CN106620188B - A kind of preparation method of clearing heat and detoxicating particle - Google Patents
A kind of preparation method of clearing heat and detoxicating particle Download PDFInfo
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- CN106620188B CN106620188B CN201611201797.7A CN201611201797A CN106620188B CN 106620188 B CN106620188 B CN 106620188B CN 201611201797 A CN201611201797 A CN 201611201797A CN 106620188 B CN106620188 B CN 106620188B
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- cornu bubali
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- cream
- water
- filtrate
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Abstract
The invention belongs to pharmaceutical fields, and in particular to clearing heat and detoxicating particle is made of following Chinese medicine material：Clearing heat and detoxicating particle of the invention uses circumfluence distillation to clearing heat and detoxicating particle, 10 times of amount water of cornu bubali, and extraction time 14 hours, the hot 0.2m that flows back3/ h, the time of beginning are 6 hours.
Description
Technical field
The present invention relates to the new preparation methods of clearing heat and detoxicating particle, belong to pharmaceutical technology field.
Background technique
Clearing heat and detoxicating particle is a variety of by the coptis, cornu bubali, radix scrophulariae, honeysuckle, glutinous rehmannia, folium isatidis, Fructus Forsythiae, rhizoma anemarrhenae gypsum etc.
Chinese medicine composition, have it is clearing heat and detoxicating, nourishing Yin and promoting production of body fluid lets out fire and other effects.Be mainly used for anemopyretic cold, mumps and
Gently, the diseases such as medium-sized encephalitis B, clinical efficacy is significant, is widely used.
The preparation method of existing clearing heat and detoxicating particle：Above nine taste, cornu bubali pound flakiness, add water to cook it is secondary, often
Secondary 7 hours, collecting decoction, filtration；Gypsum breaks into fragment, is installed with cloth bag, the coptis, radix scrophulariae, glutinous rehmannia slice, with remaining Fructus Forsythiae etc.
Four tastes add water to cook it is secondary, 2 hours every time.Filtration, filtrate merge with cornu bubali decoction liquor, filter, filtrate is concentrated into relatively close
Degree for 1.12~1.20 (heat is surveyed) clear cream, let cool, add ethyl alcohol to amount of alcohol is contained to be 60%, be sufficiently stirred, stand, take supernatant
It is concentrated into the clear cream that relative density is 1.38~1.40 (heat is surveyed).1 part of qinghuo reagent, 2.5 parts of sucrose, 1.25 parts of dextrin suitable with ethyl alcohol
Amount, is made particle, it is dry to get.
Existing preparation method there are the problem of have：The problems such as curative effect of medication is not high, and medicinal material wastes, gained particle storage one
Fixing time can crush, and effective component reduces.For this purpose, applicant improves existing preparation method, provide a kind of clear
The new preparation method of thermal detoxification particle, this method can be improved the curative effect of clearing heat and detoxicating particle, and it is effective to improve clearing heat and detoxicating particle
Component content, while solving the problems, such as that stability and particle crush.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of clearing heat and detoxicating particle.
The preparation method of clearing heat and detoxicating particle of the present invention is prepared by following Chinese medicine material medicine：
Preparation method：
1) cornu bubali pound flakiness, 0.1-0.6 parts of cornu bubalis are pulverized, spare；0.9-0.1 parts of cornu bubalis are added
The water of 10-14 times of volume, with 0.2-0.6m3The hot regurgitant volume of/h is extracted, and the hot return time of beginning is 4-6 hours, always
Total 8-16h, filtrate are spare；The cornu bubali dregs of a decoction add 4-6 times of water, are placed in pressure cooker, use pressure for 1.8 × 105Pa is decocted, and 3
It after hour, is concentrated together with phegma, receives cream.
2) gypsum breaks into fragment, glutinous rehmannia slice；Gypsum and the coptis, radix scrophulariae, glutinous rehmannia, Fructus Forsythiae, honeysuckle, folium isatidis and rhizoma anemarrhenae
It mixes, the water of 8-12 times of weight is added, with 0.1-0.6m3The hot regurgitant volume of/h is extracted 2-4 times, each 10-40min,
Filtrate is concentrated into clear cream, lets cool, and merges with cornu bubali cream, and filtration, filtrate is concentrated into clear cream, and adding ethyl alcohol to alcohol content is 50-
70%, be sufficiently stirred, stand, supernatant is taken to be concentrated into clear cream, plus auxiliary material and Cornu Bubali powder pelletize to get.
