CN102755450B - Preparation method of anti-inflammation detoxifying traditional Chinese medicine composition - Google Patents
Preparation method of anti-inflammation detoxifying traditional Chinese medicine composition Download PDFInfo
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Abstract
The invention provides a preparation method of an anti-inflammation detoxifying traditional Chinese medicine composition. The method comprises the following steps of: 1) grinding common andrographis herb into coarse powder; adding the coarse powder into a dynamic countercurrent extraction device of a five-section extraction pipe section, wherein 4-10ml/g of 75-95% ethanol is used, the extraction temperature is 65-85 DEG C, and the extraction lasts for 30-90min each time; merging the extraction liquid; and filtering to obtain the filtrate I; 2) adding root of indian stringbush into the dynamic countercurrent extraction device of a five-section extraction pipe section, wherein 6-10ml/g of water is used, the extraction temperature is 90-100 DEG C, and the extraction lasts for 30-50min in each section; merging the water extraction liquid; and filtering to obtain the filtrate II; and 3) concentrating the filtrate I obtained in the step 1) and the filtrate II obtained in the step 2) into extract respectively, merging, and performing reduced-pressure drying to obtain dry paste; or merging and concentrating, and performing reduced-pressure drying to obtain dry paste; and adding pharmaceutically acceptable accessories or not to obtain the traditional Chinese medicine composition. According to the invention, by adopting dynamic countercurrent extraction, the consumption of solvent is reduced, the extraction temperature is lowered, the extraction time is greatly shortened, and the extraction efficiency is improved.
Description
Technical field
The invention belongs to pharmaceutical field, be specifically related to a kind of preparation method comprising the Chinese medicine composition for diminishing of Herba Andrographis and Radix Wikstroemae, the preparation method of especially described composition capsule.
Background technology
Herba Andrographis is Acanthaceae Herba Andrographis platymiscium.Main component has lactone, sterol, flavone, alkaloid etc.Its bitter in the mouth, cold in nature, GUIXIN, lung, large intestine, urinary bladder channel.There is heat-clearing and toxic substances removing, the effect of removing heat from blood detumescence.Be usually used in treatment flu clinically, tonsillitis, bronchitis, acute bacillary dysentery, the multi-infection diseases such as gastroenteritis.
Radix Wikstroemae is Isolated From Thymelaeaceae Species, and research finds containing wikstroemin, Flos Wikstroemiae Dolichanthae element, Hydroxygenkwanin, the compositions such as daphnoretin, arctigenin-4'-gentiobioside, wickstromol, Luo Hong pinoresinol, (+)-Pinoresinol, cupreol, polysaccharide, acidic resins, volatile oil, saponin.Radix Wikstroemae beginning of being used as medicine is loaded in " south of the Five Ridges gather medicinal herbs record ", and it is cold in nature, bitter in the mouth, micro-pungent, poisonous, and enter lung, Liver Channel, function heat-clearing and toxic substances removing, dissipating blood stasis is relieved oedema or abdominal distension through diuresis or purgation.Be widely used in the diseases such as bronchitis, pneumonia, parotitis, lymphadenitis, rheumatalgia, advanced schistosomiasis ascites, furuncle carbuncle.
The compositions that Herba Andrographis and Radix Wikstroemae two taste Chinese medicine form, its function cures mainly as eliminating inflammation and expelling toxin; Breathe heavily for expectorant heat syndrome cough, stomachache, and acute and chronic tonsillitis, pharyngolaryngitis, pneumonia, acute gastroenteritis, acute bacillary dysentery are shown in above symptom; Make tablet or capsule application more, be called Chuanwang anti-inflammation sheet, antiphlogistic Chunwang capsule.But, the Chuanwang anti-inflammation sheet used clinically at present or antiphlogistic Chunwang capsule, Herba Andrographis, Radix Wikstroemae all adopt traditional solvent thermal circumfluence method to extract, consume a large amount of solvent, extraction time long (four hours or longer consuming time of general extraction palpus), cause energy consumption high, the production cycle is long; And extraction efficiency is low, extraction ratio and effective ingredient extraction rate all low.
