CN1330348C - Gynecoiatry leukorrhea stopping capsule and its preparation technology - Google Patents
Gynecoiatry leukorrhea stopping capsule and its preparation technology Download PDFInfo
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Abstract
The present invention relates to a gynecoiatry leukorrhea stopping capsule and a preparation technology thereof. The auxiliary materials of the capsule are starch or dextrin or the starch and the dextrin. The weight ratio of active ingredients to auxiliary materials of medicine is 2.8 to 4:1. The present invention is a gynecoiatry leukorrhea stopping capsule which has stable and reliable quality and moisture performance can cover the bitterness of original medicine, shorten disintegration time limit and generate good economic benefit. The present invention also provides a preparation process of the gynecoiatry leukorrhea stopping capsule, which has perfect process, is favorable to sufficiently reserve effective ingredients and saves cost; the preparation process can industrially produce the capsule on a large scale.
Description
Technical field
The present invention relates to employed Chinese medicinal capsule of a kind of gynaecopathia and preparation method thereof.
Background technology
FUKE ZHIDAI PIAN is that a kind of clinical practice is extensive, has the treatment chronic cervicitis of certain curative effect, the Chinese medicine preparation of the damp-heat type red and white leukorrhea disease that endometritis, encolpitis etc. cause.But this Chinese medicine preparation belongs to tablet, and patient takes the sensation bitter in the mouth, usually can feel to be difficult to swallow, and disintegration time is long, is unfavorable for the quick stripping of effective ingredient, and onset is slow.The dosage form of its single tablet also makes doctor and the nonoptional leeway of patient.And original method for making is: Cortex Ailanthi decocts with water secondary, and each 2 hours, collecting decoction filtered, and filtrate is concentrated in right amount, adds ethanol and makes and contain the alcohol amount and be about 50%, leaves standstill filtration.Cortex Phellodendri is with 85% alcohol reflux three times, and each 1.5 hours, merge extractive liquid, filtered.Poria 60% ethanol, Fructus Schisandrae Chinensis, Rhizoma Dioscoreae are used 45% ethanol, carry out percolation according to the percolation (an appendix I of Chinese Pharmacopoeia version in 2000 O) under fluid extract and the extractum item.More than each liquid reclaim ethanol respectively and be condensed into thick paste.The Carapax et Plastrum Testudinis water embathes except that the fleshing bits, decocts with water secondary, and each 6 hours, collecting decoction filtered, and filtrate is condensed into gluey thick paste; Filtering residue dries, and is ground into coarse powder, with 10% acetic acid dipping, filters the filtrate evaporate to dryness.Colla Corii Asini is ground into fine powder after with stir-baked in powder of CONCHA MERETRICIS SEU CYCLINAE, sieves, and with above-mentioned each thick paste and acetic acid extractum mixing, adds right amount of auxiliary materials, and drying is pulverized, and incapsulates, and makes 1000 approximately, promptly.There is not specific description at a lot of preparation process conditions significantly.As extract in the Cortex Ailanthi, double the problem of the water yield in the extraction process by water; In the Cortex Phellodendri alcohol extraction technology, add doubly amount of alcohol, extraction time, soak time, or the like some problems all do not have suitable explanation.How to make technology of the present invention reach optimum state,, be still a good problem to study for the staff of the field of Chinese medicines.In addition, whether dosage form after the change and technology adapt to suitability for industrialized production, are still a unknown number for the Chinese medicine worker.
Summary of the invention
It is reliable that purpose of the present invention aims to provide a kind of more stable quality, has protection against the tide, and can cover former medicine bitterness, shortens disintegration, and can produce better economic benefit gynaecologic leucorrhea removing capsule.
Another purpose of the present invention aims to provide that a kind of to have technology more perfect, is more conducive to the abundant reservation of effective ingredient, and saves cost again, can carry out the capsular preparation technology of gynaecologic leucorrhea removing of large-scale industrial production.
The objective of the invention is to realize by following manner:
Capsule of the present invention is made up of active constituents of medicine and capsule adjuvant, described active constituents of medicine is made up of Cortex Ailanthi 363g, Fructus Schisandrae Chinensis 64g, Cortex Phellodendri 363g, Carapax et Plastrum Testudinis 242g, Poria 363g, Colla Corii Asini 120g, Rhizoma Dioscoreae 363g, it is characterized in that described capsule adjuvant is starch or dextrin, or starch and dextrin, the weight ratio of active constituents of medicine and adjuvant is 2.8-4: 1.
The best active constituents of medicine and the weight ratio scope of adjuvant are 3.9-4: 1, and described adjuvant is a dextrin.
The content of every capsules active constituents of medicine is 260-280mg, and adjuvant is 70-90mg.
The preferable content of every capsules active constituents of medicine is 270-280mg, and adjuvant is 70mg.