Wherein, the water of 8-12 times of weight refers to：Gypsum, the coptis, radix scrophulariae, glutinous rehmannia, Fructus Forsythiae, honeysuckle, folium isatidis and rhizoma anemarrhenae
8-12 times of the total weight of medicinal material.
Preferably, preparation method of the invention, includes the following steps：
1) cornu bubali pound flakiness, 0.1-0.6 parts of cornu bubalis are pulverized, spare；0.9-0.1 parts of cornu bubalis are i.e.
The water of 10-14 times of volume is added, with 0.2-0.6m3The hot regurgitant volume of/h is extracted, and the hot return time of beginning is that 4-6 is small
When, (heat reflux is the timing since the 4-6 hour) 8-16h, filtrate, filtering are spare in total；The cornu bubali dregs of a decoction add water 4-6
Times, it is placed in pressure cooker, uses pressure for 1.8 × 105Pa is decocted, and after 3 hours, is concentrated together with phegma, and cream is received.
2) gypsum breaks into fragment, glutinous rehmannia slice；Then by gypsum and the coptis, radix scrophulariae, glutinous rehmannia, Fructus Forsythiae, honeysuckle, folium isatidis
It is mixed with rhizoma anemarrhenae, is added 8-10 times and measures water, with 0.2-0.4m3The hot regurgitant volume of/h is extracted 2-4 times, each 20-
40min, filtrate are concentrated into clear cream, let cool, and merge with cornu bubali cream, and filtration, filtrate is concentrated into clear cream, add ethyl alcohol to containing amount of alcohol
Be 60%, be sufficiently stirred, stand, supernatant is taken to be concentrated into clear cream, plus auxiliary material and Cornu Bubali powder pelletize to get.
Most preferably, preparation method of the invention, includes the following steps：
1) cornu bubali pound flakiness, 0.2 part of cornu bubali is pulverized, spare；10 times of amounts are added in 0.8 part of cornu bubali
Water, with 0.2m3The hot regurgitant volume of/h is extracted, and the hot return time of beginning is the 6th hour, in total 14h, filtrate, and filtering is spare；
The cornu bubali dregs of a decoction add 6 times of water, are placed in pressure cooker, use pressure for 1.8 × 105Pa is decocted, after 3 hours, together with phegma
Cream is received in concentration.
2) gypsum breaks into fragment, glutinous rehmannia slice；Then by gypsum and the coptis, radix scrophulariae, glutinous rehmannia, Fructus Forsythiae, honeysuckle, folium isatidis
It is mixed with rhizoma anemarrhenae, adds 10 amount of water, extract 150min, heat reflux 0.2m3/ h, the time of beginning are that (heat flows back 30min
The timing since 30min), after the completion of extraction, filtrate is concentrated into clear cream, lets cool, and merges with cornu bubali cream, filters, and filtrate is dense
Be reduced to clear cream, add ethyl alcohol to contain amount of alcohol be 60%, be sufficiently stirred, stand, take supernatant to be concentrated into clear cream, in addition auxiliary material and water
Horn powder granulation to get.
The preparation method is that obtained after many experiments are preferred, related experiment is as follows：
The nitrogen pool of each experiment is measured simultaneously, cornu bubali ultramicro grinding is more, and total nitrogen content is higher, cornu bubali medicine
Slag high pressure decocts the nitrogen content for decocting cornu bubali than normal pressure and obviously increases, while considering that patient's is convenient to take, chooses test 1；
By multidigit, patient is taken, and anemopyretic cold, mumps and the healing of light, medium-sized encephalitis B are apparently higher than prior art
Preparation clearing heat and detoxicating particle, can able person be easier absorb cornu bubali in amino acids substance and sterol substance.
It is analyzed from thin layer simultaneously, cholesterine；Alanine, aspartic acid, cystine, leucine, proline, tyrosine,
The substances such as histidine, valine are apparently higher than the clearing heat and detoxicating particle of prior art preparation,
Cornu bubali optimal extraction technology
Trial test is affected studies have shown that decocting number, amount of water, extraction time, hot return flow to result is extracted.