Dynamic countercurrent extraction technology, be that a kind of Chinese crude drug of dynamic extraction and countercurrent extraction technology being combined extracts new technique, treasury got, percolation, dynamically and reverse flow technique be integrated.This technology is by plural dynamic extraction pot units connected in series, increase mass transfer force, make full use of the effective ingredient Concentraton gradient between solvent and medical material, step by step effective ingredient in medical material is diffused in the relatively low solvent of initial concentration, make effective ingredient stripping to greatest extent, have that Extracting temperature is low, extraction efficiency is high, solvent load is few, concentrated low power consumption and other advantages.There is not yet the report that dynamic countercurrent extraction technology is applied to Herba Andrographis, Radix Wikstroemae compositions is extracted so far.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides the preparation method of the Chinese medicine composition for diminishing that a kind of Herba Andrographis and Radix Wikstroemae form.Described preparation method adopts dynamic countercurrent extraction technology, not only reduces solvent load, reduces Extracting temperature, and substantially reduces extraction time, improve extraction efficiency.
For realizing above-mentioned technical purpose, present invention employs following technical scheme:
A preparation method for Chinese medicine composition for diminishing, the raw material of described Chinese medicine composition consists of Herba Andrographis and Radix Wikstroemae; Described Herba Andrographis and Radix Wikstroemae adopt dynamic countercurrent extraction, and described preparation method comprises the steps:
1) get Herba Andrographis, be ground into coarse powder, drop into the dynamic countercurrent extraction device that five sections are extracted pipeline section, the ethanol consumption 4-10ml/g of 75-95%, Extracting temperature 65-85 DEG C, every section of extraction time 30-90min, merge extractive liquid, filter, obtain filtrate I;
2) get Radix Wikstroemae, drop into the dynamic countercurrent extraction device that five sections are extracted pipeline section, water consumption 6-10ml/g, Extracting temperature 90-100 DEG C, every section of extraction time 30-50min, merge aqueous extract, filter, obtain filtrate II;
3) the filtrate I that obtains of described step 1) and step 2) filtrate II that obtains, be condensed into clear paste respectively, merge, drying under reduced pressure, obtains dry cream, or concentrated after merging, and drying under reduced pressure, obtains dry cream; Add or do not add pharmaceutically acceptable adjuvant, obtain described Chinese medicine composition.
In described step 1), preferred process conditions are: the ethanol consumption 10ml/g of 75%, Extracting temperature 75 DEG C, every section of extraction time 30min.
Described step 2) in, preferred process conditions are: water consumption 8ml/g, Extracting temperature 100 DEG C, every section of extraction time 30min.
Preferably, raw material of the present invention consists of Herba Andrographis 24 weight portion and Radix Wikstroemae 16 weight portion.
The present invention also provides a kind of Herba Andrographis and Radix Wikstroemae to be the preparation method of the eliminating inflammation and expelling toxin Chinese medicine capsules of raw material.
The raw material composition of described Chinese medicine capsules comprises Herba Andrographis 2400g, Radix Wikstroemae 1600g, and described preparation method comprises the steps:
1) Herba Andrographis 2400g is got, be ground into coarse powder, drop into the dynamic countercurrent extraction device that five sections are extracted pipeline section, 75% ethanol consumption is 10ml/g, Extracting temperature 75 DEG C, every section of extraction time 30min, merge extractive liquid, leaves standstill, filter, decompression filtrate recycling ethanol, to without alcohol taste, continues to be concentrated into the clear paste that relative density is 1.20-1.30, for subsequent use;
2) get Radix Wikstroemae 1600g, drop into the dynamic countercurrent extraction device that five sections are extracted pipeline section, water consumption 10ml/g, Extracting temperature 100 DEG C, every section is extracted 30min, merges aqueous extract liquid, filters, obtains filtrate;
3) described step 2) clear paste that obtains of the filtrate that obtains and described step 1) merges, the thick paste of relative density 1.35-1.40 when being concentrated into 85 DEG C, drying under reduced pressure, obtains dry cream, adds pharmaceutically acceptable adjuvant, use 75% alcohol granulation, oven drying at low temperature, granulate, encapsulated, make 1000, to obtain final product.
The consumption (ml/ g) of Extraction solvent of the present invention, refers to the solvent volume needed for every gram of medical material.
The Chinese medicine composition of eliminating inflammation and expelling toxin of the present invention, adds applicable pharmaceutically acceptable adjuvant, can be prepared into injection or oral formulations, preferably oral formulations, as tablet, and capsule, granule, electuary etc.For oral formulations, pharmaceutically acceptable adjuvant, can be selected from one or more in starch, lactose, glucose, microcrystalline cellulose, sodium carboxymethyl cellulose etc.
