CN101485735B - Medicament composition with stone-eliminating and expelling functions and preparation method thereof - Google Patents
Medicament composition with stone-eliminating and expelling functions and preparation method thereof Download PDFInfo
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Abstract
The invention provides a medical composition with functions of dissolving and discharging stones, which is pills prepared from Herba Lysimachiae, stir-fried cowherb seed, Common Knotgrass Herb, Corydalis tuber processed by vinegar, scalded Endothelium Corneum Gigeriae Galli, Salvia Miltrorrhiza, Radix Aucklandiae, fringed pink, Radix Cyathulae, Japanese Climbing Fern Spore and a pharmaceutic adjuvant starch. The preparation method for the medical composition comprises that: firstly mixing an extract with the starch of which the weight is twice of that of the extract for stirring; drying the mixture at a temperature of 70 DEG C and reduced pressure of -0.07MPa; crushing the mixture into fine powder; mixing the fine powder evenly and preparing the fine powder into pillet mother nucleuses by water; and adding the residual starch gradually to coat the mother nucleuses to prepare pellets, and drying the pellets. The outsides of the mother nucleuses are coated with the starch, so that the pellets cannot stick and keep round and smooth when dried, the difficult problem that pellets cannot be prepared is solved, and the defect that granules are easy to absorb damp is overcome. The preparation has the advantages of safe administration, accurate dosage, controllable quality, reliable healing effect, high contents of effective ingredients, small administrative dosage, convenient administration, and sugar-free to be suitable for more patients.
Description
Technical field
The present invention relates to a kind of pharmaceutical composition with fossil, calculus effect; The invention still further relates to the preparation method of this medicine, belong to the field of Chinese medicines.
Background technology
The logical granule of nephrolith is a kind of Chinese patent medicine of classics.It makes granule by Herba Lysimachiae, Semen Vaccariae (parched), Herba Polygoni Avicularis, Rhizoma Corydalis (processed with vinegar), boiling hot Endothelium Corneum Gigeriae Galli, Radix Salviae Miltiorrhizae, the Radix Aucklandiae, Herba Dianthi, Radix Achyranthis Bidentatae, Spora Lygodii ten flavor Chinese herbal medicine.The logical granule of this nephrolith has clearing away heat-damp and promoting diuresis, promoting blood circulation and stopping pain, and fossil, the urinary calculus removing effect is used for renal calculus, pyelolithiasis, the clinical treatment of diseases such as ureteral calculus.But said preparation is a granule, and dosage form is comparatively backward, and the granule dose is big, and taking needs boiled water to take after mixing it with water, and contains a large amount of sucrose and be not suitable for diabetic and take, and the easy moisture absorption of granule, is prone to caking phenomenon in the storage process.
The Chinese medicine watered pill be with the medical material fine powder with or make adhesive with yellow wine, rice vinegar, rare medicine juice and liquid glucose etc., the pill of making is a kind of Chinese medicine compound preparation.Can medicine be prepared into the watered pill, determined multiple factor, comprising the physicochemical character of crude drug, the pre-treatment of crude drug or the preparation technology of the extraction process and the watered pill.Can keep or improve drug effect after medication preparation become pill, reduce using dosage, for a person skilled in the art, all be difficult to expect.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, and a kind of pharmaceutical composition with fossil, calculus effect is provided.Another technical scheme of the present invention has provided this preparation of drug combination method.
The invention provides a kind of pharmaceutical composition with fossil, calculus effect, it is the pill that is prepared into by following weight percentages and pharmaceutic adjuvant,
Herbal raw material:
Herba Lysimachiae 15-18% Semen Vaccariae (parched) 15-18% Herba Polygoni Avicularis 9-12%
Rhizoma Corydalis (processed with vinegar) 4-6% scalds Endothelium Corneum Gigeriae Galli 6-8% Radix Salviae Miltiorrhizae 6-8%
Radix Aucklandiae 3-5% Herba Dianthi 8-11% Radix Achyranthis Bidentatae 4-6%
Spora Lygodii 6-8%
Pharmaceutic adjuvant:
Starch 11-13%.