Consider that active constituents of medicine of the present invention belongs to the easy moisture absorption of pure dry extract, mobile poor, easy layering must add a certain amount of adjuvant in case moisture absorption, improve liquidity, and avoids layering.Thereby add starch, dextrin etc. and have moisture resistance and flowability preferably, so form the prescription of prescription ratio with starch, dextrin and medicated powder, the moisture absorption percentage rate of mensuration mixed powder, observation granulation situation and dry condition the results are shown in Table 0.
Hydroscopicity is measured: get a certain amount of above-mentioned dry extract and mixture powder, put the interior constant weight of phosphorus pentoxide desiccator 48 hours.The glass exsiccator that the bottom is filled the sodium chloride supersaturated solution is put into 25 ℃ constant incubator constant temperature 24 hours, and the relative humidity in this moment exsiccator is 75%.Put into dry extract or the mixture powder of thick about 2mm respectively in the weighing botle bottom of constant weight, accurately weighing is placed in the above-mentioned glass exsiccator (the weighing bottle cap is opened), in 25 ℃ of constant incubators preservations, regularly weighing (6,12,24,48,60 hours), be calculated as follows the moisture absorption percentage rate.
Table 0 supplementary product kind selection result table
| Dry extract medicated powder heavy (g) | Donkey-hide gelatin fine powder heavy (g) | Dextrin consumption (g) | Starch consumption (g) | Draw wet rate (%) | The granulation situation | Dry condition |
| 160 | 22.4 | |||||
| 160 | 120 | 70 | / | 13.5 | Not agglomerating, easily sieve | Caking |
| 160 | 120 | / | 70 | 15.1 | Agglomerating on a small quantity, be difficult for sieving | Caking |
| 160 | 120 | 35 | 35 | 14.6 | Not agglomerating, easily sieve | Caking |
The molten point of this product is lower, and when adopting above-mentioned several adjuvant to granulate drying, granule is met heat and all dissolved agglomerating, therefore, this product should not be granulated, and the prescription that adds dextrin can obviously improve the hygroscopicity of this product, so selecting dextrin for use is that adjuvant of the present invention is the best, it is encapsulated that powder is directly beaten in employing.
Another object of the present invention realizes by following manner:
A, Cortex Ailanthi decoct with water secondary, and each 2 hours, add for the first time 8 times of water gagings, add 7 times of water gagings for the second time, collecting decoction filters, and filtrate concentrates, and adds ethanol and makes that to contain the alcohol amount be 50%, leaves standstill, and filters.
B, Cortex Phellodendri add 85% alcohol reflux three times, each 1.5 hours, add for the first time 7 times of amounts, add 6 times of amounts for the second time, for the third time in 6 times of amounts, merge extractive liquid, filters.
C, Poria 60% ethanol, Fructus Schisandrae Chinensis and Rhizoma Dioscoreae 45% ethanol percolation, collecting the percolation liquid measure is 10 times of raw material doses.
D, Carapax et Plastrum Testudinis decoct with water secondary, and each 6 hours, add 6 times of water gagings for the first time, add 5 times of water gagings for the second time, filter, filtrate is condensed into gluey thick paste; Filtering residue dries, and is ground into coarse powder, with 3 times of amount 10% acetic acid dippings, filters the filtrate evaporate to dryness.
E, Colla Corii Asini with stir-baked in powder of CONCHA MERETRICIS SEU CYCLINAE after, be ground into fine powder, sieve.
F, above-mentioned each step is obtained being thick paste, mixing adds adjuvant, and is dry, pulverize, encapsulated.
Described adjuvant is starch or dextrin, or starch and dextrin.
Described A collecting decoction in the step filters, and it is 1.15 that filtrate is concentrated into relative density, adds ethanol and makes that to contain the alcohol amount be 50%, leaves standstill 10-14 hour.
Described C Poria 60% ethanol in the step, Fructus Schisandrae Chinensis and Rhizoma Dioscoreae 45% ethanol percolation, flow velocity is 5ml/min.
Described D flooded 10-14 hour with 3 times of amount 10% acetic acid in the step.
Described D flooded 12 hours with 3 times of amount 10% acetic acid in the step.
Gynaecologic leucorrhea removing capsule of the present invention can not make patient produce the sensation of bitter taste when taking, and have protection against the tide, and can cover the characteristics of former medicine bitterness, and the present invention helps the quick stripping of effective ingredient, and is rapid-action, and disintegration time is short.Can produce good economic benefit.By the present inventor's effort, active constituents of medicine and adjuvant are carried out effective proportioning, make more stable quality of the present invention reliable, can directly apply to large-scale industrial production.
Optimised process of the present invention is by the trial of inventor by repeatedly testing, and studies intensively to draw.Can obtain good economic benefit by enforcement of the present invention, save cost, make the active ingredient of medicine obtain more complete reservation, product quality has also promoted a class, can be patient, the doctor provides more medication better to select.