Dynamic pot group type countercurrent extraction technology is a kind of Chinese medicine extraction new technique dynamic extraction and countercurrent extraction technology combined, this technology makes full use of the effective ingredient Concentraton gradient between solvent and medical material, step by step effective ingredient in medical material is diffused in the relatively low solvent of initial concentration, make effective ingredient stripping to greatest extent, have that Extracting temperature is low, extraction efficiency is high, solvent load is few, concentrated low power consumption and other advantages.Affect the factor more complicated of dynamic countercurrent extraction, in order to Optimization Technology, inventors performed following research.
One, extraction equipment
Adopt five sections of dynamic countercurrent extraction devices extracting pipeline section.
Two, Herba Andrographis dynamic countercurrent extraction technique
Adopt Orthogonal Experiment and Design, with andrographolide yield for optimization aim, investigate the key factors such as concentration of alcohol, solvent load, every period of extraction time and Extracting temperature to the impact of optimization aim, obtain optimal processing parameter.And dynamic pot group type countercurrent extraction technique and circumfluence distillation technique are compared, fully manifested dynamic pot group type countercurrent extraction technique saving solvent, improve extraction ratio, to enhance productivity etc. in advantage.
2.2 methods and result:
2.2.1 the determination of factor level
The factor of orthogonal test and level see the following form 1.
Table 1 Herba Andrographis dynamic countercurrent extraction factor level
。
2.2.2 the Orthogonal Experiment and Design of dynamic pot group type countercurrent extraction technique
Accurately take Herba Andrographis medical material 9 parts, each 50kg, carry out dynamic countercurrent extraction by L9 (34) orthogonal test designs table.Extraction terminates rear merge extractive liquid, measures volume, sample analysis.
2.2.3 the HPLC method of andrographolide measures
2.2.3.1 chromatographic condition
Chromatographic column is C18 post; Mobile phase is methanol-water (50: 50); Determined wavelength 250 nm; Column temperature 30 DEG C; Volume flow 1. 0 mL/m in; Sampling volume 10 μ L.
2.2.3.2 the preparation of reference substance solution
It is appropriate that precision takes andrographolide reference substance, adds the solution that 60% methanol is mixed with 0.1mg/mL, to obtain final product.
2.2.3.3 the preparation of need testing solution
Precision measures sample solution 10 mL, evaporate to dryness, and residue adds 60% methanol 30 mL supersound process 30 minutes, and let cool, the methanol adding 60% is diluted to scale in right amount, shakes up, and filters, to obtain final product with 0.45 μm of filter membrane.
2.2.3.4 the preparation of standard curve
Get andrographolide reference substance solution, sample introduction 2,5,15,25,35,50 μ L analyzes respectively.Take chromatographic peak area as vertical coordinate, sample size is abscissa, and drawing standard curve obtains standard curve equation:
Y = 2 864 X - 27. 4, r = 0. 999 99。
2.2.3.5 measure
Get need testing solution and reference substance solution appropriate, sample introduction measures, and adopts external standard method to calculate.
2.2.3.6 orthogonal experiments and analysis
With L9 (3) orthogonal test designs table, with andrographolide yield for evaluation index, the results are shown in Table 2.
Quality × 100% of andrographolide quality/Herba Andrographis medical material in andrographolide yield=extracting solution
Table 2 Herba Andrographis dynamic countercurrent extraction technique orthogonal experiments
| Test number | A | B | C | D | Cumulative volume (L) | Andrographolide yield (%) |
| 1 | 1 | 1 | 3 | 1 | 200 | 0.28 |
| 2 | 1 | 2 | 2 | 3 | 300 | 0.30 |
| 3 | 1 | 3 | 1 | 2 | 500 | 0.67 |
| 4 | 2 | 1 | 2 | 3 | 200 | 0.35 |
| 5 | 2 | 2 | 3 | 1 | 300 | 0.27 |
| 6 | 2 | 3 | 1 | 2 | 500 | 0.23 |
| 7 | 3 | 1 | 3 | 2 | 200 | 0.29 |
| 8 | 3 | 2 | 1 | 3 | 300 | 0.41 |
| 9 | 3 | 3 | 2 | 1 | 500 | 0.35 |
| Average 1 | 0.187 | 0.267 | 0.327 | 0.200 | —— | —— |
| Average 2 | 0.283 | 0.357 | 0.343 | 0.243 | —— | —— |
| Average 3 | 0.430 | 0.277 | 0.230 | 0.457 | —— | —— |
| Extreme difference | 0.243 | 0.090 | 0.113 | 0.257 | —— | —— |
Orthogonal test gained andrographolide yield is analyzed, adopts the difference of twice parallel test as source of error.Intuitive analysis from table 2, the significance of 4 factors to andrographolide yield is different.Concentration of alcohol and Extracting temperature have significance for andrographolide yield, and solvent load, extraction time are not remarkable on the impact of andrographolide yield.And the result that variance analysis (see table 3) obtains is similar to intuitive analysis result, obtaining optimal extract process is: A
1b
3c
1d
2, i.e. concentration of alcohol 75 %, ethanol consumption is 10ml/g, and every period of extraction time is 30min, and Extracting temperature is 75 DEG C.Under this optimum process condition, carry out twice parallel test, experiment repeatability is better, the results are shown in Table 4.