Further preferably, it is the pill that is prepared into by following weight percentages and pharmaceutic adjuvant,
Herbal raw material:
Herba Lysimachiae 17.1% Semen Vaccariae (parched) 17.1% Herba Polygoni Avicularis 10.3%
Rhizoma Corydalis (processed with vinegar) 5.1% scalds Endothelium Corneum Gigeriae Galli 6.9% Radix Salviae Miltiorrhizae 6.9%
The Radix Aucklandiae 3.4% Herba Dianthi 8.6% Radix Achyranthis Bidentatae 5.1%
Spora Lygodii 6.9%
Pharmaceutic adjuvant:
Starch 12.6%.
Wherein, every gram contains Herba Lysimachiae, Herba Polygoni Avicularis with Quercetin (C in the pill
15O
10H
7) meter, must not be less than 0.18 milligram.
The present invention also provides this preparation of drug combination method, in the described 10 flavor herbal raw materials, getting Spora Lygodii, Semen Vaccariae packs in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, add 10 times of water gagings at every turn, extract for the first time 2.5 hours, extracted 1.0 hours for the second time, collecting decoction, filter, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.20～1.25 (75～80 ℃); Add starch and mix, mix cream with extractum, drying under reduced pressure (70 ℃ ,-0.07MPa), be ground into fine powder, mixing, the general ball of making of water, drying promptly gets pill.
Add for the first time 1 times of amount starch and mix, mix cream with extractum, drying under reduced pressure (70 ℃ ,-0.07MPa), be ground into fine powder, mixing, the general piller parent nucleus of making of water progressively adds remaining starch again, is wrapped in the parent nucleus outside and makes piller, drying.The mean diameter of described parent nucleus is the 1.5-2 millimeter.In described female ball, add the general piller of making of residue recipe quantity starch secondary, the amount that adds starch is more than 15% of parent nucleus weight.
Medicine of the present invention is that herbal raw material extractum is mixed with the starch of specified quantitative, be prepared into the parent nucleus of specified particle diameter, again at parent nucleus coated outside starch, make piller can be when drying can adhesion, solve the difficult problem that to make piller, overcome the shortcoming that granule is easy to the moisture absorption.Bolus of drug effective component content height of the present invention, taking dose be little, it is more convenient to take, be suitable for that the crowd is more extensive, outward appearance is all good.
Below the present invention is described in further detail by the specific embodiment, but do not limit the present invention, those skilled in the art can make various changes and distortion according to the present invention, only otherwise break away from spirit of the present invention, all should belong to the scope of claims of the present invention.
The specific embodiment
The preparation of embodiment 1 bolus of drug of the present invention
Herbal raw material (unit: gram):
Herba Lysimachiae 750g Semen Vaccariae (stir-fry) 750g Herba Polygoni Avicularis 450g
Rhizoma Corydalis (vinegar system) 225g Endothelium Corneum Gigeriae Galli (scalding) 300g Radix Salviae Miltiorrhizae 300g
Radix Aucklandiae 150g Herba Dianthi 375g Radix Achyranthis Bidentatae 225g
Spora Lygodii 300g
Pharmaceutic adjuvant:
Starch 550g
Its preparation method is, in the above 10 flavor Chinese herbal medicine, getting Spora Lygodii, Semen Vaccariae packs in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, add 10 times of water gagings at every turn, extract for the first time 2.5 hours, extracted 1.0 hours for the second time, collecting decoction, filter, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.20 (80 ℃); Add starch and mix, mix cream with extractum, drying under reduced pressure (70 ℃ ,-0.07MPa), be ground into fine powder, mixing, the general ball of making of water, drying is made 1000g, promptly.
The preparation of embodiment 2 bolus of drug of the present invention
Herbal raw material:
Herba Lysimachiae 17.1% Semen Vaccariae (parched) 17.1% Herba Polygoni Avicularis 10.3%
Rhizoma Corydalis (processed with vinegar) 5.1% scalds Endothelium Corneum Gigeriae Galli 6.9% Radix Salviae Miltiorrhizae 6.9%
The Radix Aucklandiae 3.4% Herba Dianthi 8.6% Radix Achyranthis Bidentatae 5.1%
Spora Lygodii 6.9%
Pharmaceutic adjuvant:
Starch 12.6%
Its preparation method is, in the above 10 flavor Chinese herbal medicine, getting Spora Lygodii, Semen Vaccariae packs in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, add 10 times of water gagings at every turn, extract for the first time 2.5 hours, extracted 1.0 hours for the second time, collecting decoction, filter, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.20 (80 ℃); Add starch and mix, mix cream with extractum, drying under reduced pressure (70 ℃ ,-0.07MPa), be ground into fine powder, mixing, the general ball of making of water, drying promptly gets bolus of drug of the present invention.
