CN102961463A - Process for preparing Ganqing granules - Google Patents
Process for preparing Ganqing granules Download PDFInfo
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- CN102961463A CN102961463A CN201210453920XA CN201210453920A CN102961463A CN 102961463 A CN102961463 A CN 102961463A CN 201210453920X A CN201210453920X A CN 201210453920XA CN 201210453920 A CN201210453920 A CN 201210453920A CN 102961463 A CN102961463 A CN 102961463A
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Abstract
The invention discloses a process for preparing Ganqing granules. The process comprises the following steps of: extracting, concentrating and drying 65 parts by weight of aleppo avens, 60 parts by weight of wintersweet roots, 50 parts by weight of cotton rose hibiscus leaves, 50 parts by weight of purple perilla, 50 parts by weight of fewflower lysionotus herbs, 75 parts by weight of herba kalimeridis and 50 parts of schizonepeta to obtain an extractant; and preparing the granules by adding auxiliaries. According to the process, preparation of the raw materials, decoction time, decoction times, decoction water adding amount and selection of filtering cloth in the extraction process, selection of concentration modes and concentration temperature in a concentration process, drying modes and temperatures in a drying process, and ingredient preparation, selection and proportion of wetting agents, granulation method and whole-granule production method in the preparation process are obtained based on a large quantity of experiments by inventors. The process is simple in procedures, obvious in preparation effect and low in cost, facilitates popularization and use; and multiple middle ingredients are not needed during production and a large amount of time and a large quantity of energy sources are not needed to spend.
Description
Technical field
The present invention relates to a kind of preparation technology who is used for the treatment of the Ganqing Granules of flu, belong to the field of Chinese medicines.
Background technology
Ganqing preparation has relieving the exterior syndrome with drugs of pungent in flavor and warm in nature, and the effect of lung qi dispersing cough-relieving is used for the diseases such as headache that anemofrigid cold causes, fear of cold, heating, watery nasal discharge, cough.Existing Ganqing preparation generally is syrup, but syrup needs to cause consumption not accurate enough with soupspoon when taking, and can affect the treatment; Syrup contains sugar and causes the diabetes patient not use; And syrup carries inconvenience, and cost of warehousing transportation is higher.Granule can well address the above problem.Existing patent ZL02134089.7 medicine for the treatment of flu " in relate to the intermediate products (being extract) of Ganqing preparation preparation method be: above-mentioned seven flavor medicine material (Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass and Herba Schizonepetae); decoct with water 2 times; each 1 hour; filter; merging filtrate; leave standstill and made precipitation in 24 hours, get supernatant concentration to an amount of, namely make the Ganqing preparation intermediate products.But the preparation method process of this patent disclosure is complicated, needs to use multiple middle batching, and cost is higher, and needs cost plenty of time (more than 25 hours) and mass energy, is unfavorable for promoting the use of.
The object of the invention is to, a kind of preparation technology of Ganqing Granules is provided.This preparation process is simple, need not to use multiple middle batching, and cost is lower, need not to spend plenty of time and mass energy, is beneficial to and promotes the use of.
For solving the problems of the technologies described above, technical scheme provided by the invention is as follows: a kind of preparation technology of Ganqing Granules, calculate by weight and take by weighing 50 parts of 65 parts of Radix seu Herba Gei aleppici, 60 parts of Radix Chimonanthi praecocis, 50 parts of Folium Hibisci Mutabiliss, 50 parts of Folium Perillaes, 50 parts of Herba Lysionoti Paucifloris, 75 parts of Herba Kalimeridis grasss and Herba Schizonepetae, with Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass and Herba Schizonepetae all be cut into 0.3-2.0cm the section or the silk, be mixed to get a product; The a product are decocted with water 2 times, each 1 hour, add 7-8 times of water gaging for the first time, add 8-9 times of water gaging for the second time, filter with 80-200 order filter cloth, merging filtrate gets the b product; The b product are carried out vacuum-concentrcted, and thickening temperature is 75 ℃-80 ℃, is concentrated into relative density and is about 1.08-1.10, gets the c product; The c product are made powder by drying under reduced pressure, microwave drying or spray drying, get extract; In extract, add adjuvant and be prepared into granular preparation; Adjuvant is dextrine powder and/or starch; The weight proportion of extract and adjuvant is 1: 4.
The preparation technology of aforesaid Ganqing Granules, the described adjuvant that adds in extract is prepared into granular preparation and is specially, make wetting agent with ethanol after adding adjuvant, then use dry granulation, adopt again No. 2 pharmacopeia sieves and No. 4 pharmacopeia sieves to carry out granulate, the granule of getting by No. 2 pharmacopeia sieve but can not be by No. 4 pharmacopeia sieves namely makes Ganqing Granules as finished product.
The preparation technology of aforesaid Ganqing Granules prepares extract according to following step;
A. Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass, Herba Schizonepetae all are cut into section or the silk of 0.3-2.0cm, are mixed to get a product;
B. a product are decocted with water 2 times, each 1 hour, add 7-8 times of water gaging for the first time, add 8-9 times of water gaging for the second time, filter with 80-200 order filter cloth, merging filtrate gets the b product;
C. the b product are carried out vacuum-concentrcted, thickening temperature is 75 ℃-80 ℃, and being concentrated into relative density is 1.09, gets the c product;
D. with the c product take 60-150 ℃ as inlet temperature, 100-220 ℃ is outlet temperature, charging rate is 10-70mLmin
-1, carry out spray drying, collect extract powder, get extract.
Among the preparation technology of aforesaid Ganqing Granules, prepare extract according to following step;
A. Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass, Herba Schizonepetae all are cut into section or the silk of 0.3-2.0cm, are mixed to get a product;
B. a product are decocted with water 2 times, each 1 hour, add 7 times of water gagings for the first time, add 8 times of water gagings for the second time, filter with 80 order filter clothes, merging filtrate gets the b product;
C. the b product are carried out vacuum-concentrcted, thickening temperature is 75 ℃-80 ℃, and being concentrated into relative density is 1.09, gets the c product;
D. with the c product with 80 ℃ of inlet temperatures, 120 ℃ is outlet temperature, charging rate is 30-40mLmin
-1, carry out spray drying, collect extract powder, get extract
Among the preparation technology of aforesaid Ganqing Granules, described extract contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 18%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 5.6%.