Table 3 variance analysis
| Soruces of variation | Sum of square of deviations | Degree of freedom | Average deviation's quadratic sum | F value | Significance |
| A | 0.0901 | 2 | 0.0451 | 4.5033 | P<0.05 |
| B | 0.0146 | 2 | 0.0073 | 0.7300 | P<0.05 |
| C | 0.0183 | 2 | 0.0091 | 0.9150 | P<0.05 |
| D | 0.1133 | 2 | 0.0567 | 5.6633 | P<0.05 |
Twice parallel verified test under table 4 Herba Andrographis dynamic countercurrent extraction optimised process
| Test | Andrographolide yield (%) | Extractum yield (%) |
| 1 | 1.95 | 4.09 |
| 2 | 1.97 | 4.07 |
2.2.4 the comparison of Different Extraction Method:
Heat reflow method: at extraction pot in-built 50kg Herba Andrographis medical material, adds 500 L 75% ethanol, after 80-85 DEG C of backflow 2 h, medical material and extracting solution is filtered after being separated, obtains extracting solution 1; In medicinal residues, add 500 L 75% ethanol, after continuing backflow 2 h, obtain extracting solution 2; Merge extractive liquid, 1,2, measures the yield of the andrographolide in merge extractive liquid.
Infusion process: take 50kg Herba Andrographis medical material, adds airtight 2 h of 70% ethanol of a times amount.Medical material is loaded in percolator, slowly add 75% ethanol from percolator top, reach 10ml/g to consumption, flood.Open percolator end opening after dipping, carry out percolation with certain flow velocity, collect and obtain percolate 500 L, used time 6h, measure the yield of the andrographolide in extracting solution.
Soxhlet extraction: take Herba Andrographis medical material 50kg, be placed in apparatus,Soxhlet's, adds 75% ethanol 500L and extracts 8 h in 85 DEG C, measure the yield of the andrographolide in extracting solution.Hot reflux, percolation, surname extraction technique and dynamic pot group type countercurrent extraction Herba Andrographis technique are compared, the results are shown in Table 5.
Compared with Soxhlet Effect of Alcohol Extracting Procedureto Total, the extraction ratio of dynamic pot group type countercurrent extraction technique slightly declines, but the solvent-oil ratio of unit medical material reduces 38. 6%, and extraction time is more the reduction of 87. 3%; Compared with seepage pressure effects technique, when unit medical material solvent-oil ratio is identical, the andrographolide extraction ratio of dynamic pot group type countercurrent extraction technique improves 27. 1%.The extraction time of medical material saves 89%; Compared with circumfluence distillation technique, the andrographolide extraction ratio of dynamic pot group type countercurrent extraction technique improves 13.2%, and the solvent-oil ratio of unit medical material reduces 50%, and the extraction time of unit medical material saves 88%.Visible, the sharpest edges of pot group type countercurrent extraction technique are greatly to save Extraction solvent, shorten extraction time, reduce the energy consumption that subsequent evaporation is concentrated, can ensure higher extraction efficiency again, lower Extracting temperature simultaneously.
The comparison of table 5 Herba Andrographis Different Extraction Method
| Extracting method | Andrographolide yield (%) | Extractum (g/ml) |
| Hot reflux | 1.74 | 2.59 |
| Diafiltration | 1.72 | 1.41 |
| Soxhlet extraction | 2.05 | 3.13 |
| Dynamic countercurrent | 1.96 | 4.06 |
The dynamic pot group type countercurrent extraction technological parameter of this research and utilization Orthogonal Optimization Test method to Herba Andrographis medical material is optimized research, and optimum process condition is: 75% ethanol extraction, ethanol consumption 10ml/g, every section of extraction time 30 min, Extracting temperature 75 DEG C.And dynamic pot group type countercurrent extraction technique is compared with hot reflux, percolation, surname extraction technique, when ensureing higher yields, greatly save Extraction solvent, reduce the energy consumption of subsequent evaporation concentration process, fully demonstrating the advantage of dynamic pot group type countercurrent extraction, is a kind of efficient, energy-conservation new technique.