The preparation of embodiment 3 bolus of drug of the present invention
Herbal raw material:
Herba Lysimachiae 15% Semen Vaccariae (parched) 15% Herba Polygoni Avicularis 12%
Rhizoma Corydalis (processed with vinegar) 6% scalds Endothelium Corneum Gigeriae Galli 8% Radix Salviae Miltiorrhizae 8%
The Radix Aucklandiae 3% Herba Dianthi 8% Radix Achyranthis Bidentatae 6%
Spora Lygodii 8%
Pharmaceutic adjuvant:
Starch 11%
Its preparation method is, in the above 10 flavor Chinese herbal medicine, getting Spora Lygodii, Semen Vaccariae packs in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, add 10 times of water gagings at every turn, extract for the first time 2.5 hours, extracted 1.0 hours for the second time, collecting decoction, filter, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.25 (75 ℃); Add starch and mix, mix cream with extractum, drying under reduced pressure (70 ℃ ,-0.07MPa), be ground into fine powder, mixing, the general ball of making of water, drying promptly gets bolus of drug of the present invention.
The preparation of embodiment 4 bolus of drug of the present invention
Herbal raw material:
Herba Lysimachiae 18% Semen Vaccariae (parched) 18% Herba Polygoni Avicularis 9%
Rhizoma Corydalis (processed with vinegar) 4% scalds Endothelium Corneum Gigeriae Galli 6% Radix Salviae Miltiorrhizae 6%
The Radix Aucklandiae 5% Herba Dianthi 11% Radix Achyranthis Bidentatae 4%
Spora Lygodii 6%
Pharmaceutic adjuvant:
Starch 13%
Its preparation method is, in the above 10 flavor Chinese herbal medicine, getting Spora Lygodii, Semen Vaccariae packs in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, add 10 times of water gagings at every turn, extract for the first time 2.5 hours, extracted 1.0 hours for the second time, collecting decoction, filter, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.22 (79 ℃); Add starch and mix, mix cream with extractum, drying under reduced pressure (70 ℃ ,-0.07MPa), be ground into fine powder, mixing, the general ball of making of water, drying promptly gets bolus of drug of the present invention.
The discrimination method of embodiment 5 medicines of the present invention
(1) get this product, porphyrize is got 3g, adds methanol 50ml, supersound process 15 minutes, filter, filtrate evaporate to dryness, residue add water makes dissolving, adds strong ammonia solution and transfers to alkalescence, extracts 3 times with the ether jolting, each 10ml divides and gets ether layer, and ether solution evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Rhizoma Corydalis control medicinal material 0.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with petroleum ether (60～90 ℃)-chloroform-methanol (10: 4: 0.5) is developing solvent, launch, take out, dry, iodine is smoked, puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(2) get this product, porphyrize is got 3g, add 70% ethanol 30ml, supersound process 15 minutes filters, evaporate to dryness in the filtrate water-bath, residue adding distil water 25ml makes dissolving, transfers pH to 2 with dilute hydrochloric acid, with ether 25ml extraction 2 times, divide and get ether layer, ether solution evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), drawing each 10 μ l of above-mentioned two kinds of solution puts respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid (10: 4: 1.6) is developing solvent, launch, take out, dry, put in the ammonia steam smoked after, put under the ultraviolet light (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
The test that the adjuvant of embodiment 6 pharmaceutical composition pills of the present invention and adjuvant are selected
1, Study on extraction
1.1 soaking heart time and pick up investigates
Take by weighing medical material by prescription, add 10 times of water gagings and soaked 25 minutes, the saturating heart of medical material filters the medicinal liquid that is not adsorbed, and collects filtrate, measures filtrate volume, and trying to achieve pick up is 190%.
1.2 the water extraction condition is investigated
The principal element that influence is extracted has solvent consumption, extraction time, extraction time, adopts the single factor experiment method, is that index is screened with the quercetin content.
Quercetin is measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000).
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler, is mobile phase with methanol-0.2% phosphoric acid solution (55: 45), detects wavelength 370nm, and number of theoretical plate calculates with the Quercetin peak should be not less than 2500.