The preparation technology of aforesaid Ganqing Granules, described ethanol is 75% ethanol.
Among the preparation technology of aforesaid Ganqing Granules, described Ganqing Granules contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 4%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 0.8%.
Compared with prior art, the present invention is on the prescription of original clear sense preparation, through the preparation technology of the clear sense granule that obtains on the basis of repeatedly testing, contrast, concluding and summing up.In the present invention, the decocting time in the extraction process, number of times and amount of water; Concentrated mode in the concentration technology is selected and thickening temperature; Drying mode in the drying process and temperature; And the batching proportioning in the preparation process, wetting agent selection and proportioning, method of granulating and granulate method all are the results who obtains on inventor's great many of experiments basis.Preparation process of the present invention is simple, need not to use multiple middle batching, and cost is lower, need not to spend plenty of time and mass energy, is beneficial to and promotes the use of.Utilize the present invention to produce Ganqing Granules, the material composition dissolution is good, and the prepared using degree is high; The Ganqing Granules property of medicine of utilizing the present invention to produce is stable, and therapeutic effect is better than existing preparation; And consumption is enough accurate, can use for the diabetes patient, and easy to carry, cost of warehousing transportation is lower.
The present inventor has done series of experiments, proves that preparation technology provided by the invention is effectively controlled, and the Ganqing Granules property of medicine of utilizing the present invention to produce is stable, and therapeutic effect is better than existing preparation.
Experimental example 1.
Decocting time in the extraction process, number of times, amount of water to Radix seu Herba Gei aleppici in the middle product with gallic acid (C
7H
6O
5) meter and Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter content impact.
Experimental technique:
Experiment materials: Radix seu Herba Gei aleppici 65g, Radix Chimonanthi praecocis 60g, Folium Hibisci Mutabilis 50g, Folium Perillae 50g, Herba Lysionoti Pauciflori 50g, Herba Kalimeridis grass 75g, Herba Schizonepetae 50g.Select different decocting times, number of times, amount of water, the Radix seu Herba Gei aleppici in the mensuration intermediate product is with gallic acid (C
7H
6O
5) meter and Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter content.Be specially: take amount of water, decocting time, decoction number of times as factor (seeing Table 1), get it filled by above-mentioned materials 1/2, extract by table 2, merging filtrate, be concentrated into 300-350mL, precision pipettes 50mL and places the 100mL volumetric flask, adds ethanol and is settled to scale, shake up, with 0.45 μ m filtering with microporous membrane.The factor level table sees Table 1, and the orthogonal test scheme sees Table 2.
Table 1 factor level table
Table 2 orthogonal test scheme table
Carry out assay by content assaying method under the Ganqing Granules intermediate products item, the results are shown in Table 3.
Table 3 result of the test
Orthogonal experiments is carried out intuitive analysis and variance analysis, the results are shown in Table 4,5.
Table 4 intuitive analysis result
Table 5 the results of analysis of variance
In view of quadrature analysis result in the above-mentioned table 5, consider the yield that does not have stone acid and lysionotin, intend investigating extraction scheme ten: namely get it filled by the clear prescription 1/2 of sense, add 7 times of water gagings for the first time, decocted 1 hour, with 80-100 order filter-cloth filtering, for the second time add 8 times of water gagings, decocted 1 hour, with 80-100 order filter-cloth filtering, merging filtrate is concentrated into 300-350mL.Precision pipettes 50mL and places the 100mL volumetric flask, adds ethanol and is settled to scale, shakes up, with 0.45 μ m filtering with microporous membrane.Carry out assay by content assaying method under the Ganqing Granules intermediate products item, the results are shown in Table 6.
Table 6 result of the test
Result and orthogonal test table 3 results of experiment ten are carried out variance analysis jointly, the results are shown in Table 7.
Table 7 the results of analysis of variance
As shown in Table 7, to gallic acid, P
Amount of water=0.708〉0.05, P
Decoct number of times=0.303〉0.05, P
Decocting time=0.380〉0.05, to lysionotin, P
Amount of water=0.241〉0.05, P
Decoct number of times=0.356〉0.05, P
Decocting time=0.293〉0.05, so amount of water, decoct number of times, decocting time to gallic acid, lysionotin there are no significant difference.
To sum up analyze, the extraction process of Ganqing Granules preparation method can be defined as: get it filled by the clear prescription of sense, add 7 times of water gagings for the first time, decocted 1 hour, and with 80-100 order filter-cloth filtering, added 8 times of water gagings for the second time, decocted 1 hour, with 80～100 order filter-cloth filterings, merging filtrate.
Experimental example 2.
Concentrated mode in the concentration technology and temperature to Radix seu Herba Gei aleppici in the middle product with gallic acid (C
7H
6O) meter and Herba Lysionoti Pauciflori are with lysionotin (C
18H
16O
7) meter content impact.
Experimental technique: obtain the filtrate in the experimental example 1, be placed in the RE-52A type Rotary Evaporators and concentrate, be concentrated into relative density and be about about 1.09, measure the content of its gallic acid, lysionotin, the results are shown in following table 8 to table 10.
The mensuration of table 8 relative density
Table 9 assay
Table 10 the results of analysis of variance
By the results of analysis of variance of above-mentioned table 10 as can be known, different temperatures, vacuum concentratedly have a significant difference to what feel clear intermediate products.
Respectively account for 50% ratio in gallic acid and lysionotin, in view of gallic acid and lysionotin are effective ingredient, its desired value should be the bigger the better, index degree of membership=(desired value-index minima)/(index maximum-index minima), comprehensive mark=gallic acid degree of membership * 50%+ lysionotin * 50%, by above-mentioned formula experimental result is carried out comprehensive grading, and carry out variance analysis, the results are shown in Table 11,12.