Three, Radix Wikstroemae dynamic countercurrent extraction
3.1 influence factors determine: at present, the extraction process of Radix Wikstroemae medical material mainly adopts extraction process by water.The solvent load of every kilogram of medical material is about 100 L, and extraction time reaches ten hours, there is the shortcomings such as solvent load is large, the time is long, temperature is high and extraction efficiency is low, energy consumption is high.This research adopts Orthogonal Experiment and Design, is optimized the dynamic pot group type countercurrent extraction technological parameter of wickstoemin in Radix Wikstroemae medical material.With wickstoemin yield for optimization aim, investigate the key factors such as water consumption, every period of extraction time and Extracting temperature to the impact of optimization aim, obtain optimal processing parameter.And dynamic pot group type countercurrent extraction technique and circumfluence distillation technique are compared, fully manifested dynamic pot group type countercurrent extraction technique saving solvent, improve extraction ratio, to enhance productivity etc. in advantage.
3.2 methods and result:
3.2.1 the determination of factor level
The factor of orthogonal test and level see the following form 6.
Table 6 Radix Wikstroemae dynamic countercurrent extraction factor level
。
3.2.2 the Orthogonal Experiment and Design of dynamic pot group type countercurrent extraction technique
Accurately take Radix Wikstroemae medical material 9 parts, each 50kg, by orthogonal test L9 (3) design table, carry out dynamic countercurrent extraction.Extraction terminates rear merge extractive liquid, measures volume, sample analysis.
3.2.3 the H PL C method of wickstoemin measures
3.2.3.1 chromatographic condition: chromatographic column is C 18 post; Mobile phase is methanol-water (50: 50); Determined wavelength 252 nm; Column temperature 30 DEG C; Volume flow 1. 0 mL/m in; Sampling volume 10 μ L.
3.2.3.2 the preparation of reference substance solution: it is appropriate that precision takes wickstoemin reference substance, adds the solution that 50% methanol is mixed with 0.1mg/mL, to obtain final product.
3.2.3.3 the preparation of need testing solution: precision measures sample solution 10 mL, evaporate to dryness, residue adds 50% methanol 30 mL supersound process 30 minutes, and let cool, the methanol adding 50% is diluted to scale in right amount, shakes up, and filters, to obtain final product with 0.45 μm of filter membrane.
3.2.3.4 the preparation of standard curve: get wickstoemin reference substance solution, sample introduction 2,5,15,25,35,50 μ L analyzes respectively.Take chromatographic peak area as vertical coordinate, sample size is abscissa, and drawing standard curve obtains standard curve equation
Y = 2 349 X - 23. 6, r = 0. 999 99。
3.2.3.5 measure: it is appropriate to get need testing solution and reference substance solution, and sample introduction measures, and adopts external standard method to calculate.
3.2.3.6 orthogonal experiments and analysis: with L9 (3) orthogonal test designs table, with wickstoemin yield () for evaluation index, the results are shown in Table 7.
Quality × 100% of wickstoemin quality/Radix Wikstroemae medical material in wickstoemin yield=extracting solution
Table 7 Radix Wikstroemae dynamic countercurrent extraction orthogonal experiments
。
Orthogonal test gained wickstoemin yield is analyzed, adopts the difference of twice parallel test as source of error.Intuitive analysis from table 7, the significance of 3 factors to wickstoemin yield is different.Solvent load and Extracting temperature have significance for wickstoemin yield, and unit extraction time is not remarkable on the impact of wickstoemin yield.And the result that variance analysis (see table 8) obtains is similar to intuitive analysis result, obtaining optimal extract process is: A
3b
1c
3, namely water consumption is 8ml/g, and every period of extraction time is 30min, and Extracting temperature is 100 DEG C.Under this optimum process condition, carry out twice parallel test, experiment repeatability is better, the results are shown in Table 9.