The key parameter amount of water for influencing cornu bubali extraction effect, extraction time, hot return flow, decoction time have mainly been investigated in this research
The factors such as number, are arranged 3 levels, using L934Orthogonal table optimizes buffalo using cornu bubali nitrogen pool as evaluation index
Angle extraction process.Orthogonal design factor level table is shown in Table 1.
Nitrogen content is measured according to 2005 editions Ⅸ the first methods of L n2 method of pharmacopeia annex.
1 water extraction process factor level table of table
A pound flakiness cornu bubali 20kg is taken, by L9(34) orthogonal array requires test, extracting solution is concentrated into relative density
1.05 (80 DEG C) measure nitrogen content.Orthogonal and it the results are shown in Table 2.
2 cornu bubali decocting process orthogonal design of table and result
Optimal condition：10 times of amount water, extraction time 14 hours, heat reflux 0.2m3/ h, the time of beginning are 6 hours.
As can be seen from the results, using nitrogen content in concentrate as inspection target, using very poor intuitive analysis shows that influence factor is big
Small is D > B > C > A, and variance analysis shows to decoct number D to result is extracted with significantly affecting, and according to K value, D factor should be selected
Level 3, B factor should select level 1, and C factor should select level 1, and A factor should select level 1, optimum extraction process D3B1C1A1, i.e., plus
Enter 10 times of amount water, with 0.2m3The hot regurgitant volume of/h is extracted, and the hot return time of beginning is the 6th hour, in total 14h.
3 variance analysis of table
F0.05(2,2)=19.000
The verifying of cornu bubali extraction process
According to above-mentioned preferred condition, three batches are verified, the results showed that, the extraction process is reliable and stable, the results are shown in Table 4.
4 cornu bubali extraction process verification result of table
Cornu bubali traditional extraction technique is compared with new process
This research is compared selection process and traditional handicraft using nitrogen content in the concentrate extracted as inspection target
Analysis, the results showed that, cornu bubali Optimized extraction techniques concentrate content is higher than traditional handicraft.It the results are shown in Table 5.
5 cornu bubali new process of table extract compared with traditional handicraft compared with
Other medicinal material extract technical studies
Trial test is affected studies have shown that decocting number, amount of water, extraction time, hot return flow to result is extracted.
The key parameter amount of water for influencing other medicinal material extract effects in addition to cornu bubali, extraction time, heat have mainly been investigated in this research
Return flow decocts the factors such as number, 3 levels is arranged, using L934Orthogonal table is to comment with the chlorogenic acid rate of transform
Valence index, optimization formulation extraction process.Orthogonal design factor level table is shown in Table 6.
6 medicinal material extract technological factor water-glass of table
Optimal condition is：Add 10 amount of water, extracts 150min, heat reflux 0.2m3/h, the time of beginning is 30min
The prescription medicine 20kg for taking pre-treatment is tested by L9 (34) orthogonal array requirement, measures green original in extracting solution
Acid content calculates the chlorogenic acid rate of transform.Orthogonal and it the results are shown in Table 7.
The clearing heat and detoxicating particle prescription extraction process orthogonal design of table 7 and result
As can be seen from the results, using the rate of transform of chlorogenic acid as inspection target, using very poor intuitive analysis shows that influence factor is big
Small is D > A > B > C, and variance analysis shows to decoct number D to result is extracted with significantly affecting, and according to K value, D factor should be selected
Level 3, A factor should select level 1, and B factor should select level 1, and C factor should select level 1, optimum extraction process D3A1C1B1, add water
10 amounts extract 150min, and heat reflux 0.2m3/h, the time of beginning is 30min
8 variance analysis of table
F0.05(2,2)=19.000
Study on extraction confirmatory experiment
According to above-mentioned preferred condition, three batches are verified, the results are shown in Table 9.The result shows that the extraction process is reliable and stable.
The clearing heat and detoxicating particle medicinal material water of table 9 proposes verification test result
The preparation method is that obtained after many experiments screen, illustrate the present invention below by way of experimental data
Beneficial effect：
Test the assay of 1, effective component
It is compared with existing drug, the assay of effective component in drug
The assay result for testing effective component in 2, the 6th month accelerated stability tests is as follows：
The present invention in terms of existing technologies, greatly improves the stability and quality of product, reduces side effects of pharmaceutical drugs,
The content of effective component is also improved simultaneously, and the present invention goes back simplification of flowsheet, reduces production cost, is suitble to large-scale production.