Table 11 comprehensive grading table
Table 12 comprehensive grading the results of analysis of variance
By table 12 the results of analysis of variance as can be known, different concentration technologies have significant difference to experimental result.
The different concentration technologies of table 13 compare in twos
By the concentration technology of table 13 in twos more as can be known, do not have significant difference between 80 ℃ and 75 ℃.
In sum, the concentration technology that the Ganqing Granules intermediate products merge the filtrate b product of gained is, vacuum-concentrcted, and temperature is 75 ℃-80 ℃.
Experimental example 3.
The different dry drying method, to Radix seu Herba Gei aleppici in the middle product with gallic acid (C
7H
6O) meter and Herba Lysionoti Pauciflori are with lysionotin (C
18H
16O
7) meter content impact and on the impact of middle product characters.
The screening of drying process:
1. hypobaric drying method: get Ganqing Granules intermediate products concentrated solution (about relative density 1.09), namely the c product place vacuum drying oven, the control temperature is 50-80 ℃, vacuum be-0.02～-0.08Mpa, heat make it drying after, take out, be ground into the extract powder of 80-200 mesh sieve.
2. micro-wave drying method: get Ganqing Granules intermediate products concentrated solution (about relative density 1.09), be the c product, place the material box of microwave special use, put into microwave drying oven, the control temperature is 25～50 ℃, vacuum is-0.02～-0.08Mpa, heating makes it to take out after dry, is ground into the extract powder of 80-200 mesh sieve.
3. spray drying method: get Ganqing Granules intermediate products concentrated solution (about relative density 1.09), i.e. c product, take 60-150 ℃ as inlet temperature, 100-220 ℃ is outlet temperature, charging rate is 10-0mLmin
-1, carry out spray drying, collect extract powder.
4. atmosphere pressure desiccation: get Ganqing Granules intermediate products concentrated solution (about relative density 1.09), be the c product, put in the 500mL evaporating dish, place Constant Temp. Oven, the control temperature is that 100 ℃ of heating make it dry rear the taking-up, is ground into the extract powder of 80-200 mesh sieve.
Above-mentioned four kinds of resulting extract powders of drying means are carried out character relatively, the results are shown in Table 14.
Table 14 different dry drying method gained extract powder character relatively
According to pressing content assaying method under the Ganqing Granules intermediate products item, different dry drying method gained extract powder is carried out assay, the results are shown in Table 15-16.
Table 15 different dry drying method assay result (n=3)
Table 16 different dry drying method lysionotin assay result (n=3)
Result of the test is carried out variance analysis, see the following form 17.
Table 17 different dry drying method analysis of variance table
As shown in Table 17, P
Gallic acid=0.000＜0.05, P
Lysionotin=0.000＜0.05, show that the different dry drying method all has a significant impact gallic acid and lysionotin.
In view of producing practical situation, constant pressure and dry is unavailable, therefore respectively account for 50% ratio in gallic acid and lysionotin, in view of gallic acid and lysionotin are effective ingredient, its desired value should be the bigger the better, index degree of membership=(desired value-index minima)/(index maximum-index minima), comprehensive mark=gallic acid degree of membership * 50%+ lysionotin * 50%, by above-mentioned formula experimental result is carried out comprehensive grading, and carry out variance analysis, the results are shown in Table 18-19.
Table 18 different dry drying method comprehensive grading table
Table 19 different dry drying method comprehensive grading the results of analysis of variance
By table 18-19 as can be known, drying under reduced pressure, microwave drying, three kinds of drying meanss of spray drying do not have significant difference to result of the test.But in conjunction with to these three kinds of resulting characters powders of drying means, and the consideration in large production, best, the used shortest time of spray drying gained powder appearance character adopted, so determine that spray drying is the drying means of intermediate products.
Experimental example 4.
Different auxiliary material is on the impact of end product (feeling clearly granule) character.
Carry out the screening of adjuvant, select respectively the adjuvants commonly used such as starch, dextrine powder, granulate take ethanol as wetting agent, carry out comprehensive grading take mouldability, bulk density, flowability, hygroscopicity as evaluation index, select suitable adjuvant.
Table 20 factor level table
Ethanol with variable concentrations is made wetting agent, investigates the situation of soft material processed, is standard with " that rubs is agglomerating, and that touches is namely loose ", selects best wetting agent, sees table 21 for details.
Table 21 different wetting agent soft material situation processed
Therefore, select the ethanol of 60%-85% to do wetting agent.
The extracting solution of the intermediate products of Ganqing Granules, i.e. c product, relative density is about 1.09, but mostly be water soluble ingredient, less sticky, be not suitable for using wet granulation, so granulate with dry granulation method, make adjuvant with dextrine powder and starch respectively, make wetting agent with the ethanol of 60%-85% and granulate.
For guaranteeing the finished particle size evenly, thus adopt No. 2 pharmacopeia sieves and No. 4 pharmacopeia sieve granulate, get by No. 2 pharmacopeia sieves but the granule that can not sieve by No. 4 pharmacopeia as finished product.
Experimental example 5.
Measure mouldability, bulk density, angle of repose, melting and the hygroscopicity of granule.And take mouldability, bulk density, angle of repose, melting and hygroscopicity as index comprehensive evaluation, preferred best adjuvant.
Aggregative indicator=(15/ maximum mouldability value) * mouldability value+(15/ maximum bulk density value) * bulk density value+(minimum angle of repose value * 15)/angle of repose value+(20/ maximum melting value) * melting value+(minimum hydroscopicity value * 35)/hydroscopicity value
The mensuration of ratio of briquetting:
The granule for preparing is weighed, cross first the pharmacopeia sieve No. one, after No. five pharmacopeia sieves, collection can be sieved by a pharmacopeia but can not by the granule of No. five pharmacopeia sieves, be weighed.