Table 8 variance analysis
| Soruces of variation | Sum of square of deviations | Degree of freedom | Average deviation's quadratic sum | F value | Significance |
| A | 0.0803 | 2 | 0.0402 | 4.2013 | P<0.05 |
| B | 0.0130 | 2 | 0.0065 | 0.7100 | P<0.05 |
| C | 0.0162 | 2 | 0.0081 | 0.8360 | P<0.05 |
Twice parallel verified test under table 9 Radix Wikstroemae dynamic countercurrent extraction optimised process
| Test | Wickstoemin yield (%) | Extractum yield (%) |
| 1 | 1.61 | 5.63 |
| 2 | 1.59 | 5.57 |
3.2.4 the comparison of Different Extraction Method:
Heat reflow method: at extraction pot in-built 50kg Radix Wikstroemae medical material, after adding soak by water 2 h of 8 times amount, filters medical material and extracting solution after being separated, obtains extracting solution 1; In medicinal residues, add the water of 8 times amount, after continuing decoction 2 h, obtain extracting solution 2; Merge extractive liquid, 1,2, measures the yield of the wickstoemin in merge extractive liquid.
Water extraction process and dynamic pot group type countercurrent extraction Herba Andrographis technique are compared, the results are shown in Table 10.
Compared with water extraction process, the wickstoemin extraction ratio of dynamic pot group type countercurrent extraction technique improves 50%, and the solvent-oil ratio of unit medical material is constant, and the extraction time of unit medical material saves 50%.Visible, the sharpest edges of pot group type countercurrent extraction technique are greatly to save Extraction solvent, shorten extraction time, reduce the energy consumption that subsequent evaporation is concentrated, can ensure higher extraction efficiency again simultaneously.
Table 10 Radix Wikstroemae Different Extraction Method compares
| Extracting method | Wickstoemin yield (%) | Extractum (g/ml) |
| Water extraction | 1.07 | 3.18 |
| Dynamic countercurrent | 1.60 | 5.60 |
The dynamic pot group type countercurrent extraction technological parameter of this research and utilization Orthogonal Optimization Test method to Radix Wikstroemae medical material is optimized research, and optimum process condition is: water consumption; 8 times of medical material amounts, carry time 30min for every section, Extracting temperature 100 DEG C.And dynamically pot group type countercurrent extraction technique, compared with water extraction process, when ensureing higher yields, greatly saving extraction time, fully demonstrating the advantage of dynamic pot group type countercurrent extraction.
Detailed description of the invention
Below by embodiment and comparative example, the present invention will be further described.
Embodiment 1 one kinds of antiinflammatory toxin resolving capsules
Raw material composition comprises Herba Andrographis 2400g, Radix Wikstroemae 1600g, prepares as follows:
1) Herba Andrographis 2400g is got, be ground into coarse powder, drop into the dynamic countercurrent extraction device that five sections are extracted pipeline section, 75% ethanol consumption is 10ml/g, Extracting temperature 75 DEG C, every section of extraction time 30min, merge extractive liquid, leaves standstill, filter, decompression filtrate recycling ethanol, to without alcohol taste, continues to be concentrated into the clear paste that relative density is 1.20-1.30, for subsequent use;
2) get Radix Wikstroemae 1600g, drop into the dynamic countercurrent extraction device that five sections are extracted pipeline section, water consumption 10ml/g, Extracting temperature 100 DEG C, every section of extraction time 30min, merge aqueous extract liquid, filter, obtain filtrate;
3) described step 2) clear paste that obtains of the filtrate that obtains and described step 1) merges, the thick paste of relative density 1.35-1.40 when being concentrated into 85 DEG C, and drying under reduced pressure, obtains dry cream, add starch, use 75% alcohol granulation, oven drying at low temperature, granulate, encapsulated, make 1000, to obtain final product.
Embodiment 2 one kinds of eliminating inflammation and expelling toxin sheets
Raw material composition comprises Herba Andrographis 2000g, Radix Wikstroemae 1500g, prepares as follows:
1) Herba Andrographis 2000g is got, be ground into coarse powder, drop into the dynamic countercurrent extraction device that five sections are extracted pipeline section, 85% ethanol consumption is 6ml/g, Extracting temperature 85 DEG C, every section of extraction time 60min, merge extractive liquid, leaves standstill, filter, decompression filtrate recycling ethanol, to without alcohol taste, continues to be concentrated into the clear paste that relative density is 1.20-1.30, for subsequent use;
2) get Radix Wikstroemae 1000g, drop into the dynamic countercurrent extraction device that five sections are extracted pipeline section, water consumption 8ml/g, Extracting temperature 90 DEG C, every section of extraction time 60min, merge aqueous extract liquid, filter, obtain filtrate;
3) described step 2) clear paste that obtains of the filtrate that obtains and described step 1) merges, the thick paste of relative density 1.35-1.40 when being concentrated into 85 DEG C, and drying under reduced pressure, obtains dry cream, add microcrystalline cellulose, use 75% alcohol granulation, oven drying at low temperature, tabletting, makes 1000, to obtain final product.