Specific embodiment
By following specific embodiments, the present invention is further illustrated, but not as limitation of the invention.
Embodiment 1：
Above nine taste, cornu bubali pound flakiness, 0.2 part of cornu bubali is pulverized, spare；0.8 part of cornu bubali adds
Enter 10 times of amount water, with 0.2m3The hot regurgitant volume of/h is extracted, and the hot return time of beginning is the 6th hour, in total 14h.Filtrate concentration
It is 1.05 filterings to relative density, receives cream, it is spare；The cornu bubali dregs of a decoction add 6 times of water, are placed in pressure cooker, use pressure for 1.8 ×
105Pa is decocted, and after 3 hours, is concentrated together with phegma, and cream is received.Glutinous rehmannia slice；Gypsum and the coptis, radix scrophulariae, glutinous rehmannia, Fructus Forsythiae, gold
Honeysuckle flower, folium isatidis and rhizoma anemarrhenae mix, and add 10 amount of water, extract 150min, heat reflux 0.2m3/h, and the time of beginning is
30min (heat reflux is the timing since 30min), after the completion of extraction, it is 1.05 (heat is surveyed) that filtrate, which is concentrated into relative density,
Clear cream is let cool, and is merged with cornu bubali cream, filtration, and filtrate is concentrated into the clear cream that relative density is 1.12~1.20 (heat is surveyed), adds second
Alcohol is 60% to amount of alcohol is contained, and is sufficiently stirred, and is stood, and taking supernatant to be concentrated into relative density is the clear of 1.38-1.40 (heat is surveyed)
Cream.
1 part of qinghuo reagent, 2.5 parts of sucrose, 1.25 parts of dextrin, Cornu Bubali powder is pelletized with efficient wet mixer-granulator, is made
Particle, with boiling drier it is dry to get.
Embodiment 2：
It is weighted according to the following proportion raw material：
Above nine taste, cornu bubali pound flakiness, 0.2 part of cornu bubali is pulverized, spare；0.8 part of cornu bubali adds
Enter 10 times of amount water, with 0.2m3The hot regurgitant volume of/h is extracted, and the hot return time of beginning is the 6th hour, in total 14h.Cornu bubali medicine
Slag adds 6 times of water, is placed in pressure cooker, uses pressure for 1.8 × 105Pa is decocted, and after 3 hours, is concentrated together with phegma, is received
Cream.It is 1.05 filterings that filtrate, which is concentrated into relative density, receives cream, spare；Glutinous rehmannia slice；Gypsum and the coptis, radix scrophulariae, glutinous rehmannia, Fructus Forsythiae,
Honeysuckle, folium isatidis and rhizoma anemarrhenae mix, and add 10 amount of water, extract 150min, heat reflux 0.2m3/h, and the time of beginning is
30min (heat reflux is the timing since 30min), after the completion of extraction, it is 1.05 (heat is surveyed) that filtrate, which is concentrated into relative density,
Clear cream is let cool, and is merged with cornu bubali cream, filtration, and it is spare that filtrate is concentrated into the clear cream that relative density is 1.12~1.20 (heat is surveyed).
3.75 parts of dextrin are added and Cornu Bubali powder is added in one-step-granulating method, spray into clear cream, fluidized bed granulation.
The step does not take alcohol precipitation, directly uses one-step-granulating method, and above-mentioned dextrin does not limit to a clear cream and 3.75 parts of dextrin ratios
Example.
