CN1839982A - Prostatitis-treating capsule and its preparing method and quality control method - Google Patents
Prostatitis-treating capsule and its preparing method and quality control method Download PDFInfo
- Publication number
- CN1839982A CN1839982A CN 200610038154 CN200610038154A CN1839982A CN 1839982 A CN1839982 A CN 1839982A CN 200610038154 CN200610038154 CN 200610038154 CN 200610038154 A CN200610038154 A CN 200610038154A CN 1839982 A CN1839982 A CN 1839982A
- Authority
- CN
- China
- Prior art keywords
- add
- radix
- time
- adds
- fine powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a tablet for treating prostatitis and its preparing process, wherein the tablet is prepared from corktree bark, radix paeoniae rubrathe, root of red rooted saliva, peach kernels, eupatene, spicebush root, seed of cowherb, dahurian angelica root through disintegrating into fines, heating with water, concentrating the filtrate into grease, decompressing and drying, disintegrating into fines, obtaining granules and loading into capsules.
Description
Technical field
The present invention relates to a kind of Chinese medicine, be specifically related to the Preparation method and its quality control technique of new Chinese medicine prostatitis-treating capsule.
Background technology
ANLIETONG PIAN is that office of National Drug Administration issues standard country standard for traditional Chinese medicines compilation (Chinese patent medicine provincial standard rising national standard part) surgery gynecological fascicle and records kind, consider in the former tablet that production technology defective and capsule be convenient to take, can improve medicine stability and bioavailability.So the applicant has carried out secondary research and development and innovation to this kind, is developed into capsule with new technology.
Prostatitis-treating capsule is on the basis of former tablet manufacturing technology, and further clear and definite extracting in water multiple overcomes former technology weak point in the extraction process, adds new adjuvant pregelatinized Starch etc. and make capsule as excipient in moulding process.
Summary of the invention
The purpose of this invention is to provide Chinese medicine new Chinese medicine prostatitis-treating capsule and preparation method thereof, Quality Control Technology.Prostatitis-treating capsule has clearing away heat-damp and promoting diuresis, the effect of blood circulation promoting and blood stasis dispelling.Be used for syndrome of stagnant dampness-heat, disease is seen: frequent micturition, and urgent micturition, it is not smooth to urinate, lower abdominal distention pain etc.Taking convenience has improved the usage degree of effective ingredient in the medical material.
Technical scheme of the present invention illustrates in the specific embodiment.
Concrete loop embodiment
Embodiment 1:
(1) prescription: Cortex Phellodendri 200g Radix Paeoniae Rubra 200g Radix Salviae Miltiorrhizae 100g Semen Persicae 140g
Herba Lycopi 120g Radix Linderae 120g Semen Vaccariae 80g Radix Angelicae Dahuricae 80g
Pregelatinized Starch 4g
More than make 1000.
(2) method for making: Cortex Phellodendri powder is broken into fine powder, and is standby; Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water gagings and are heated to 80 ℃, add Semen Persicae again, continue heating and decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filtered, filtrate is condensed into thick paste, and drying under reduced pressure is ground into fine powder; Above-mentioned fine powder and pregelatinized Starch mixing are made granule, incapsulate, promptly.
" doubly amount " definition among the present invention: w/v, unit are g/ml.
(3) extraction solvent (water) consumption is investigated
1. water absorption rate is investigated
Take by weighing Radix Paeoniae Rubra 40g Radix Salviae Miltiorrhizae 20g, Semen Persicae 28g, Herba Lycopi 24g, Radix Linderae 24g, Semen Vaccariae 16g, Radix Angelicae Dahuricae 16g, totally three parts, add 20 times of water gagings respectively, soak after 45 minutes, unnecessary unabsorbed water to be poured out, measurement volumes is calculated water absorption rate, the results are shown in Table 1.
Table 1 water absorption rate is investigated the result
| Tested number | Water absorption rate (%) | Meansigma methods (%) |
| 1 2 3 | 110.1 119.0 113.1 | 114.1 |
The result shows: the average water absorption rate of medical material is 114.1%.
2. extraction solvent (water) consumption is investigated
● instrument and reagent, experiment equipment
LC-10ATP type infusion pump (day island proper Tianjin company); SPD-10AVP type detector (day island proper Tianjin company) JS-3050 chromatographic work station (big Liaanjiang county Shengong department); Chromatographic column: Diamonsil-C
18(150 * 4.6mm, 5 μ m; Di Ma company).
The peoniflorin reference substance: Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides, lot number: 110736-200423.
Agents useful for same is that chromatographically pure, water are the distilled water except that acetonitrile, and other reagent is analytical pure.