Embodiment 3 one kinds of eliminating inflammation and expelling toxin electuaries
Raw material composition comprises Herba Andrographis 2400g, Radix Wikstroemae 2000g, prepares as follows:
1) Herba Andrographis 2400g is got, be ground into coarse powder, drop into the dynamic countercurrent extraction device that five sections are extracted pipeline section, 95% ethanol consumption is 4ml/g, Extracting temperature 65 DEG C, every section of extraction time 90min, merge extractive liquid, leaves standstill, filter, decompression filtrate recycling ethanol, to without alcohol taste, continues to be concentrated into the clear paste that relative density is 1.20-1.30, for subsequent use;
2) get Radix Wikstroemae 2000g, drop into the dynamic countercurrent extraction device that five sections are extracted pipeline section, water consumption 6ml/g, Extracting temperature 95 DEG C, extract 50min/ section, merge aqueous extract liquid, filter, obtain filtrate;
3) described step 2) clear paste that obtains of the filtrate that obtains and described step 1) merges, the thick paste of relative density 1.35-1.40 when being concentrated into 85 DEG C, and drying under reduced pressure, obtains dry cream, add starch and glucose, use 75% alcohol granulation, oven drying at low temperature, pack, every bag of 4g, to obtain final product.
The drug effect of Chinese medicine composition for diminishing prepared by comparative example two kinds of techniques compares
One, tested material
1) the described dry cream of embodiment 1 preparation, hereinafter referred to as " new process combination thing "
2) Chinese medicine composition for diminishing prepared of solvent thermal circumfluence method, hereinafter referred to as " old process combination thing ", prepare by the following method:
(1) get Herba Andrographis 2400g, be ground into coarse powder, add the ethanol heating extraction secondary of 6 times amount 85%, each 2 hours, merge extractive liquid, leave standstill, filter, decompression filtrate recycling ethanol, to without alcohol taste, continues to be concentrated into the clear paste that relative density is 1.20-1.30, for subsequent use;
(2) get Radix Wikstroemae 1600g, add 8 times amount soak by water secondaries, each 3 hours, collecting decoction, filter, obtain filtrate;
(3) described step 2) clear paste that obtains of the filtrate that obtains and described step 1) merges, and the thick paste of relative density 1.35-1.40 when being concentrated into 85 DEG C, drying under reduced pressure, obtains dry cream, to obtain final product.
Two, the impact of xylol induced mice ear swelling
Get Jiangxi kind white mice 72; Body weight 18g-22g, each 36 of male and female, be divided into 6 groups at random, often organize 12, i.e. model control group, old process combination thing group, the basic, normal, high dosage group of positive drug Dexamethasone group, new process combination thing, each group is oral administration (model control group is to the distilled water of same volume), and administration volume is 30ml/kg, once a day, successive administration four days, concrete administration and grouping situation refer to table 11.Namely last administration rear left ear is coated with dimethylbenzene 0.03ml, after 2 hours, cervical dislocation is put to death, the ears sheet at same position is laid respectively with the card punch of 9mm, ten thousand/analytical balance is used to weigh immediately, left ear deducts auris dextra sheet as swelling, and calculates its inhibitory rate of intumesce, carries out statistical procedures, more each administration group with the diversity of model control group, the results detailed in Table 11.The computing formula of inhibitory rate of intumesce is as follows:
Inhibitory rate of intumesce=(the average swelling of model group-average swelling of administration group) average swelling × 100% of ÷ model group
the impact (X ± S) of the mice ear caused by table 11 different process compositions xylol
Note: with model control group ratio, *: P < 0.05; *: P < 0.01;
The above results shows, each treatment group is compared with model group respectively, and the mice ear that xylol causes has obvious inhibitory action, and three dosage groups of new process combination thing exist obvious dose-effect relationship; New process combination thing is obviously better than old technique to the inhibitory action of mice ear, and effective dose is low.