The preparation of reference substance solution: precision takes by weighing Quercetin reference substance 10mg, puts in the 50ml measuring bottle, with dissolve with methanol and be diluted to scale, shakes up; Get 1ml to 10ml measuring bottle, with dissolve with methanol and be diluted to scale, shake up, promptly get (containing Quercetin 0.02mg among every 1ml).
The preparation of need testing solution: the accurate extracting solution (containing Herba Lysimachiae crude drug 2.25g, Herba Polygoni Avicularis crude drug 1.35g) of drawing, put in the 100ml conical flask, add 2.3% methanol hydrochloride solution 40ml, put in 85 ℃ of water-baths and refluxed 1 hour, be cooled to room temperature, change in the 50ml measuring bottle, be diluted to scale with methanol, shake up, filter, filtrate is as need testing solution.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
1. amount of water is investigated:
Take by weighing 4 parts of medical materials by prescription, add 8 times of amounts, 10 times of amounts, 12 times of amounts, 14 times of amounts at every turn respectively, water extraction twice extracted 2.5 hours for the first time; Extracted 1.0 hours for the second time, collect and respectively test the gained extracting solution, measure quercetin content, the results are shown in Table 1.
Table 1 amount of water is investigated
Can get by table 1, add 10 times of water gagings after the increase of Quercetin extracted amount very little, therefore add water and be defined as 10 times of amounts.
2. extraction time is investigated:
Take by weighing 4 parts of medical materials by prescription, add 10 times of water gagings at every turn, extract twice, extracted 2.5 hours for the first time; Extracted respectively 0.5 hour, 1.0 hours, 1.5 hours, 2.0 hours for the second time, collect and respectively test the gained extracting solution, measure quercetin content, the results are shown in Table 2.
Investigate for the second time by extraction time for table 2
Can be got by table 2, extract for the second time that the Quercetin extracted amount no longer increases after 1.0 hours, therefore extraction time is defined as 1.0 hours for the second time.
2, filter
The medical material aqueous extract filters with 200 mesh sieves, collects filtrate.
3, concentrate
Filtrate respectively normal pressure, decompression (75 ℃ ,-0.07Mpa) to be concentrated into the extractum relative density be 1.20～1.25 (75～80 ℃), collects extractum, measure concentrate before and after quercetin content, the results are shown in Table 3.
Table 3 concentrates forward and backward quercetin content to be changed
Can get by table 3, behind the concentrating under reduced pressure quercetin content loss less, show that to adopt concentrating under reduced pressure reasonable.
4, Study on Forming
4.1 paste-forming rate is measured
Take by weighing medical material by prescription, extract, filter, collect filtrate by gained technology, the accurate extracting solution that contains 10g crude drug amount drawn in the evaporating dish of constant weight, evaporate to dryness in the water-bath, residue takes out in 105 ℃ of dryings 3 hours, put and put coldly in the exsiccator, take out, weigh, calculate.The results are shown in Table 4.
Table 4 paste-forming rate is measured
Can be got by table 4: average paste-forming rate is 11.80%.
4.2 prescription design
Because of the logical granule prescription of nephrolith usage and dosage is: oral, a daily dose primary crude drug 15.3g.Now make pill, relate to the formulation usage and dosage, inevitable relevant with Chinese medical concrete amount and supplementary product consumption.One daily dose primary crude drug 15.3g, paste volume are that (experiment records medicinal material extract rate average out to: 11.80%), by taking every day 2 times, each 1 bag, specification is the 2g/ bag to 1.8g, and then adjuvant need add 2.2g.According to last calculating, preparation prescription is:
Extract medical material 3825g (the logical granule of nephrolith has 7.5 times of sugared type recipe quantity), paste volume is about 450g, and (experiment records medicinal material extract rate average out to: 11.80%), make 1000g altogether, adjuvant need add and be about 550g.