Ratio of briquetting=rear the granular mass that sieves/front quality * 100% sieves
The mouldability score value calculates using formula: (15/ maximum mouldability value) * mouldability value
Table 22 ratio of briquetting is measured
The mensuration of bulk density:
Bulk density claims again apparent density or bulk density, means the quality of unit volume granule.The used volume of bulk density refers to that the space is at interior cumulative volume between granule and itself space and granule and the granule.It is little that the bulk density of granule is greatly namely piled volume, can represent closely degree and determine what of volume integral dosage of granule.
Granule after experimental procedure will be sieved is put into dry graduated cylinder, and the volume number (V) at its nearly scale place is read in vibration gently; As M (g), both ratio is bulk density with the quality after sieving.Bulk density=M/V
The bulk density score value calculates using formula: (15/ maximum bulk density value) * bulk density value
Table 23 bulk density is measured
The mobile investigation:
Flowability is one of critical nature of granule, and mobile quality is relevant with the accuracy of the quality of granule, divided dose, commonly uses flow velocity on the pharmaceutics and represents angle of repose.Angle of repose is less, and flowability better.
Experimental procedure adopts the fixed funnel method, 3 funnels are connected up and down and be fixed in the At The Height of 1cm on the graph paper of horizontal positioned, pour into granule in the funnel of going up most along hopper walls carefully, until the tip of the cone that forms on the graph paper touches the end opening of funnel, measure the diameter (2r) of conical base by graph paper, calculate tg α=H/r angle of repose.Do calculating mean value 5 times.
Angle of repose, score value calculated using formula: (be worth * 15 minimum angle of repose)/be worth angle of repose
Table 24 is measured angle of repose
The mensuration of melting:
Get test sample 1g, heating water 200mL stirred 5 minutes, observed immediately and should all melt or be the suspendible shape, and sol particle should all be dissolved, and has allowed slight precipitation.Character after dissolving with it is divided into third gear with it: be designated as 100 minutes without breeze, slightly breeze is designated as 90 minutes, has breeze to be designated as 80 minutes.
Dissolve the rate score value and calculate using formula: (20/ maximum melting value) * melting value
The test of table 25 melting
Hygroscopicity is investigated:
Adopt the wettability test method, determine extractum add relevant diluent after its resistance to water soak whether meet technological requirement, screening experiment: get granule 1g, accurately weighed, put in the flat weighing bottle of own constant weight, accurately weighed, 25 ℃ of temperature, constant incubator under (bottom is placed with in the glass exsiccator of NaCl saturated solution and regularly puts into NaCl until form the NaCl supersaturated solution) condition that relative humidity is 75% is preserved, respectively at 2,4,6,8,10,12,24,36,48,72,96,108,120,144,168,192,214,226,240h measures its hygroscopic capacity, calculates the moisture absorption percentage rate with following formula.Moisture absorption percentage rate during with 48h calculates the hydroscopicity score value.The results are shown in Table 26.
Granule heavy * 100% before moisture absorption percentage rate=(the front granule of granule weight-moisture absorption is heavy after the moisture absorption)/moisture absorption.The hydroscopicity score value calculates using formula: (minimum hydroscopicity value * 35)/hydroscopicity value.
The mensuration of table 26 hydroscopicity score value
By the above results as can be known, behind the interpolation adjuvant, can obviously reduce the hygroscopicity of extract; And after placing 48h, hydroscopicity reaches balance substantially, sees accompanying drawing 1 for details---the moisture absorption percentage curves.
Table 27 intuitive analysis
Table 28 comprehensive grading
Screening ratio of adjuvant according to comprehensive grading is extract powder: aleurone is smart: starch=1: 4: 0-1: 0: 4.
The mensuration of critical relative humidity (CRH):
Take by weighing 6 parts of granules, every part of about 0.5g, be tiled in the weighing botle that is dried to constant weight, accurately weighed, open bottle cap, put in the glass exsiccator of the sulfuric acid solution that fills variable concentrations, in 25 ℃ constant incubator, preserved 7 days, take out weighing botle, accurately weighed weight is calculated the moisture absorption percentage rate, the results are shown in Table 29, with hydroscopicity to the relative humidity sucting wet curve of mapping to get, see accompanying drawing 2 as can be known, the critical relative humidity value of this granule approximately is 65%, therefore when the packing granule, relative humidity should be controlled at below 65%, with the quality of assurance section granule.
Table 29 critical relative humidity
Consumption of the present invention and specification.
Prescription Chinese crude drug total amount is 400g, investigates the result as can be known according to technique, and dried cream yield is about 30g.In conjunction with actual production, it is suitable at 120g to add the adjuvant amount.Abide by the clear syrup consumption of original sense (oral, a 20mL, 3 times on the one), according to each serving with the constant principle of crude drug amount, the usage and dosage of Ganqing Granules is: oral, and a 3g, 3 times on the one.Once taking the crude drug amount is 8g.
For better proof the present invention is in the advantage aspect pharmacological effect, the energy-conserving and environment-protective, we have carried out the research of the contrast tests such as pharmacological effect, fuels and energy statistics with the present invention and existing patent ZL02134089.7 " a kind of medicine for the treatment of flu ".
The pharmacodynamic study of Ganqing Granules:
Pharmacodynamic test of active extract:
Experimental animal: healthy Kunming mouse, cleaning level, body weight is about 18-22g, and is male, provided the animal quality certification number by the Guiyang Medical College Experimental Animal Center: SCXK (Guizhou Province) 2012-0001.
Medicine: Ganqing Granules (product that utilizes preparation technology of the present invention to produce, specification: the 3g/ bag); Feel clear syrup (Braun Guizhou Pharmaceutical Enterprise Group Co, lot number: 20110801, specification: 20ml/ props up).
Dosage is calculated: feel clear granule specification: every gram Ganqing Granules is equivalent to 2.67g crude drug powder, i.e. 2.67g crude drug/g.Becoming body weight for humans to press 60kg calculates.Feel the Coming-of-Age Day of clear granule and use dosage: (2.67g crude drug/g * 1 bag/time * 3g/ bag * 3 times/day) ÷ 60kg=0.4g crude drug/kg/ day.