Two, on the impact of mouse peritoneal capillary permeability
Get Jiangxi kind white mice 60; Body weight 18g-22g, each 30 of male and female, be divided into 6 groups at random, often organize 10, i.e. model control group, old technique group, the basic, normal, high dosage group of positive drug Dexamethasone group, new technology, each group is oral administration (model control group is to the distilled water of same volume), and administration volume is 30ml/kg, once a day, successive administration four days, concrete administration and grouping situation refer to table 12.After last administration 30min, to mouse tail vein iv0.5% normal saline 0.1ml/10g; Lumbar injection 0.7% acetic acid 0.2ml/ only immediately, put to death on time after 10 minutes, abdominal cut leather belly and muscle, divide with 5ml normal saline and wash abdominal cavity four times, sucking-off cleaning mixture, 3000r/min, centrifugal 15 minutes, gets supernatant, absorbance is measured at 590nm wavelength place with uv2450 ultraviolet spectrophotometer, carry out statistical procedures, respectively organize medicine with the diversity of model group, refer to table 12.
table 12 different process compositions is on the impact (X ± S) of mouse peritoneal capillary permeability
| Group | Number of animals (n) | Dosage (g/kg) | Mus ear swelling degree (mg) |
| Model group | 10 | — | 0.294±0.086 |
| New process combination thing high dose group | 10 | 0.78 | 0.184±0.057** |
| Dosage group in new process combination thing | 10 | 0.39 | 0.229±0.056* |
| New process combination thing low dose group | 10 | 0.19 | 0.236±0.054* |
| Old process combination thing group | 10 | 4.68 | 0.196±0.071** |
| Dexamethasone group | 10 | 3.12mg | 0.149±0.036** |
Note: with model control group ratio, *: P < 0.05; *: P < 0.01;
The above results shows, each treatment group is compared with model group respectively, has increasing of the mouse peritoneal permeability significantly suppressing acetic acid to cause; New process combination thing presents certain dose-effect relationship; New process combination thing is obviously better than old technique to the influence of mouse peritoneal capillary permeability, and effective dose is low.。
Three, conclusion
Adopt described Chinese medicine composition for diminishing prepared by dynamic filling group formula countercurrent extraction technique of the present invention, antiinflammatory action is obviously better than compositions prepared by traditional circumfluence distillation technique.
Claims (2)
1. a preparation method for Chinese medicine composition for diminishing, the raw material of described Chinese medicine composition consists of Herba Andrographis and Radix Wikstroemae; It is characterized in that: described Herba Andrographis and Radix Wikstroemae adopt dynamic pot group type countercurrent extraction, and described preparation method comprises the steps:
1) get Herba Andrographis, be ground into coarse powder, drop into the dynamic countercurrent extraction device that five-part form extracts pipeline section, the ethanol consumption 10ml/g of 75%, Extracting temperature 75 DEG C, every section of extraction time 30min, merge extractive liquid, filter, obtain filtrate I;
2) get Radix Wikstroemae, drop into the dynamic countercurrent extraction device that five-part form extracts pipeline section, water consumption 8ml/g, Extracting temperature 100 DEG C, every section of extraction time 30min, merge aqueous extract, filter, obtain filtrate II;
3) the filtrate I that obtains of described step 1) and step 2) filtrate II that obtains, be condensed into clear paste respectively, merge, drying under reduced pressure, obtains dry cream, or concentrated after merging, and drying under reduced pressure, obtains dry cream; Add or do not add pharmaceutically acceptable adjuvant, obtain described Chinese medicine composition.
2. preparation method according to claim 1, is characterized in that: described raw material consists of Herba Andrographis 24 weight portion and Radix Wikstroemae 16 weight portion.
3. a preparation method for eliminating inflammation and expelling toxin Chinese medicine capsules, the raw material of described Chinese medicine capsules consists of Herba Andrographis 2400g, and Radix Wikstroemae 1600g, is characterized in that: described preparation method comprises the steps:
1) get Herba Andrographis 2400g, be ground into coarse powder, drop into the dynamic countercurrent extraction device that five-part form extracts pipeline section, 75% ethanol consumption is 10ml/g, Extracting temperature 75 DEG C, every section of extraction time 30min.Merge extractive liquid, leaves standstill, and filters, and decompression filtrate recycling ethanol, to without alcohol taste, continues to be concentrated into the clear paste that relative density is 1.20-1.30, for subsequent use;
2) get Radix Wikstroemae 1600g, drop into the dynamic countercurrent extraction device that five-part form extracts pipeline section, water consumption 10ml/g, Extracting temperature 100 DEG C, every section of extraction time 30min, merge aqueous extract liquid, filter, obtain filtrate;
3) described step 2) clear paste that obtains of the filtrate that obtains and described step 1) merges, be concentrated into the thick paste of 85 DEG C of relative density 1.35-1.40, drying under reduced pressure, obtains dry cream, adds pharmaceutically acceptable adjuvant, use 75% alcohol granulation, oven drying at low temperature, granulate, encapsulated, make 1000, to obtain final product.
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