● determining of evaluation index
Consider the prostatitis-treating capsule clearing away heat-damp and promoting diuresis, blood circulation promoting and blood stasis dispelling.Be used for dampness and heat stasis disease, disease is seen: frequent micturition, and urgent micturition, it is not smooth to urinate, lower abdominal distention pain etc." principal agent in the Radix Paeoniae Rubra side of being, peoniflorin is the drug effect position, thus its be index components be again active component, so select paeoniflorin content as one of evaluation index.Simultaneously, the paste-forming rate height has certain influence to preparations shaping among the preparation technology in the extraction process, so take all factors into consideration, selects paeoniflorin content and paste-forming rate as evaluation index.
● paste-forming rate is measured
Take by weighing Radix Paeoniae Rubra 40g, Radix Salviae Miltiorrhizae 20g, Semen Persicae 28g, Herba Lycopi 24g, Radix Linderae 24g, Semen Vaccariae 16g, Radix Angelicae Dahuricae 16g, extract merge extractive liquid, with the different water yields shown in the factor level table, put and be concentrated into thick paste in the water-bath, put again drying baker in 80 ℃ of drying under reduced pressure to constant weight, calculate paste-forming rate, promptly.
● paeoniflorin content is measured
Measure 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; Nitrile-0.1% phosphoric acid (13:87) is mobile phase; Detect wavelength 230nm.Number of theoretical plate calculates by the peoniflorin peak should be not less than 2500.
It is an amount of that the preparation precision of reference substance solution takes by weighing the peoniflorin reference substance, adds 50% methanol and make the solution that every 1ml contains 40 μ g, promptly.
The dry extract under " paste-forming rate mensuration " item is got in the preparation of need testing solution, and porphyrize is got about 0.15g, and accurate the title decides, add 50% methanol 30ml, supersound extraction 30 minutes filters, and filtrate is put evaporate to dryness in the water-bath, residue adds water 10ml gradation heating makes dissolving, filters, and filtrate is added on polyamide column (40 orders, the 4.0g that has handled well, post 1.8cm, dry column-packing) on, add water 50ml eluting, collect eluent, move in the 50ml measuring bottle, thin up is to scale, close plug shakes up, promptly.
Accurate reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure promptly.
● the factor level design
On the basis that water absorption rate is investigated, we choose 3 levels, promptly add 6,8,10 times of amounts and carry out optimal process, and to measure paste-forming rate and paeoniflorin content as evaluation index, the factor level design sees Table 2.
Table 2 factor level table
● experimental result
We select three levels, promptly add 6,8,10 times of amount solvents and carry out the investigation of extraction solvent (water) consumption, test as its evaluation index to measure paeoniflorin content and paste-forming rate, the factor level arrangement sees Table 3, each test takes by weighing Radix Paeoniae Rubra 40g, Radix Salviae Miltiorrhizae 20g, Semen Persicae 28g, Herba Lycopi 24g, Radix Linderae 24g, Semen Vaccariae 16g, Radix Angelicae Dahuricae 16g extraction solvent (water) the consumption scheme operation by EXPERIMENTAL DESIGN, measure paeoniflorin content and paste-forming rate respectively and calculate the peoniflorin total amount down with above-mentioned " evaluation index " item, 2 parts of each test operation repetitives the results are shown in Table 3.
Table 3 extraction solvent (water) consumption is investigated result of the test (n=2)
| Extraction solvent (doubly) extraction time (h) | Paste-forming rate (%) | Dry extract heavy (g) | Paeoniflorin content * (mg/g) | Peoniflorin total amount (mg) |
| 6(2、1.5、1) 8(2、1.5、1) 10(2、1.5、1) | 10.02 11.43 11.92 | 16.83 19.20 20.03 | 12.68 12.89 11.20 | 213.4 247.5 224.3 |
* annotate: paeoniflorin content in every g dry extract.
The result shows: 8 times of amount solvent extraction effects all are better than 6,10 times of amounts, and from the actual consideration of suitability for industrialized production, selective extraction technology is extracted three times for adding 8 times of amount solvents, and 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time.
3. extraction process by water demonstration test
For investigating the stability of above-mentioned preferred extraction process, take by weighing Radix Paeoniae Rubra 200g, Radix Salviae Miltiorrhizae 100g, Semen Persicae 140g, Herba Lycopi 120g, Radix Linderae 120g, Semen Vaccariae 80g, Radix Angelicae Dahuricae 80g, three parts, by above-mentioned preferred manufacturing procedure preparation, get paste-forming rate and survey paeoniflorin content and calculate the peoniflorin total amount, the results are shown in Table 4.