Embodiment 3：
It is weighted according to the following proportion raw material：
Above nine taste, cornu bubali pound flakiness, 0.2 part of cornu bubali is pulverized, spare；0.8 part of cornu bubali adds
Enter 10 times of amount water, with 0.2m3The hot regurgitant volume of/h is extracted, and the hot return time of beginning is the 6th hour, in total 14h.Cornu bubali medicine
Slag adds 6 times of water, is placed in pressure cooker, uses pressure for 1.8 × 105Pa is decocted, and after 3 hours, is concentrated together with phegma, is received
Cream.It is 1.05 filterings that filtrate, which is concentrated into relative density, receives cream, spare；Glutinous rehmannia slice；Gypsum and the coptis, radix scrophulariae, glutinous rehmannia, Fructus Forsythiae,
Honeysuckle, folium isatidis and rhizoma anemarrhenae mix, and add 10 amount of water, extract 150min, heat reflux 0.2m3The time of/h, beginning is
30min (heat reflux is the timing since 30min), after the completion of extraction, it is 1.05 (heat is surveyed) that filtrate, which is concentrated into relative density,
Clear cream is let cool, and is merged with cornu bubali cream, filtration, and filtrate is concentrated into the clear cream that relative density is 1.12~1.20 (heat is surveyed), adds second
Alcohol is 60% to amount of alcohol is contained, and is sufficiently stirred, and is stood, and taking supernatant to be concentrated into relative density is the clear of 1.15-1.20 (heat is surveyed)
Cream.3.75 parts of dextrin are added and Cornu Bubali powder is added in one-step-granulating method, spray into clear cream, fluidized bed granulation.
It is 1.15-1.20 (heat is surveyed) that above-mentioned clear liquid, which is concentrated into relative density, and relative density is not limited to 1.15-1.20 (heat
Survey), as long as energy spray gun can spray, it can not also limit to a clear cream and 3.75 parts of cyclodextrin ratios with 1.21-1.24, it can also
With 1 part of qinghuo reagent, 2.5 parts of sucrose, 1.25 parts of dextrin, wherein sucrose can arbitrarily be changed with cyclodextrin ratios.
Claims (1)
1. a kind of preparation method of clearing heat and detoxicating particle, is prepared by following Chinese medicine material medicine：
Preparation method：
1) cornu bubali pound flakiness, 0.2 part of cornu bubali is pulverized, spare；10 times of amount water are added in 0.8 part of cornu bubali,
With 0.2m3The hot regurgitant volume of/h is extracted, and the hot return time of beginning is the 6th hour, in total 14h, filtrate, and filtering is spare；Buffalo
The angle dregs of a decoction add 6 times of water, are placed in pressure cooker, use pressure for 1.8 × 105Pa is decocted, and after 3 hours, is concentrated together with phegma,
Cream is received,
2) gypsum breaks into fragment, glutinous rehmannia slice；Then by gypsum and the coptis, radix scrophulariae, glutinous rehmannia and are known Fructus Forsythiae, honeysuckle, folium isatidis
Mother mixes, and adds 10 times of water amounts, 150min is extracted, with 0.2m3The hot regurgitant volume of/h is extracted, and starting hot return time is the
30min, after the completion of extraction, filtrate is concentrated into clear cream, lets cool, and merges with cornu bubali cream, and filtration, filtrate is concentrated into clear cream, adds second
Alcohol is 60% to amount of alcohol is contained, and is sufficiently stirred, and stands, supernatant is taken to be concentrated into clear cream, in addition auxiliary material and Cornu Bubali powder granulation, i.e.,
?.
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| CN1456226A (en) * | 2003-01-22 | 2003-11-19 | 毛友昌 | Preparation of acrid rhinitis pills |
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| CN102552655A (en) * | 2010-12-29 | 2012-07-11 | 江西济民可信集团有限公司 | Detection method for Chinese herbal preparation of particles capable of clearing heat and detoxicating |
| CN103006773A (en) * | 2012-12-31 | 2013-04-03 | 河南辅仁堂制药有限公司 | Traditional Chinese granule for children for clearing heat |
| CN104510758A (en) * | 2015-01-10 | 2015-04-15 | 江西济民可信药业有限公司 | Cornu bubali concentrated powder and preparation method for concentrated cornu bubali particles |
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| CN1215610A (en) * | 1998-10-16 | 1999-05-05 | 湖南正清制药集团股份有限公司 | Antipyretic and antitoxic particles and preparing method thereof |
| CN1456226A (en) * | 2003-01-22 | 2003-11-19 | 毛友昌 | Preparation of acrid rhinitis pills |
| CN101091760A (en) * | 2007-04-17 | 2007-12-26 | 崔振国 | Regeneration ointment for skin deteriment and preparation method |
| CN102552655A (en) * | 2010-12-29 | 2012-07-11 | 江西济民可信集团有限公司 | Detection method for Chinese herbal preparation of particles capable of clearing heat and detoxicating |
| CN103006773A (en) * | 2012-12-31 | 2013-04-03 | 河南辅仁堂制药有限公司 | Traditional Chinese granule for children for clearing heat |
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