Feel clear syrup specification: every mL feels clear syrup and is equivalent to 0.4g crude drug powder, i.e. 0.4g crude drug/mL.Becoming body weight for humans to press 60kg calculates.Feel the Coming-of-Age Day of clear syrup and use dosage: (0.4g crude drug/mL * 1/time * 20mL/ prop up * 3 times/days) ÷ 60kg=0.4g crude drug/kg/ day.
About Mouse Weight 18-22g, dosage is 10 times of adults, and mice dosage every day should be 4g crude drug/kg/ day.Mice every day, maximum dosage was 0.8mL, and therefore feeling clear granule should be dissolved in the water, and makes concentration and is: 4g crude drug/kg/ day * 20g ÷ 0.8mL=0.1g/mL.
The concentration of feeling clear syrup also should be: 4g crude drug/kg/ day * 20g ÷ 0.8mL=0.1g/mL.
The test liquid preparation:
1. feel clear granule test liquid: get one bag of clear granule of sense, be dissolved in the 80mL water, get namely that to contain crude drug concentration be the 0.1g/mL medicinal liquid.
2. feel clear syrup test liquid: get one in clear syrup of sense, be diluted to 80ml, get namely that to contain crude drug concentration be the 0.1g/mL medicinal liquid.
Test method and result:
Impact on ear swelling due to the mice dimethylbenzene: take healthy male mice as experimental subject, be divided into 6 groups, 10 every group.Take normal saline as matched group, Ganqing Granules group and the clear syrup group of sense are study group, and dimethylbenzene is proinflammatory agent, relatively the antiphlogistic effects of the two.Continuous five days gavages, once a day, last caused inflammation after 1 hour.At the front and back of auris dextra two sided coatings dimethylbenzene, volume is 0.02mL/, and left ear is not done any processing.Behind the 4h, with sacrifice of animal, cut ears and lay round auricle at same position respectively with 8mm diameter card punch, torsion balance is weighed.Every Mus auris dextra sheet weight deducts left auricle and heavily is swelling, and matched group and study group are carried out statistical procedures.The results are shown in Table 30.
Table 30 antiinflammatory test result of the test
Table 31 antiinflammatory test t assay
As shown in Table 31, result of the test is carried out in twos paired t-test, and each study group and normal saline group be (1-2) relatively, and the P value is all less than 0.05, illustrate that each study group all can xylol causes mice ear inhibitory action is arranged, prove that whether feel clear liquid medicine leaves standstill and all have antiinflammatory action; And (3) P value illustrates that also less than 0.05 Ganqing Granules group xylol causes mice ear obvious inhibitory action is arranged between two study groups, and its action effect is better than feeling clear syrup group.
The impact pain caused on mice acetic acid: take healthy male mice as experimental subject, be divided into 6 groups, 10 every group.Take normal saline as matched group, Ganqing Granules group and the clear syrup group of sense are study group, relatively the analgesic effect of the two.Gastric infusion, the gavage amount is the 0.4mL/10g body weight, once a day, continuous 5 days, after the last administration 1 hour, lumbar injection 0.6% acetic acid normal saline solution, 0.2mL/ were only, observe and inject the writhing number of times that mice occurs in rear 15 minutes, be calculated as follows medicine the suppression ratio of writhing response is passed judgment on the medicine analgesic effect:
Suppression ratio %=(normal saline group writhing mean-reagent group writhing mean)/normal saline group writhing mean * 100%
Table 32 analgesic test result
The interpretation of result of table 33 analgesic test
As shown in Table 33, result of the test is carried out in twos paired t-test as can be known, and each study group compares (1-2) with the normal saline group, and the P value is all less than 0.05, show that study group's Dichlorodiphenyl Acetate causes mice pain obvious inhibitory action is arranged, prove whether static the sense clear liquid medicine is and all have an analgesic activity; And (3) P value illustrates that also less than 0.05 Ganqing Granules group Dichlorodiphenyl Acetate causes mice pain obvious inhibitory action is arranged between two study groups, and its action effect is better than feeling clear syrup group.
Mice ammonia is induced the impact of cough: take healthy male mice as experimental subject, take normal saline as contrast, Ganqing Granules group and the clear syrup group of sense are study group, relatively the antitussive effect of the two.Gastric infusion, the gavage amount is the 0.4mL/10g body weight, and once a day, continuous 5 days, 30min after the last administration adopted the strong aqua ammonia spraying to cause the method for coughing and tests.
Table 34 antitussive result of the test
By the result of table 34 as seen, the cough latent period that Ganqing preparation can make mice ammonia induce prolongs, and the cough number of times reduces.
The interpretation of result of table 35 antitussive test cough latent period
Shown by table 35 analysis result, each study group compares (1-2) with normal saline, the P value proves that all less than 0.05 the mouse cough that Ganqing preparation is induced ammonia all has significant difference incubation period, proves the whether static effect that all has the prolongation cough latent period of sense clear liquid medicine; And (3) P value shows that also less than 0.05 the mouse cough that the Ganqing Granules group is induced ammonia has obvious prolongation effect, its action effect to be better than feeling clear syrup group incubation period between two study groups.
The interpretation of result of table 36 antitussive test 2min cough number of times
Shown that by table 36 analysis result each study group compares (1-2) with normal saline, the P value proves that all less than 0.05 the mouse cough time number average that Ganqing preparation is induced ammonia has significant difference, proves the whether static effect that all has antitussive of sense clear liquid medicine; And (3) P value shows that also less than 0.05 mouse cough number of times that the Ganqing Granules group is induced ammonia has the effect of obvious minimizing between two study groups, and its action effect is better than feeling clear syrup group.
Acute toxicity test:
Test objective: observe continuous several times in the tested material Ganqing Granules group one day and give the acute toxic reaction and the death condition that produce behind the animal.
Experimental animal: healthy Kunming mouse, cleaning level, body weight is about 18-22g, male and female half and half are provided by the Guiyang Medical College Experimental Animal Center, the animal quality certification number: SCXK (Guizhou Province) 2012-0001.
