10 μ l, repeat sample introduction 6 times, record chromatogram, calculates average peak area and RSD value.Result RSD < 2%, proves that this law system precision is good.Refer to table 6 data.
Repeatability
The same batch sample of Example 26 parts, measure by content assaying method, result RSD < 2%, illustrates that the repeatability of this method is good.Result is as follows:
Intermediate precision
Measure by content assaying method, get same batch sample, different instrument, different analyst measure, the precision between result of calculation.
Result of the test shows: the coefficient of variation RSD=1.50% of sample size measured by different instrument, different analyst, different intervals, shows that the Intermediate precision of this method is good.
Accuracy
The accuracy reflecting method is tested by average recovery.Get the compositions 0.5g of the embodiment 2 of known content, 9 parts, precision add chlorogenic acid reference substance solution respectively compound concentration be each 3 parts of the solution of 80%, 100%, 120%, measure its content respectively, measured value is compared with theoretical value, calculates the response rate of chlorogenic acid.
Accuracy test result
The range of linearity
Precision measure chlorogenic acid reference substance mother solution 1. (concentration is 0.4288mg/ml) 2.8,2.5,2.0ml, put respectively in the brown volumetric flask of 10ml, add 50% dissolve with methanol and be diluted to scale, as concentration 1, concentration 2, concentration 3; Precision measure chlorogenic acid reference substance mother solution 2. (concentration is 0.352mg/ml) 1.9,0.5,0.5ml, put in the brown volumetric flask of 10ml, 10ml, 25ml respectively, add 50% dissolve with methanol and be diluted to scale, as concentration 4, concentration 5, concentration 6, draw each 10 μ l of above-mentioned 6 kinds of concentrations control product solution (or 5 μ l, 2 μ l) respectively, injection liquid chromatography, each concentration sample introduction 2 times, calculates average peak area.With peak area (A) for vertical coordinate (Y), with its sample size (μ g) for abscissa (X), carry out linear regression by method of least square, obtain canonical plotting.
Linear and scope result of the test
Sample solution stability test
Example 2 compositions, porphyrize, takes 1.0g, accurately weighed, put in tool plug conical flask, precision adds 50% methanol 50ml, weighed weight, supersound process (power 150w, frequency 40kHz) 30 minutes, let cool, more weighed weight, the weight of less loss is supplied with 50% methanol, shake up, filter, get subsequent filtrate, obtained need testing solution, sample introduction 10 μ l.Measure at different time points sample introduction, determine whether need testing solution is stablized within a period of time with the RSD of measurement result.The results are shown in following table.
Solution stability testing
Result of the test shows: need testing solution is good at 24 hours internal stabilities.
Serviceability test
For investigating the ruggedness of the method, adjust typical variable in liquid chromatography respectively: different brands chromatographic column, column temperature ± 5 DEG C, flow velocity ± 20% and Mobile phase B mutually in phosphoric acid concentration 0.4% ± 0.2%, assay is carried out, with the RSD of each size of experiment measurement result for inspection target is investigated it with same batch sample.Result is as follows:
Calculate RSD%≤2.0% of content results, main peak tailing factor is not more than 2.0, and separating degree is greater than 1.5.
Serviceability test data
Serviceability test result
Above result shows, when each typical variable of the method has a little variation, less to this product assay Influence on test result, therefore the ruggedness of this method is better.
The above embodiment is only that protection scope of the present invention is not limited thereto in order to absolutely prove the preferred embodiment that the present invention lifts.The equivalent alternative or conversion that those skilled in the art do on basis of the present invention, all within protection scope of the present invention.Protection scope of the present invention is as the criterion with claims.
Claims (7)
1. treat the Chinese medicine composition of anemopyretic cold for one kind, it is characterized in that, it is made up of following raw material medicaments: Flos Lonicerae 320-360 weight portion, Fructus Forsythiae 320-360 weight portion, Radix Saposhnikoviae 320-360 weight portion, Radix Platycodonis 320-360 weight portion, Radix Scutellariae 220-270 weight portion, Rhizoma Phragmitis 180-220 weight portion, Radix Glycyrrhizae 160-180 weight portion.