Illustrate respectively with regard to each processing step below.
One, Poria, is investigated the percolation extraction conditions so adopt with the percolation extraction respectively of 45% ethanol with 60% ethanol, Fructus Schisandrae Chinensis and Rhizoma Dioscoreae.
The investigation of Poria percolate collecting amount
Get three parts of Poria coarse granules, every part of 100g uses 60% ethanol respectively, floods to carry out percolation after 48 hours, and percolation speed 5ml/min collects 8 times, 10 times, 12 times percolates respectively, is concentrated into 100ml, measures yield of extract.
Yield of extract is measured precision and is measured above-mentioned medicinal liquid 10ml, puts in the evaporating dish that is dried to constant weight, puts in the water-bath behind the evaporate to dryness, in 105 ℃ of dryings 3 hours, in the dislocation exsiccator, cool off 30 minutes, accurately rapidly claims to decide weight, and the calculating yield of extract the results are shown in Table 1.
The investigation of table 1 percolate collecting amount is table as a result
| The percolation liquid measure | Extractum must be measured (g) | Yield of extract (%) |
| 8 | 10.32 | 10.32 |
| 10 | 12.26 | 12.26 |
| 12 | 12.78 | 12.78 |
By table 1 result as can be known, collect the percolate of 10 times of medical material amounts, yield of extract reaches 12.26%, collect the percolate of 12 times of medical material amounts, yield of extract is not significantly increased, so consider from saving time, save cost two aspects, selects the percolate collecting amount to be advisable with 10 times of medical material amounts.
Rhizoma Dioscoreae, Fructus Schisandrae Chinensis percolate collecting amount are investigated
Get three parts of Rhizoma Dioscoreae and Fructus Schisandrae Chinensis coarse granules, every part of 100g (getting Fructus Schisandrae Chinensis 16g, Rhizoma Dioscoreae 91g) in the prescription ratio, use 45% ethanol, flood and carry out percolation after 48 hours, percolation speed 5ml/min, collect 8 times, 10 times, 12 times percolates respectively, be concentrated into 100ml, measure yield of extract and schisandrin amount.
Yield of extract is measured precision and is measured above-mentioned medicinal liquid 10ml, puts in the evaporating dish that is dried to constant weight, puts evaporate to dryness in the water-bath, in 105 ℃ of dryings 3 hours, in the dislocation exsiccator, cool off 30 minutes, accurately rapidly claims to decide weight, calculating yield of extract.
The schisandrin assay is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With methanol-water (13: 7) is mobile phase; The detection wavelength is 250nm.Theoretical cam curve is calculated by schisandrin should be not less than 2000.
It is an amount of that the schisandrin reference substance is got in the preparation of reference substance solution, adds methanol and make the solution that contains 0.1mg among every 1ml, promptly.
The preparation of need testing solution is got percolate as need testing solution.
Chinese Magnolivine Fruit (crossing sieve No. three) 0.1g is got in the preparation of schisandra chinensis medicinal material need testing solution, and accurate the title decides, and puts in the 25ml measuring bottle, adds the about 20ml of methanol, supersound process (power 250W, frequency 20KHz) 20 minutes, take out, put coldly, add methanol to scale, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively above-mentioned need testing solution and each the 5 μ l of reference substance solution of drawing of algoscopy inject chromatograph of liquid, measure, and calculate, promptly.
Yield of extract and schisandrin quantitative determination the results are shown in Table 2.
Table 2 percolate collecting amount is investigated table as a result
| The percolation liquid measure | Extractum must be measured g | Yield of extract % | Schisandrin mg | Schisandrin rate of transform % |
| 8 | 6.37 | 5.95 | 41.6 | 61.9 |
| 10 | 8.46 | 7.91 | 49.8 | 74.1 |
| 12 | 8.62 | 8.06 | 50.4 | 75 |
Investigate the result as can be known by table 2, collect the percolate of 10 times of medical material amounts, yield of extract reaches 7.91%, and the schisandrin rate of transform reaches 74.1%; Collect the percolate of 12 times of medical material amounts, the yield of extract and the schisandrin rate of transform are not significantly increased, so consider from saving time, save cost two aspects, select the percolate collecting amount to be advisable with 10 times of medical material amounts.
This research is 0.42% with schisandra chinensis medicinal material schisandrin content.
Two, Cortex Ailanthi extraction process by water condition is preferred
Consumption to extraction solvent is investigated.
1, method is got Cortex Ailanthi medical material 100g, is the examination factor with the amount of water, and the dry extract yield is determined extraction process for investigating index.