Medicine: Ganqing Granules group test sample: get 50 bags of Ganqing Granules, with 40mL water it is disperseed mixing, make that to be equivalent to contain crude drug concentration be the 10g/mL test sample.
Test method: through preliminary experiment, give a gavage Ganqing Granules of mice group test sample 0.4mL/10g, do not cause dead mouse.Be limited to drug level and the administration volume can not increase again, can't measure LD50, so carry out the mensuration of maximum tolerated dose.
Get 20 of mices, male and female half and half, body weight is about 18-22g, with Ganqing Granules group test sample, by maximum concentration (every mL is equivalent to crude drug in whole 10g) and the maximum gavage capacity (0.4mL/10g) of mice, every 2h is administered once, administration 6 times, dosage is 1200g crude drug/kg/ day, and this dosage is Coming-of-Age Day 3000 times of dosing.Raise routinely after the mice administration and observed 7 days.
Result of the test: mice is not dead, the overt toxicity reaction do not occur.It is safe that the extracting solution of proof Ganqing Granules does not leave standstill.
Conclusion: the Ganqing Granules group is 1200g crude drug/kg in the maximum tolerated dose of decimal gastric infusion, 3000 times of the consumption that is equivalent to be grown up, and the acute toxicity that prompting sense clear liquid medicine does not leave standstill is very little, oral safety.
Result and discussion:
Take the normal saline group as reference, Ganqing Granules group and the clear syrup group of sense are carried out antiinflammatory, analgesia, antitussive experiment, the relatively drug action of two kinds of Ganqing preparations.
Pharmacological evaluation proves, require among the clear supernatant samples of sense of " leaving standstill 24h; get supernatant concentration to 600-700ml " preparation and the present invention extracting solution directly to be concentrated into the non-sample that leaves standstill of 600-700ml according to the extraction process of the preparation method of the Ganqing preparation intermediate products that relate in the clear syrup preparation method of sense among the existing patent ZL02134089.7 " a kind of medicine for the treatment of flu ", verify through pharmacodynamics, both have significant antiinflammatory, analgesia, antitussive effect, and antiinflammatory, analgesia, antitussive effect that the present invention shows are more remarkable.
Acute toxicity testing proves simultaneously that also the sense clear liquid medicine of cancellation " leaving standstill 24h " does not produce the phenomenon that causes dead mouse.After can thinking that cancellation " is left standstill 24h ", the variation of matter does not occur in the drug effect aspect of sense clear liquid medicine.Prove that step that cancellation of the present invention " is left standstill 24h " is reasonably, it is rational utilizing the drug action of the clear granular preparation of sense that the present invention produces.
The fuels and energy statistics:
According to the weight portion meter, 100 times of the above-mentioned Ganqing Granules recipe quantity of foundation are the pilot scale scheme.As the investigation factor, investigate continuously the surcharge that three batches of volumes of production produce take " whether cancel and leave standstill 24h ", the result is shown in following table 37:
The surcharge that three batches of volumes of production of 100 times of recipe quantities of table 37 produce relatively
As shown in Table 37, cancellation is to the process that leaves standstill of the intermediate products of Ganqing Granules, can save human and material resources, reduce production costs, improve to a certain extent the rate that comes into force, the checking of above-mentioned pharmacodynamics is arranged in addition, can prove that the preparation technology of a kind of Ganqing preparation of the present invention has novelty, have breakthrough, for large production provides a kind of new environmental protection and energy saving, more efficiently novel form.
Description of drawings
Fig. 1 is the moisture absorption percentage curves figure during hygroscopicity of the present invention is investigated;
Fig. 2 be during hygroscopicity of the present invention is investigated with hydroscopicity to relative humidity map sucting wet curve figure.
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1:
The preparation technology of Ganqing Granules: calculate by weight and take by weighing Radix seu Herba Gei aleppici 65g, Radix Chimonanthi praecocis 60g, Folium Hibisci Mutabilis 50g, Folium Perillae 50g, Herba Lysionoti Pauciflori 50g, Herba Kalimeridis grass 75g and Herba Schizonepetae 50g, Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass and Herba Schizonepetae all are cut into 0.3～2.0cm section or silk, are mixed to get a product; The a product are decocted with water 2 times, each 1 hour, add 7 times of water gagings for the first time, add 8 times of water gagings for the second time, filter with 200 order filter clothes, merging filtrate gets the b product; The b product are carried out vacuum-concentrcted, and thickening temperature is 80 ℃, is concentrated into relative density and is about 1.10, gets the c product; The c product are made powder by drying under reduced pressure, get extract; In extract, add adjuvant and be prepared into granular preparation; Adjuvant is dextrine powder; The weight proportion of extract and adjuvant is 1: 4.Adding adjuvant in extract is prepared into granular preparation and is specially, make wetting agent with 85% ethanol after adding adjuvant, then use dry granulation, adopt again No. 2 pharmacopeia sieves and No. 4 pharmacopeia sieves to carry out granulate, the granule of getting by No. 2 pharmacopeia sieve but can not be by No. 4 pharmacopeia sieves namely makes Ganqing Granules as finished product.Extract contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 18%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 5.6%.Ganqing Granules contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 4%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 0.8%.Oral, a 3g, 3 times on the one.