Herba Lysimachiae 750g, Semen Vaccariae (stir-fry) 750g, Herba Polygoni Avicularis 450g, Rhizoma Corydalis (vinegar system) 225g, Endothelium Corneum Gigeriae Galli (scalding) 300g, Radix Salviae Miltiorrhizae 300g, Radix Aucklandiae 150g, Herba Dianthi 375g, Radix Achyranthis Bidentatae 225g, Spora Lygodii 300g
Adjuvant: 550g
Make 1000g altogether
4.3 become ball research
Consider that whole technology obtains through refining into aqueous extract with water, and the hygroscopicity of extractum is not strong, in conjunction with the special process characteristics of piller, the ball hygroscopicity of making is not strong.So needn't add too many adjuvant, generally select starch, dextrin to get final product, can reduce the viscosity of extractum in molding, increased the roundness of pill simultaneously, smoothness, the moisture resistance of raising piller.
Confirm to add 1 times of above dextrin of amount or starch mixes with extractum through experimentation, mix cream, drying under reduced pressure (70 ℃ ,-0.07MPa), be ground into fine powder, mixing, the general system of water substantially can the molding pill, but adhesion during made piller drying can't make the finished product piller.Add dextrin or amount of starch to 2 times, can make the finished product piller substantially, but finished product piller roundness, smoothness extreme difference (see Table 5, table 6).Therefore adopt the general ball technical solution of a secondary difficult problem.
Experiment mixes with extractum by adding 1 times of amount dextrin or starch, mixes cream, (70 ℃ of drying under reduced pressure,-0.07MPa), be ground into fine powder, mixing, the general system of water, substantially can play parent nucleus by the molding pill, to to a certain degree ((experiment confirm parent nucleus particle diameter has decisive action to ball quality of the present invention: the mean diameter of parent nucleus is at the 1.5-2 millimeter, and finished product piller rounding is smooth at the 1.5-2 millimeter for the mean diameter of parent nucleus, evenly, mass effect good (see Table 7, table 8).)), add 15% above dextrin or starch again and continue general system, can make the finished product piller, and finished product piller rounding, smooth, evenly (see Table 9, table 10).
Table 5 adopts conventional method pill experiment situation with starch
Table 6 adopts conventional method pill experiment situation with dextrin
Table 7 parent nucleus size (adjuvant is a starch, with the general ball of 20% adjuvant secondary) is to the influence of the watered pill of the present invention:
Table 8 parent nucleus size (adjuvant is a dextrin, with the general ball of 20% adjuvant secondary) is to the influence of the watered pill of the present invention:
The general ball supplementary product consumption of table 9 secondary (adjuvant is a starch) is to the influence of the watered pill of the present invention:
The general ball supplementary product consumption of table 10 secondary (adjuvant is a dextrin) is to the influence of the watered pill of the present invention:
4.4 adjuvant is selected
1. supplementary product kind screening
In the experiment respectively with the general pill of the manual water of starch, dextrin of 120% amount, adopt the general ball of secondary, add 1 times of amount starch for the first time and mix, mix cream with extractum, (70 ℃ of drying under reduced pressure,-0.07MPa), be ground into fine powder, mixing, the general piller parent nucleus of making of water, again remaining starch is progressively added, be wrapped in the parent nucleus outside and make piller, drying.Be placed in 75.28% the relative humidity (25 ℃) 72 hours.Investigate ball hydroscopicity.The results are shown in Table 11
Table 11 supplementary product kind screening table
Add starch, dextrin hydroscopicity basically identical as shown in Table 11 respectively,, select starch to get final product because starch is adjuvant commonly used.
2. supplementary product consumption screening
The results are shown in Table 12.
The screening of table 12 starch consumption
It is better when the starch addition is in 1.2～1.5 times of dried cream of theory as seen from the above table.But the starch addition is many, and dose is just big, is advisable about 1.22 times (550g) that therefore definite starch addition is dried cream amount.
Press in the experiment with the dried cream different proportion of theory and add the starch pill, adopt the general ball of secondary, add 1 times of amount starch for the first time and mix, mix cream with extractum, (70 ℃ of drying under reduced pressure,-0.07MPa), be ground into fine powder, mixing, the general piller parent nucleus of making of water, again remaining starch is progressively added, be wrapped in the parent nucleus outside and make piller, drying.Investigate its hygroscopicity with method.
4.4 compare before and after dry
With extractum with after starch mixes, drying under reduced pressure (below 80 ℃ ,-0.07Mpa), collect dry thing, measure that dry forward and backward quercetin content changes and relatively Rhizoma Corydalis, Radix Salviae Miltiorrhizae thin layer chromatography change, the results are shown in Table 13.