2, dry extract yield determination method is got Cortex Ailanthi medical material 100g, decoct with water secondary, collecting decoction filters, filtrate is concentrated into small size, get certain volume, put in the evaporating dish of constant weight, put evaporate to dryness in the water-bath, again in 105 ℃ of dryings 3 hours, put in the exsiccator and cooled off 0.5 hour, precision is weighed, and is calculated as follows the dry extract yield.
3, add the selection that water doubly measures and get Cortex Ailanthi 100g, add the decocting that different medical materials doubly measure and boil secondary, each 2 hours, collecting decoction served as to investigate index with dried cream yield, preferably adds water and doubly measures, and the results are shown in Table 3.
Table 3 Cortex Ailanthi adds water and doubly measures investigation table as a result
| Amount of water (doubly) | 6 5 | 8 7 | 10 9 |
| Dried cream yield (%) | 5.24 | 6.89 | 6.95 |
The above results shows: Cortex Ailanthi adds 8 times of water gagings for the first time, adds 7 times of water gagings for the second time and decocts, and each 2 hours, dried cream yield increased few, determines that therefore the Cortex Ailanthi extracting method is: get Cortex Ailanthi and decoct with water secondary, add 8 times of amounts for the first time, add 7 times of amounts for the second time.
The Chinese toon severe edema due to hypofunction of the spleen is carried the preferred of back alcohol precipitation process condition
After Cortex Ailanthi decocted with water in the former technology, medicinal liquid was concentrated in right amount, added ethanol and made and contain alcohol amount and be about 50%, leave standstill, filter, in alcohol precipitation process, the dry extract yield of the relative density of medicinal liquid after to precipitate with ethanol is influential, therefore, the spissated relative density of medicinal liquid before adding ethanol is investigated.
1, method is the examination factor with the relative density of medicine liquid, and the dry extract yield is determined alcohol precipitation process for investigating index.
2, the assay method of dry extract yield is got Cortex Ailanthi medical material 100g, decoct with water secondary, add for the first time 8 times of water gagings, add 7 times of water gagings for the second time, each is 2 hours, collecting decoction, filter, filtrate is concentrated into certain relative density, and adding ethanol to medicinal liquid, to contain the alcohol amount be 50%, left standstill 12 hours, filter, filtrate recycling ethanol also is concentrated into small size, gets certain volume, put in the evaporating dish of constant weight, put evaporate to dryness in the water-bath,, put in the exsiccator cooling 0.5 hour again in 105 ℃ of dryings 3 hours, precision is weighed, and is calculated as follows the dry extract yield.
3, Cortex Ailanthi medical material 100g is got in the selection of relative density of medicine liquid, decocts with water secondary, adds 8 times of water gagings for the first time, add for the second time 7 times of water gagings, each 2 hours, collecting decoction, filter, filtrate is concentrated into certain relative density, and adding ethanol to medicinal liquid, to contain alcohol amount be 50%, left standstill 12 hours, filter, with dried cream yield serves as to investigate index, and preferred suitable relative density of medicine liquid the results are shown in Table 4.
Relative density after table 4 Chinese toon severe edema due to hypofunction of the spleen extract concentrates is investigated table as a result
| Relative density (60 ℃) | 1.05 | 1.10 | 1.15 |
| Dried cream yield (%) | 5.84 | 5.02 | 4.38 |
The above results shows: Chinese toon severe edema due to hypofunction of the spleen extract is concentrated into relative density (60 ℃ of surveys) 1.15 o'clock, dried cream yield is minimum, the purpose of considering alcohol precipitation process is in order to remove impurity, be advisable so that dried cream yield is low, therefore, before adding the alcohol precipitation, selecting the relative density (60 ℃ of surveys) after Chinese toon severe edema due to hypofunction of the spleen extract concentrates is 1.15.
The investigation of three Cortex Phellodendri alcohol extraction process conditions
1, factor level design
Cortex Phellodendri was with 85%7 pure heating extraction three times, each 1.5 hours in the former tablet technology.Add 85% ethanol doubly amount, soak time, extraction time be the key factor that influences extraction effect, so with alcohol adding amount, soak time, extraction time be the examination factor, design three levels, the factor level table sees Table 5.
Table 5 factor level table
2, Orthogonal Experiment and Design
Select orthogonal table L
9(3
4) carry out orthogonal test, be that index is screened technology with the extracted amount of dry extract yield, berberine.
2.1 the mensuration of dried cream yield
Get Cortex Phellodendri 100g, add 85% alcohol reflux three times by Orthogonal Experiment and Design, merge extractive liquid, filters, and filtrate recycling ethanol also is concentrated into small size, transfer in the evaporating dish of known weight, water bath method again in 105 ℃ of dryings 3 hours, was put in the exsiccator cooling 0.5 hour, precision is weighed, and is calculated as follows dried cream yield.