2. Chinese medicine composition according to claim 1, is characterized in that it is made up of following raw material medicaments: Flos Lonicerae 345 weight portion, Fructus Forsythiae 345 weight portion, Radix Saposhnikoviae 345 weight portion, Radix Platycodonis 345 weight portion, Radix Scutellariae 250 weight portion, Rhizoma Phragmitis 200 weight portion, Radix Glycyrrhizae 170 weight portion.
3. the Chinese medicine composition that one of claim 1-2 is described, is characterized in that described compositions is pill, capsule, tablet, granule or oral liquid.
4. Chinese medicine composition according to claim 3, is characterized in that described compositions is granule.
5. the preparation method of the Chinese medicine composition of the described anemopyretic cold of one of claim 1-2, comprises the steps: by recipe quantity extracting honeysuckle, Fructus Forsythiae, Radix Saposhnikoviae, Radix Platycodonis, Radix Scutellariae, Rhizoma Phragmitis and Radix Glycyrrhizae seven flavor medicine material, decoct with water twice, collecting decoction, filter, filter vacuum concentrating under reduced pressure, adds ethanol, stir evenly, leave standstill, filter, filtrate recycling ethanol, vacuum-concentrcted is extractum, adds different auxiliary material make preparation according to the process requirements making different dosage form.
6. the preparation method of Chinese medicine composition described in claim 4, comprise the steps: by recipe quantity extracting honeysuckle, Fructus Forsythiae, Radix Saposhnikoviae, Radix Platycodonis, Radix Scutellariae, Rhizoma Phragmitis and Radix Glycyrrhizae seven flavor medicine material, decoct with water twice, collecting decoction, filter, filter vacuum concentrating under reduced pressure, add ethanol, stir evenly, leave standstill, filter, filtrate recycling ethanol, vacuum-concentrcted is extractum, then be 1% (weight) according to starch consumption, fluid extract is given money as a gift in 70% (weight), residue adjuvant is that the ratio of Icing Sugar takes cane sugar powder and starch, put mix homogeneously in one-step-granulating method, the fluid extract relative density that the seven flavor medicine materials such as Flos Lonicerae extract is 1.20 ~ 1.30 (60 DEG C), spray into, one-step palletizing, inlet temperature 80 ~ 100 DEG C, charging rate 30 ~ 50g/min, temperature of charge 50 ~ 70 DEG C.
7. the method for quality control of the Chinese medicine composition that one of claim 1-2 is described, it is characterized in that using the Chinese medicine composition Content of Chlorogenic Acid of chromatograph of liquid to one of claim 1-2 to detect, wherein chromatographic column filler is octadecyl silane, take acetonitrile as mobile phase A, with 0.4% phosphoric acid solution for Mobile phase B, carry out gradient elution, determined wavelength is 327nm, sampling volume 10 μ l, the preparation method detecting sample is: get testing sample 1.0g, porphyrize, accurately weighed, put 50ml measuring bottle, add 50% methanol and be about 40ml, airtight, supersound process 30 minutes, let cool, by 50% methanol constant volume to scale, shake up, filter and get final product.
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| CN115252683A (en) * | 2022-08-15 | 2022-11-01 | 红云制药(玉溪)有限公司 | Method for preparing children cough and asthma granule by adopting one-step granulation |
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| CN103705633A (en) * | 2013-12-19 | 2014-04-09 | 任继勇 | Traditional Chinese medicine pill for treating anemopyretic cold |
| CN103860697A (en) * | 2014-03-20 | 2014-06-18 | 中国中医科学院广安门医院 | Chinese medicine composition for treating exogenous febrile diseases and application thereof |
| CN104415240A (en) * | 2013-08-20 | 2015-03-18 | 李霞 | Medicine liquid for treating wind-heat cold |
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| CN104415240A (en) * | 2013-08-20 | 2015-03-18 | 李霞 | Medicine liquid for treating wind-heat cold |
| CN103705633A (en) * | 2013-12-19 | 2014-04-09 | 任继勇 | Traditional Chinese medicine pill for treating anemopyretic cold |
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| CN115252683A (en) * | 2022-08-15 | 2022-11-01 | 红云制药(玉溪)有限公司 | Method for preparing children cough and asthma granule by adopting one-step granulation |
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