The dry forward and backward comparative result of table 13
Can be got by table 13: dry forward and backward quercetin content, Rhizoma Corydalis, Radix Salviae Miltiorrhizae thin layer chromatography have no significant change, and illustrate that the drying process condition is reasonable, feasible.
4.5 pulverize
Extract dry product is pulverized, crossed 80 mesh sieves, weigh, calculate flour extraction, the results are shown in Table 14.
Table 14 flour extraction is investigated
Can be got by table 14, flour extraction all is higher than 95%, so the regulation flour extraction must not be lower than 95%.
4.6 mix
In order to guarantee the end product quality homogeneity, serve as to investigate index with quercetin content uniformity in the fine powder, investigated three-dimensional mixer with the mixed mixing uniformity of fine powder.
Test method: be divided into three layers of upper, middle and lowers after will mixing, every layer is selected two some sampling and measuring quercetin contents, calculates the RSD value of 6 points.
Content assaying method: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000).
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler, is mobile phase with methanol-0.2% phosphoric acid solution (55: 45), detects wavelength 370nm, and number of theoretical plate calculates with the Quercetin peak should be not less than 2500.
The preparation of reference substance solution: precision takes by weighing Quercetin reference substance 10mg, puts in the 50ml measuring bottle, with dissolve with methanol and be diluted to scale, shakes up; Get 1ml to 10ml measuring bottle, with dissolve with methanol and be diluted to scale, shake up, promptly get (containing Quercetin 0.02mg among every 1ml).
The preparation of need testing solution: it is an amount of to get this product, and porphyrize is got the about 3g of fine powder, the accurate title, decide, and puts in the 100ml conical flask, adds methanol solution 30ml and hydrochloric acid 1ml, put in 85 ℃ of water-baths and refluxed 1 hour, be cooled to room temperature, change in the 50ml measuring bottle, be diluted to scale with methanol, shake up, the accurate 2ml that inhales is in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, centrifugal, cross microporous filter membrane (0.45um), get filtrate as need testing solution.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
The results are shown in Table 15:
The blended uniformity of table 15 fine powder is table as a result
Result of the test shows, RSD＜5%, and mix homogeneously, technology is rationally feasible.
4.7 pill
To pulverize gained half extractum fine powder mixing, the general piller of making of water adopts the general ball of secondary, add for the first time 1 times of amount starch and mix, mix cream, (70 ℃ of drying under reduced pressure with extractum,-0.07MPa), be ground into fine powder, mixing, the general piller parent nucleus of making of water, again remaining starch is progressively added, be wrapped in the parent nucleus outside and make piller, dry (60 ℃) collect piller.
4.8 piller physical property
1. character: pilot scale 10 batch samples are brown to tan piller; Mildly bitter flavor.
2. piller is mobile investigates
It is an amount of to get piller, makes it flow down and be cone shape through a funnel, surveys its angle of repose, investigates the flowability of piller, the results are shown in Table 16.
Table 16 piller is mobile to be investigated
The result shows: 14.6 ° of piller average out to angle of repose illustrate that it is better mobile.
3. critical relative humidity is measured
Take by weighing 7 parts of pillers, every part of about 2g, the accurate title, decide, and places respectively under the different relative humidity environment that cause with the variable concentrations sodium hydroxide solution, placed 10 days under 25 ℃ of conditions, measures its weight change, measures the piller critical relative humidity, the results are shown in Table 17.
Table 17 critical relative humidity is measured
Can get critical relative humidity by sucting wet curve is 55%, and prompting is in packing, when storing, and envionmental humidity should be controlled at below 50%, to guarantee stability of formulation.
4. the mensuration of bulk density
It is an amount of to take by weighing piller, places the 250ml graduated cylinder respectively, falls for several times with certain altitude, makes degree of tightness suitable, reads the shared volume of piller, calculates bulk density, the results are shown in Table 18.
Table 18 piller bulk density measurement result
Can get by table 18: piller bulk density average out to 0.59g/ml.
5, pilot scale
According to experiment screening technology, 10 batches of pilot scales the results are shown in Table 19,20,21.