2.2 the assay of berberine in Cortex Phellodendri medical material and the dry extract
Content assaying method with reference to Rhizoma Coptidis in the need testing solution processing method in the content assaying method of Chinese Pharmacopoeia version Rhizoma Coptidis in 2000 and " Chinese patent medicine quality standard and the standard substance research ".
Chromatographic condition: with octadecylsilane chemically bonded silica is filler; Acetonitrile-0.05mol/L potassium dihydrogen phosphate (10% potassium hydroxide is transferred pH5.0) (28: 72) is a mobile phase; The detection wavelength is 265nm.Number of theoretical plate calculates by the berberine hydrochloride peak should be not less than 2000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the berberine hydrochloride reference substance, adds methanol and make the solution that contains 0.025mg among every 1ml, promptly.
The preparation of dry extract need testing solution: get this product, porphyrize is got about 0.1g, and accurate the title decides, and puts in the 100ml measuring bottle, adds the about 80ml of hydrochloric acid-methanol (1: 100), and supersound process 30 minutes adds methanol and is diluted to scale, shakes up, and filters, and gets subsequent filtrate, promptly.
The preparation of medical material need testing solution: get the about 0.1g of Cortex Phellodendri fine powder (crossing sieve No. 3), the accurate title, decide, and puts in the 100ml measuring bottle, add the about 80ml of hydrochloric acid-methanol (1: 100), put in 60 ℃ of water-baths and heated 15 minutes, take out supersound process 30 minutes, room temperature is placed and is spent the night, add methanol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
This research is 0.7% with the content of berberine in the Cortex Phellodendri medical material.
2..3 alcohol extraction orthogonal test scheme, result and variance analysis
Alcohol extraction orthogonal test scheme, result and variance analysis see Table 6,7,8.
Table 6 alcohol extraction orthogonal test scheme and table as a result
Table 7 alcohol is promoted cream yield analysis of variance table
| Soruces of variation | Sum of deviation square | Degree of freedom | Variance | The F value | Significance |
| A | 1.1183 | 2 | 0.5592 | 8.4 | ＞0.05 |
| B | 0.6072 | 2 | 0.3036 | 4.6 | ＞0.05 |
| C | 3.9696 | 2 | 1.984 | 29.8 | ＜0.05* |
| Error e | 0.133 | 2 | 0.0665 |
Wherein " * " looks into F-distribution critical table: F for significant difference is arranged
0.05(2,2)=19.00
Promote cream yield The results of analysis of variance as can be known from table 7 alcohol: the C factor has significant difference (P＜0.05), A, B factor there are no significant difference (P＞0.05), that is: decocting time has appreciable impact to dried cream yield, soak time, adds 85% ethanol and doubly measures and do not make significant difference.Can get by range analysis, be in proper order: C＞A＞B, that is: decocting time＞add doubly amount＞soak times of 85%7 alcohol the influence of dried cream yield; A in the A factor
2＞A
3＞A
1, select best level A
2, B in the B factor
1＞B
2＞B
3, select best level B
3, C in the C factor
2＞C
3＞C
1, select best level C
2, the intuitive analysis result shows that optimised process consists of A
2B
1C
2
The analysis of variance table of table 8 alcohol extraction berberine extracted amount
| Soruces of variation | Sum of deviation square | Degree of freedom | Variance | The F value | Significance |
| A | 178.01 | 2 | 89.01 | 12.1 | ＞0.05 |
| B | 0.1233 | 2 | 0.0616 | 0.01 | ＞0.05 |
| C | 1037.55 | 2 | 518.78 | 70.3 | ＜0.05* |
| Error e | 14.7606 | 2 | 7.3803 |
From table 8 The results of analysis of variance as can be known: the C factor has significant difference (P＜0.05), A, B factor there was no significant difference (P＞0.05), that is: and decocting time has appreciable impact to the berberine extracted amount, adds that 85% ethanol is doubly measured, soak time does not make significant difference.Can get by range analysis, to the influence of berberine extracted amount be in proper order: C＞A＞B, A in the A factor
2＞A
3＞A
1, select best level A
2, B in the B factor
1＞B
2＞B
3, select best level B
1, C in the C factor
2＞C
1＞C
3, select best level C
2, the intuitive analysis result shows that optimised process consists of A
2B
1C
2
Investigate index for comprehensive above-mentioned two, preferred best of breed is A
2B
1C
2, the material of promptly getting it filled adds 85% ethanol and decocts three times, adds 7 times of amounts for the first time, adds 6 times of amounts each 1.5 hours for the second time, for the third time.
Four, the investigation of Carapax et Plastrum Testudinis extraction process by water condition
Doubly measure and investigate adding water.
1, method is got Carapax et Plastrum Testudinis medical material 50g, is the examination factor to add that water doubly measures, and the dry extract yield is determined extraction process for investigating index.