Embodiment 2:
The preparation technology of Ganqing Granules: calculate by weight and take by weighing Radix seu Herba Gei aleppici 65g, Radix Chimonanthi praecocis 60g, Folium Hibisci Mutabilis 50g, Folium Perillae 50g, Herba Lysionoti Pauciflori 50g, Herba Kalimeridis grass 75g and Herba Schizonepetae 50g, with Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass, Herba Schizonepetae all be cut into 0.3-2.0cm the section or the silk, be mixed to get a product; The a product are decocted with water 2 times, each 1 hour, add 7 times of water gagings for the first time, add 8 times of water gagings for the second time, filter with 80 order filter clothes, merging filtrate gets the b product; The b product are carried out vacuum-concentrcted, and thickening temperature is 80 ℃, and being concentrated into relative density is 1.08, gets the c product; With the c product take 60 ℃ as inlet temperature, 100 ℃ is outlet temperature, charging rate is 10mLmin
-1, carry out spray drying, collect extract powder, get extract; In extract, add adjuvant and be prepared into granular preparation; Adjuvant is the mixture of dextrine powder and starch, and the weight ratio of dextrine powder and starch is 1: 1; The weight proportion of extract and adjuvant is 1: 4.Adding adjuvant in extract is prepared into granular preparation and is specially, make wetting agent with 65% ethanol after adding adjuvant, then use dry granulation, adopt again No. 2 pharmacopeia sieves and No. 4 pharmacopeia sieves to carry out granulate, the granule of getting by No. 2 pharmacopeia sieve but can not be by No. 4 pharmacopeia sieves namely makes Ganqing Granules as finished product.Extract contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 18%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 5.6%.Ganqing Granules contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 4%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 0.8%.Oral, a 3g, 3 times on the one.
Embodiment 3:
The preparation technology of Ganqing Granules: calculate by weight and take by weighing Radix seu Herba Gei aleppici 65g, Radix Chimonanthi praecocis 60g, Folium Hibisci Mutabilis 50g, Folium Perillae 50g, Herba Lysionoti Pauciflori 50g, Herba Kalimeridis grass 75g and Herba Schizonepetae 50g, with Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass, Herba Schizonepetae all be cut into 0.3-2.0cm the section or the silk, be mixed to get a product; The a product are decocted with water 2 times, each 1 hour, add 7 times of water gagings for the first time, add 8 times of water gagings for the second time, filter with 80 order filter clothes, merging filtrate gets the b product; The b product are carried out vacuum-concentrcted, and thickening temperature is 75 ℃, and being concentrated into relative density is 1.09, gets the c product; With the c product by take 80 ℃ as inlet temperature, 120 ℃ is outlet temperature, charging rate is 35mLmin
-1, carry out spray drying, collect extract powder, get extract.In extract, add adjuvant and be prepared into granular preparation; Adjuvant is the mixture of dextrine powder and starch, and the weight ratio of dextrine powder and starch is 3: 1; The weight proportion of extract and adjuvant is 1: 4.Adding adjuvant in extract is prepared into granular preparation and is specially, make wetting agent with 60% ethanol after adding adjuvant, then use dry granulation, adopt again No. 2 pharmacopeia sieves and No. 4 pharmacopeia sieves to carry out granulate, the granule of getting by No. 2 pharmacopeia sieve but can not be by No. 4 pharmacopeia sieves namely makes Ganqing Granules as finished product.Extract contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 18%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 5.6%.Ethanol is the ethanol of %.Ganqing Granules contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 4%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 0.8%.Oral, a 3g, 3 times on the one.
Embodiment 4:
The preparation technology of Ganqing Granules: calculate by weight and take by weighing Radix seu Herba Gei aleppici 65g, Radix Chimonanthi praecocis 60g, Folium Hibisci Mutabilis 50g, Folium Perillae 50g, Herba Lysionoti Pauciflori 50g, Herba Kalimeridis grass 75g and Herba Schizonepetae 50g, with Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass, Herba Schizonepetae all be cut into 0.3-2.0cm the section or the silk, be mixed to get a product; The a product are decocted with water 2 times, each 1 hour, add 7 times of water gagings for the first time, add 8 times of water gagings for the second time, filter with 100 order filter clothes, merging filtrate gets the b product; The b product are carried out vacuum-concentrcted, and thickening temperature is 75 ℃, and being concentrated into relative density is 1.09, gets the c product; With the c product take 150 ℃ as inlet temperature, 220 ℃ is outlet temperature, charging rate is 70mLmin
-1, carry out spray drying, collect extract powder, get extract.In extract, add adjuvant and be prepared into granular preparation; Adjuvant is starch; The weight proportion of extract and adjuvant is 1: 4.Adding adjuvant in extract is prepared into granular preparation and is specially, make wetting agent with 75% ethanol after adding adjuvant, then use dry granulation, adopt again No. 2 pharmacopeia sieves and No. 4 pharmacopeia sieves to carry out granulate, the granule of getting by No. 2 pharmacopeia sieve but can not be by No. 4 pharmacopeia sieves namely makes Ganqing Granules as finished product.Extract contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 18%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 5.6%.Ganqing Granules contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 4%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 0.8%.Oral, a 3g, 3 times on the one.
Embodiment 5:
The preparation technology of Ganqing Granules: calculate by weight and take by weighing Radix seu Herba Gei aleppici 65g, Radix Chimonanthi praecocis 60g, Folium Hibisci Mutabilis 50g, Folium Perillae 50g, Herba Lysionoti Pauciflori 50g, Herba Kalimeridis grass 75g and Herba Schizonepetae 50g, with Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass, Herba Schizonepetae all be cut into 0.3-2.0cm the section or the silk, be mixed to get a product; The a product are decocted with water 2 times, each 1 hour, add 7 times of water gagings for the first time, add 8 times of water gagings for the second time, filter with 80 order filter clothes, merging filtrate gets the b product; The b product are carried out vacuum-concentrcted, and thickening temperature is 75 ℃, and being concentrated into relative density is 1.09, gets the c product; With the c product take 80 ℃ as inlet temperature, 120 ℃ is outlet temperature, charging rate is 35mLmin
-1, carry out spray drying, collect extract powder, get extract.In extract, add adjuvant and be prepared into granular preparation; Adjuvant is starch; The weight proportion of extract and adjuvant is 1: 4.Adding adjuvant in extract is prepared into granular preparation and is specially, make wetting agent with 75% ethanol after adding adjuvant, then use dry granulation, adopt again No. 2 pharmacopeia sieves and No. 4 pharmacopeia sieves to carry out granulate, the granule of getting by No. 2 pharmacopeia sieve but can not be by No. 4 pharmacopeia sieves namely makes Ganqing Granules as finished product.Extract contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 18%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 5.6%.Ganqing Granules contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 4%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 0.8%.Oral, a 3g, 3 times on the one.