Table 19 process stabilizing Journal of Sex Research
Table 20 steady quality Journal of Sex Research
Table 21 steady quality Journal of Sex Research
By table 19,20,21 as seen, bolus of drug pilot product process stabilizing of the present invention, end product quality is reliable; The extraction process and the Study on Forming result of the single factor research of bolus of drug of the present invention are reasonable, feasible process.Therefore, final definite bolus of drug production technology of the present invention is: ten flavors in the prescription, Spora Lygodii, Semen Vaccariae are packed in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, add 10 times of water gagings at every turn, extract for the first time 2.5 hours, extracted 1.0 hours for the second time, collecting decoction, filter, decompression (75 ℃ ,-0.07Mpa) be concentrated into the extractum that relative density is 1.20～1.25 (75～80 ℃); Add appropriate amount of starch and mix, mix cream with extractum, drying under reduced pressure (70 ℃ ,-0.07MPa), be ground into fine powder, mixing, the general ball of making of water, drying, 1000g is made in packing, promptly.
Embodiment 7 bolus of drug of the present invention and the contrast of former granule:
One, dosage form contrast
Bolus of drug prescription of the present invention derives from the 02nd contained kind of " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation " SHENSHITONG CHONGJI (granule) (WS
3-B-0304-90) ", for Xuhua Pharmaceutical Co., Ltd., Sichuan changes the exclusive new drug that agent forms on the logical particulate basis of the original nephrolith of company.Function cures mainly: clearing away heat-damp and promoting diuresis, promoting blood circulation and stopping pain, fossil, calculus.Be used for renal calculus, pyelolithiasis, vesical calculus, ureteral calculus.This medicine is the general enriched pellet of water, leads on the granule comparison dosage form with former dosage form nephrolith to have a clear superiority in.
" bolus of drug of the present invention " compares with " nephrolith leads to granule " dosage form
The logical granule of bolus of drug of the present invention and nephrolith compares: directly oral, do not need warm boiled water, and take more convenient; Directly oral, part is covered the preparation astringent taste, more helps the patient and takes; Obey into dose day and be reduced to by former dosage form day clothes patent medicine 30g and pill day obey into dose 4g, day obeying into dose obviously reduces.Overcome the shortcoming of the granule moisture absorption, stability is good.Have simultaneously carry, characteristics such as storage, convenient transportation, therefore, and have a clear superiority on the logical granule comparison bolus of drug dosage form of the present invention of former dosage form nephrolith.
Two, technology contrast
Bolus of drug of the present invention has been optimized the extraction process parameter by experiment of single factor research; By Study on Forming, reduce supplementary product kind and consumption, made the pill dosage form, more reasonable with the technology that the logical granule of former nephrolith compares bolus of drug of the present invention.
" bolus of drug of the present invention " compares with " nephrolith leads to granule " technology
The logical granule of bolus of drug of the present invention and nephrolith compares: extraction process has been optimized extraction process by experiment of single factor research, makes paste-forming rate bring up to 11.80% from 9.02%; Add the adjuvant aspect and study the minimizing supplementary product consumption by experiment, make day obey into dose and obviously reduce, be suitable for the crowd because of using Icing Sugar to enlarge patent medicine simultaneously; After moulding process is made enriched pellet by Study on Forming water is general, have a clear superiority on the dosage form with on the logical granule comparison dosage form of former dosage form nephrolith; Starch and water concentration contract after extractum mixes, and increase by one time drying under reduced pressure, are well positioned to meet the general pill requirement of water; Suitably reduced baking temperature (becoming before and after the ball), made into pharmaceutically active ingredient and destroy still less.Therefore, more reasonable with the technology of the logical granule comparison of former nephrolith bolus of drug of the present invention.
Three, quality standard contrast
Bolus of drug of the present invention is differentiated and the assay project by increasing thin layer on the basis of the logical granular mass standard of nephrolith, has improved quality standard significantly, makes the quality of the pharmaceutical preparations have more controllability, and the end product quality that dispatches from the factory is more stable.
" bolus of drug of the present invention " compares with " nephrolith leads to granule " quality standard
The logical granular mass standard of former nephrolith does not have thin layer and differentiates and the assay project, bolus of drug of the present invention increases by methodological study that Rhizoma Corydalis, Radix Salviae Miltiorrhizae thin layer are differentiated and quercetin content is measured and (seen application number: 200510021405.4, the applying date: on August 4th, 2005), improved quality standard significantly, make the quality of the pharmaceutical preparations have more controllability, the end product quality that dispatches from the factory is more stable.