2, the assay method of dry extract yield is got Carapax et Plastrum Testudinis medical material 50g, decocts with water secondary, each 6 hours, collecting decoction, filter, filtrate is concentrated into small size, gets certain volume, put in the evaporating dish of constant weight, put evaporate to dryness in the water-bath,, put in the exsiccator cooling 0.5 hour again in 105 ℃ of dryings 3 hours, precision is weighed, and is calculated as follows the dry extract yield.
3, add the selection that water is doubly measured
Get Carapax et Plastrum Testudinis 50g, add the decocting that different medical materials doubly measure and boil secondary, each 6 hours, collecting decoction served as to investigate index with dried cream yield, preferably adds water and doubly measures, and the results are shown in Table 9.
Table 9 Carapax et Plastrum Testudinis adds water and doubly measures investigation table as a result
| Amount of water (doubly) | 5 4 | 6 5 | 7 6 |
| Dried cream yield (%) | 5.11 | 6.67 | 6.86 |
The above results shows: Carapax et Plastrum Testudinis adds 6 times of water gagings for the first time, adds for the second time 5 times of water gagings and decocts, and each 6 hours, dried cream yield increased few, and determine that therefore Carapax et Plastrum Testudinis adds water and doubly measures and be: Carapax et Plastrum Testudinis decocts with water secondary, adds 6 times of amounts for the first time, adds 5 times of amounts for the second time.
4. Carapax et Plastrum Testudinis water is proposed the investigation of back medicinal residues acetic acid extracting technology condition
Medicinal residues dried after Carapax et Plastrum Testudinis water was carried in the former tablet technology, were ground into coarse powder, with 10% acetic acid dipping, so 10% acetic acid is doubly measured and dip time is investigated to adding.
1), method gets the medicinal residues after Carapax et Plastrum Testudinis medical material (50g) decocts with water, airing, with add 10% acetic acid doubly amount, dip time, dipping number of times be the examination factor, the dry extract yield is determined extraction process for investigating index.
2), the assay method of dry extract yield gets Carapax et Plastrum Testudinis medical material 50g, decocts with water secondary, each 6 hours, collecting decoction filters, and the slag of getting it filled dries, be ground into coarse granule, add 10% acetic acid dipping, filter, filtrate is concentrated into small size, gets certain volume, puts in the evaporating dish of constant weight, put evaporate to dryness in the water-bath,, put in the exsiccator cooling 0.5 hour again in 105 ℃ of dryings 3 hours, precision is weighed, and is calculated as follows the dry extract yield.
3), the selection of acetic acid extracting condition
Doubly measuring dipping 12 hours 3.1 the selection Carapax et Plastrum Testudinis medicinal residues of dipping number of times add 3 times of amount 10% acetic acid, serves as to investigate index with dried cream yield, determines the dipping number of times, the results are shown in Table 10.
Table 10 Carapax et Plastrum Testudinis medicinal residues acetic acid lixiviate number of times is investigated table as a result
| The dipping number of times | 1 | 2 | 3 |
| Dried cream yield (%) | 7.03 | 7.12 | 7.15 |
The above results shows: the Carapax et Plastrum Testudinis medicinal residues add 10% acetic acid dipping 1 time, and its dry extract yield substantially no longer increases.So select dipping technology once.
Adding 2,3,4 times of amount 10% acetic acid dippings 12 hours respectively 3.2 add the selection Carapax et Plastrum Testudinis medicinal residues that 10% acetic acid doubly measures, serves as to investigate index with dried cream yield, determines that solvent doubly measures, and the results are shown in Table 11.
Table 11 Carapax et Plastrum Testudinis medicinal residues acetic acid extraction solvent consumption is investigated table as a result
| 10% acetic acid amount (doubly) | 2 | 3 | 4 |
| Dried cream yield (%) | 5.87 | 7.03 | 7.13 |
The above results shows: the Carapax et Plastrum Testudinis medicinal residues add 3 times of amount 10% acetic acid dippings, and its dry extract yield substantially no longer increases.So select to add the technology of 3 times of amount 10% acetic acid.
Doubly measuring the dipping different time 3.3 the selection Carapax et Plastrum Testudinis medicinal residues of dip time add 3 times of amount 10% acetic acid, serves as to investigate index with dried cream yield, determines dip time, the results are shown in Table 12.
Table 12 Carapax et Plastrum Testudinis medicinal residues acetic acid extraction time is investigated table as a result
| Dip time | 6 | 12 | 18 |
| Dried cream yield (%) | 6.32 | 7.03 | 7.16 |
The above results shows: the Carapax et Plastrum Testudinis medicinal residues add 3 times of amount 10% acetic acid dippings 12 hours, and its dry extract yield substantially no longer increases.So select 12 hours technology of dipping.
In sum, Carapax et Plastrum Testudinis medicinal residues acetic acid lixiviate optimum condition is: add 3 times of amount 10% acetic acid dippings 12 hours.