Claims (7)
1. the preparation technology of a Ganqing Granules, it is characterized in that: calculate by weight and take by weighing 50 parts of 65 parts of Radix seu Herba Gei aleppici, 60 parts of Radix Chimonanthi praecocis, 50 parts of Folium Hibisci Mutabiliss, 50 parts of Folium Perillaes, 50 parts of Herba Lysionoti Paucifloris, 75 parts of Herba Kalimeridis grasss and Herba Schizonepetae, with Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass and Herba Schizonepetae all be cut into 0.3-2.0cm the section or the silk, be mixed to get a product; The a product are decocted with water 2 times, each 1 hour, add 7-8 times of water gaging for the first time, add 8-9 times of water gaging for the second time, filter with 80-200 order filter cloth, merging filtrate gets the b product; The b product are carried out vacuum-concentrcted, and thickening temperature is 75 ℃-80 ℃, is concentrated into relative density and is about 1.08-1.10, gets the c product; The c product are made powder by drying under reduced pressure, microwave drying or spray drying, get extract; In extract, add adjuvant and be prepared into granular preparation; Adjuvant is dextrine powder and/or starch; The weight proportion of extract and adjuvant is 1:4.
2. the preparation technology of Ganqing Granules according to claim 1, it is characterized in that: the described adjuvant that adds in extract is prepared into granular preparation, be specially, make wetting agent with ethanol after adding adjuvant, then use dry granulation, adopt again No. 2 pharmacopeia sieve and No. 4 pharmacopeia sieves to carry out granulate, get by No. 2 pharmacopeia sieves but the granule that can not sieve by No. 4 pharmacopeia as finished product, namely make Ganqing Granules.
3. the preparation technology of Ganqing Granules according to claim 1 is characterized in that: prepare extract according to following step;
A. Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass, Herba Schizonepetae all are cut into section or the silk of 0.3-2.0cm, are mixed to get a product;
B. a product are decocted with water 2 times, each 1 hour, add 7-8 times of water gaging for the first time, add 8-9 times of water gaging for the second time, filter with 80-200 order filter cloth, merging filtrate gets the b product;
C. the b product are carried out vacuum-concentrcted, thickening temperature is 75 ℃-80 ℃, and being concentrated into relative density is 1.09, gets the c product;
D. with the c product take 60-150 ℃ as inlet temperature, 100-220 ℃ is outlet temperature, charging rate is 10-70 mLmin
-1, carry out spray drying, collect extract powder, get extract.
4. the preparation technology of Ganqing Granules according to claim 3 is characterized in that: prepare extract according to following step;
A. Radix seu Herba Gei aleppici, Radix Chimonanthi praecocis, Folium Hibisci Mutabilis, Folium Perillae, Herba Lysionoti Pauciflori, Herba Kalimeridis grass, Herba Schizonepetae all are cut into section or the silk of 0.3-2.0cm, are mixed to get a product;
B. a product are decocted with water 2 times, each 1 hour, add 7 times of water gagings for the first time, add 8 times of water gagings for the second time, filter with 80 order filter clothes, merging filtrate gets the b product;
C. the b product are carried out vacuum-concentrcted, thickening temperature is 75 ℃-80 ℃, and being concentrated into relative density is 1.09, gets the c product;
D. with the c product with 80 ℃ of inlet temperatures, 120 ℃ is outlet temperature, charging rate is 30-40 mLmin
-1, carry out spray drying, collect extract powder, get extract.
5. according to claim 1, the preparation technology of 3 or 4 described Ganqing Granules, it is characterized in that: described extract contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 18%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 5.6%.
6. the preparation technology of Ganqing Granules according to claim 2, it is characterized in that: described ethanol is 75% ethanol.
7. the preparation technology of Ganqing Granules according to claim 1 and 2, it is characterized in that: described Ganqing Granules contains Radix seu Herba Gei aleppici with gallic acid (C
7H
6O
5) meter, be no less than 4%; Contain Herba Lysionoti Pauciflori with lysionotin (C
18H
16O
7) meter, be no less than 0.8%.
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| CN201210453920XA CN102961463A (en) | 2012-11-14 | 2012-11-14 | Process for preparing Ganqing granules |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107929445A (en) * | 2017-11-29 | 2018-04-20 | 济南市儿童医院 | A kind of pharmaceutical composition for treating the infection of the upper respiratory tract and preparation method thereof |
| CN111773276A (en) * | 2020-03-24 | 2020-10-16 | 贵州省中国科学院天然产物化学重点实验室(贵州医科大学天然产物化学重点实验室) | Application of kalimeris indica cold-feeling compound in preparation of novel coronavirus infection resisting medicines |
| CN116159115A (en) * | 2023-01-13 | 2023-05-26 | 崔书克 | Preparation method of novel coronavirus prevention and treatment traditional Chinese medicine composition |
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| CN1857457A (en) * | 2005-08-24 | 2006-11-08 | 贵州百灵企业集团制药有限公司 | Ganqing preparation and its preparing process |
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| DE202010013170U1 (en) * | 2010-12-21 | 2011-04-28 | Yangsen Biotechnology Co., Ltd., Bei-Tou | Composition of essential oils for the treatment and / or prevention of respiratory diseases |
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| CN1413693A (en) * | 2002-11-13 | 2003-04-30 | 贵州省安顺制药厂 | Drug for treating cold |
| WO2006033351A1 (en) * | 2004-09-22 | 2006-03-30 | Kyoto University | Thioredoxin expression inducing composition |
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| CN107929445A (en) * | 2017-11-29 | 2018-04-20 | 济南市儿童医院 | A kind of pharmaceutical composition for treating the infection of the upper respiratory tract and preparation method thereof |
| CN111773276A (en) * | 2020-03-24 | 2020-10-16 | 贵州省中国科学院天然产物化学重点实验室(贵州医科大学天然产物化学重点实验室) | Application of kalimeris indica cold-feeling compound in preparation of novel coronavirus infection resisting medicines |
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