Four, dose contrast
After bolus of drug of the present invention is made piller, obeying under the identical situation of crude drug amount with logical granule day of nephrolith, bolus of drug day of the present invention obeys into dose and obviously reduces, and is former nephrolith logical particulate 1/7.5.
" bolus of drug of the present invention " compares with " nephrolith leads to granule " dose
Logical granule day of former nephrolith obeys the crude drug amount and is: 15.3g, and day obeys into dose and is: 30g; Bolus of drug day of the present invention is obeyed the crude drug amount: 15.3g, day obeys into dose and is: 4g.Obeying under the identical situation of crude drug amount with logical granule day of nephrolith, bolus of drug day of the present invention obeys into dose and obviously reduces, and is former nephrolith logical particulate 1/7.5.
Claims (3)
- One kind prepare have fossil, the method for the pharmaceutical composition of calculus effect, it is characterized in that it comprises the steps:A, take off herbal raw material and the pharmaceutic adjuvant of stating percentage by weight,Herbal raw material:Herba Lysimachiae 15-18% Semen Vaccariae (parched) 15-18% Herba Polygoni Avicularis 9-12%Rhizoma Corydalis (processed with vinegar) 4-6% scalds Endothelium Corneum Gigeriae Galli 6-8% Radix Salviae Miltiorrhizae 6-8%Radix Aucklandiae 3-5% Herba Dianthi 8-11% Radix Achyranthis Bidentatae 4-6%Spora Lygodii 6-8%Pharmaceutic adjuvant:Starch 11-13%;In b, the described 10 flavor herbal raw materials, getting Spora Lygodii, Semen Vaccariae packs in the cloth bag, decoct with water secondary with eight flavors such as all the other Herba Lysimachiaes, add 10 times of water gagings at every turn, extract for the first time 2.5 hours, extracted collecting decoction 1.0 hours for the second time, filter, at 75 ℃, being evaporated to relative density under the-0.07Mpa condition is 1.20～1.25, the extractum that temperature is 75～80 ℃; Add starch, the starch addition is counted its 1 times of amount with the dried cream of theory, mixes, and mixes cream, at 70 ℃, drying under reduced pressure under the condition of-0.07Mpa is ground into fine powder, mixing, water is general makes female ball, adds the general piller of making of residue recipe quantity starch secondary, and drying promptly gets pill; The mean diameter of described parent nucleus is the 1.5-2 millimeter.
- 2. preparation of drug combination method according to claim 1 is characterized in that: it is the pill that is prepared into by the herbal raw material of following weight percentage ratio and pharmaceutic adjuvant,Herbal raw material:Herba Lysimachiae 17.1% Semen Vaccariae (parched) 17.1% Herba Polygoni Avicularis 10.3%Rhizoma Corydalis (processed with vinegar) 5.1% scalds Endothelium Corneum Gigeriae Galli 6.9% Radix Salviae Miltiorrhizae 6.9%The Radix Aucklandiae 3.4% Herba Dianthi 8.6% Radix Achyranthis Bidentatae 5.1%Spora Lygodii 6.9%Pharmaceutic adjuvant:Starch 12.6%.
- 3. preparation of drug combination method according to claim 1 and 2 is characterized in that, every gram contains Herba Lysimachiae, Herba Polygoni Avicularis with Quercetin C in the pill 15O 10H 7Meter must not be less than 0.18 milligram.
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| CN102133272B (en) * | 2011-03-24 | 2012-12-26 | 江苏苏南药业实业有限公司 | Preparation method of granules for treating nephrolith |
| CN102716196A (en) * | 2012-07-07 | 2012-10-10 | 广州汉方现代中药研究开发有限公司 | Preparation method for sugarless Shenshitong granule |
| CN102988497A (en) * | 2012-08-23 | 2013-03-27 | 江苏苏南药业实业有限公司 | Preparation method of sugar-free Shenshitong granules |
| CN104644954B (en) * | 2013-11-19 | 2017-12-01 | 南阳医学高等专科学校 | A kind of Chinese herbal medicine for treating stone in urinary system |
| CN105998285A (en) * | 2016-06-12 | 2016-10-12 | 莫佳 | Traditional Chinese medicine preparation for treating urinary calculi and preparation method thereof |
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