The present invention incites somebody to action and new, old dosage form is compared, and the results are shown in Table 13.
Table 13 FUKE ZHIDAI PIAN and capsule comparison sheet
The above results shows: the quality standard of capsule is than tablet height.
Description of drawings
Accompanying drawing is a process chart of the present invention.
The specific embodiment
Embodiment 1
Get Cortex Ailanthi 363g, Fructus Schisandrae Chinensis 64g, Cortex Phellodendri 363g, Carapax et Plastrum Testudinis 242g, Poria 363g, Colla Corii Asini 120g, Rhizoma Dioscoreae 363g respectively.
A, Cortex Ailanthi decoct with water secondary, and each 2 hours, add for the first time 8 times of water gagings, add 7 times of water gagings for the second time, collecting decoction filters, and it is 1.15 that filtrate is concentrated into relative density,, add ethanol and make that to contain the alcohol amount be 50%, left standstill 12 hours, filter.B, Cortex Phellodendri add 85% alcohol reflux three times, each 1.5 hours, add for the first time 7 times of amounts, add 6 times of amounts for the second time, for the third time in 6 times of amounts, merge extractive liquid, filters.C, Poria 60% ethanol, Fructus Schisandrae Chinensis and Rhizoma Dioscoreae 45% ethanol percolation, flow velocity is 5ml/min, collecting the percolation liquid measure is 10 times of raw material doses.D, Carapax et Plastrum Testudinis decoct with water secondary, and each 6 hours, add 6 times of water gagings for the first time, add 5 times of water gagings for the second time, filter, filtrate is condensed into gluey thick paste; Filtering residue dries, and is ground into coarse powder, floods 12 hours with 3 times of amount 10% acetic acid, filters the filtrate evaporate to dryness.E, Colla Corii Asini with stir-baked in powder of CONCHA MERETRICIS SEU CYCLINAE after, be ground into fine powder, sieve.F, above-mentioned each step is obtained being thick paste, mixing adds adjuvant dextrin 70 and restrains into 1000, and is dry, pulverize, and adorns capsule No. 0.
Embodiment 2-4
Three batches of pilot product steps are poly-with embodiment 1.
In order to verify and to improve the preparation technology that experimentation goes out, so that reach the operability of production and to the adaptability of relevant devices, we amplify 10 times with preparation prescription and feed intake, and use the multi-function extractor of pilot plant, vacuum concentration, drying equipment.To the optimum process technology condition that research under laboratory condition obtains, carry out three batches of pilot scale researches, and each key process technology parameter of itemized record.And three batches of pilot products are carried out quality inspection, the results are shown in Table 14.
Three batches of pilot scale sample datas of table 14 table
| Lot number | Embodiment 2 20030105 | Embodiment 3 20030107 | Embodiment 4 20030109 | |
| Total inventory (kg) | 18.78 | 18.78 | 18.78 | |
| Donkey-hide gelatin fine powder (Kg) | 1.2 | 1.2 | 1.2 | |
| Dextrin (Kg) | 0.7 | 0.7 | 0.7 | |
| Medicated powder heavy (kg) | 1.54 | 1.56 | 1.55 | |
| Finished product theoretical yield (grain) | 10000 | 10000 | 10000 | |
| Finished product is actual must measure (grain) | 9820 | 9885 | 9857 | |
| Finished product yield (%) | 98.2 | 98.85 | 98.57 | |
| The quality inspection | Character | Be capsule, content is a chocolate brown powder; Feeble QI, bitter in the mouth, little sour raw meat. | Be capsule, content is a chocolate brown powder; Feeble QI, bitter in the mouth, little sour raw meat. | Be capsule, content is a chocolate brown powder; Feeble QI, bitter in the mouth, little sour raw meat. |
| Differentiate | Detect Fructus Schisandrae Chinensis | Detect Fructus Schisandrae Chinensis | Detect Fructus Schisandrae Chinensis | |
| Detect Cortex Phellodendri | Detect Cortex Phellodendri | Detect Cortex Phellodendri | ||
| Detect Poria | Detect Poria | Detect Poria | ||
| Detect Rhizoma Dioscoreae | Detect Rhizoma Dioscoreae | Detect Rhizoma Dioscoreae | ||
| Moisture content (%) | 4.5 | 4.4 | 4.2 | |
| Disintegration (min) | 15 | 16 | 16 | |
| Look into | Content uniformity | Up to specification | Up to specification | Up to specification |
| Content of berberine hydrochloride (mg/ grain) | 1.40 | 1.68 | 1.53 | |
| Bacterial population (individual/g) | 50 | 50 | 50 | |
| Fungi count (individual/g) | ＜10 | ＜10 | ＜10 | |
| Escherichia coli (individual/g) | Do not detect | Do not detect | Do not detect |
Above result shows: gynaecologic leucorrhea removing capsules preparation technique condition is reasonable, feasible; Extract, concentrate, method such as drying with amplify production equipment and adapt; Prepared product quality is qualified, and is stable, can be used for commercial production.
Embodiment 5
Other step is with embodiment 1, wherein adds adjuvant dextrin 35 grams, starch 35 is restrained into 1000, and is dry, pulverize, and adorns capsule No. 0.
Embodiment 6
Other step wherein adds supplementary product starch 70 and restrains into 1000 with embodiment 1, and capsule is adorned in dry, pulverizing No. 0.
Embodiment 7
Other step is with embodiment 1, and wherein every capsules Chinese medicine activity becomes 260mg, and supplementary product starch 90 grams are made 1000.
Embodiment 8
Other step is with embodiment 1, and wherein every capsules Chinese medicine activity becomes 280mg, and supplementary product starch 70 grams are made 1000.
Embodiment 9
Other step is with embodiment 1, and wherein every capsules Chinese medicine activity becomes 270mg, and supplementary product starch 70 grams are made 1000.
Claims (2)
1, gynaecologic leucorrhea removing capsule, form by active constituents of medicine and capsule adjuvant, described active constituents of medicine is made by Cortex Ailanthi 363g, Fructus Schisandrae Chinensis 64g, Cortex Phellodendri 363g, Carapax et Plastrum Testudinis 242g, Poria 363g, Colla Corii Asini 120g, Rhizoma Dioscoreae 363g, it is characterized in that: adding the capsule adjuvant is dextrin 70g, and make 1000 by following preparation technology, A, Cortex Ailanthi decoct with water secondary, each 2 hours, add 8 times of water gagings for the first time, add 7 times of water gagings for the second time, collecting decoction, filter, filtrate concentrates, and adds ethanol and makes that to contain the alcohol amount be 50%, leave standstill, filter;
B, Cortex Phellodendri add 85% alcohol reflux three times, each 1.5 hours, add for the first time 7 times of amounts, add 6 times of amounts for the second time, for the third time in 6 times of amounts, merge extractive liquid, filters;
C, Poria 60% ethanol, Fructus Schisandrae Chinensis and Rhizoma Dioscoreae 45% ethanol percolation, collecting the percolation liquid measure is 10 times of raw material doses;
D, Carapax et Plastrum Testudinis decoct with water secondary, and each 6 hours, add 6 times of water gagings for the first time, add 5 times of water gagings for the second time, filter, filtrate is condensed into gluey thick paste; Filtering residue dries, and is ground into coarse powder, with 3 times of amount 10% acetic acid dippings, filters the filtrate evaporate to dryness;
E, Colla Corii Asini with stir-baked in powder of CONCHA MERETRICIS SEU CYCLINAE after, be ground into fine powder, sieve;
F, above-mentioned each step is obtained being thick paste, mixing adds adjuvant, and is dry, pulverize, encapsulated.
2, the capsular technology of the preparation described gynaecologic leucorrhea removing of claim 1,
A, Cortex Ailanthi decoct with water secondary, and each 2 hours, add for the first time 8 times of water gagings, add 7 times of water gagings for the second time, collecting decoction filters, and it is 1.15 that filtrate is concentrated into relative density, adds ethanol and makes that to contain the alcohol amount be 50%, leaves standstill 10-14 hour, filters;
B, Cortex Phellodendri add 85% alcohol reflux three times, each 1.5 hours, add for the first time 7 times of amounts, add 6 times of amounts for the second time, for the third time in 6 times of amounts, merge extractive liquid, filters;
C, Poria 60% ethanol, Fructus Schisandrae Chinensis and Rhizoma Dioscoreae 45% ethanol percolation, flow velocity is 5ml/min, collecting the percolation liquid measure is 10 times of raw material doses;
D, Carapax et Plastrum Testudinis decoct with water secondary, and each 6 hours, add 6 times of water gagings for the first time, add 5 times of water gagings for the second time, filter, filtrate is condensed into gluey thick paste; Filtering residue dries, and is ground into coarse powder, floods 12 hours with 3 times of amount 10% acetic acid, filters the filtrate evaporate to dryness;
E, Colla Corii Asini with stir-baked in powder of CONCHA MERETRICIS SEU CYCLINAE after, be ground into fine powder, sieve;
F, above-mentioned each step is obtained being thick paste, mixing adds dextrin, and is dry, pulverize, encapsulated.
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| CN110333305A (en) * | 2019-06-30 | 2019-10-15 | 广西万寿堂药业有限公司 | The detection method of content of gynaecologic leucorrhea removing Chinese medicine composition |
| CN110339277A (en) * | 2019-08-20 | 2019-10-18 | 广西万寿堂药业有限公司 | FUKE ZHIDAI PIAN and preparation method thereof |
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