Table 4 extraction process by water checking scale-up
| Tested number | Paste-forming rate (%) | Dry extract heavy (g) | Paeoniflorin content * (mg/g) | Peoniflorin total amount (mg) |
| 1 2 3 | 11.42 11.48 11.45 | 95.93 96.43 96.18 | 12.82 12.90 12.61 | 1229.8 1243.9 1212.8 |
* annotate: paeoniflorin content in every g dry extract.
The result shows that 8 times of water gaging extraction processes of selection are stablized feasible.According to above-mentioned experimental result, establish extraction process by water and decoct three times for adding 8 times of water gagings, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time.
4. baking temperature is investigated
Because the dry sample that obtains easily hardens under the condition of normal pressure, drying time is long, so this product adopts drying under reduced pressure, take by weighing Radix Paeoniae Rubra 40g, Radix Salviae Miltiorrhizae 20g, Semen Persicae 28g, Herba Lycopi 24g, Radix Linderae 24g, Semen Vaccariae 16g, Radix Angelicae Dahuricae 16g prepares thick paste by screening technology, be divided into three parts and be tiled on the porcelain dish, the about 1cm of thickness is respectively at 60 ℃, 80 ℃, 105 ℃ drying under reduced pressure, with drying time, paeoniflorin content, whether breeze is arranged is that index is investigated, and the results are shown in Table 5.
Table 5 thick paste drying test result
| Temperature (℃) | Drying time (h) | Paeoniflorin content (mg/g) * | Character |
| 60 80 105 | 7.8 4.8 3.1 | 12.78 12.74 12.86 | No breeze does not have breeze a small amount of breeze is arranged |
* annotate: paeoniflorin content in every g dry extract.
The result shows: though 105 ℃ of drying times are short, have a small amount of breeze to occur, 60 ℃ of drying times are oversize, so select 80 ℃ to be this kind drying process.
5. prescription screening and result of the test
According to capsule molding requirement, get " extraction process by water demonstration test " experiment number 1 extractum down, as investigating index the molding prescription is screened disintegration with moisture, flowability and the capsule of capsule 's content, fill a prescription and the results are shown in Table 6.
Table 6 capsule shaping formula table
| Sequence number | 1 | 2 | 3 | 4 |
| Cortex Phellodendri powder (g) | 20.0 | 20.0 | 20.0 | 20.0 |
| Dry extract (g) starch (g) pregelatinized Starch (g) microcrystalline Cellulose (g) | 9.6 - - - | 9.6 0.4 - - | 9.6 - 0.4 - | 9.6 - - 0.4 |
| Water flow disintegration (min) | Up to specification general 25 | Up to specification general 20 | Up to specification 17 | Up to specification general 19 |
The result shows: every index of prescription 3 all is better than other prescription, so select prescription 3 as capsular optimum formula.
7. moulding process is verified scale-up and is detected data
Get down experiment number 2,3 extractum of Cortex Phellodendri and " extraction process by water demonstration test ", prepare 2 lot number prostatitis-treating capsules and detect, the results are shown in Table 7, table 8 by the preparation technology of screening.
Table 7 capsule shaping confirmatory experiment result
| Lot number | Cortex Phellodendri (g) | Extract powder (g) | Pregelatinized Starch (g) | Finished product number (grain) |
| 050201 050202 | 200 200 | 96.43 96.18 | 4 4 | 975 970 |
Table 8 capsule shaping confirmatory experiment detects data
| Lot number | Character | Moisture (%) | Content uniformity | Disintegration (min) | Paeoniflorin content (mg/ grain) | Microbial limit * |
| 050,201 050202 | Content is brown granule; Mildly bitter flavor, puckery.Content is brown granule; Mildly bitter flavor, puckery. | 3.4 3.4 | Up to specification | 19 18 | 1.30 1.32 | Up to specification |
Embodiment 2:
(1) prescription: Cortex Phellodendri 200g Radix Paeoniae Rubra 200g Radix Salviae Miltiorrhizae 100g Semen Persicae 140g
Herba Lycopi 120g Radix Linderae 120g Semen Vaccariae 80g Radix Angelicae Dahuricae 80g
Magnesium stearate 1.5g
More than make 1000.
(2) method for making
More than eight flavors, getting Radix Paeoniae Rubra, to be ground into fine powder standby; Cortex Phellodendri powder is broken into coarse powder, adds to contain 1% tart 70% alcohol reflux three times, and the first time, 8 times of amounts were 1.5 hours, and 6 times of amounts of second and third time 1 hour filter, and merging filtrate reclaims ethanol, gets concentrated solution; Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water gagings and are heated to 80 ℃, add Semen Persicae again, continue heating and decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filters, and filtrate and above-mentioned concentrated solution merge, be condensed into thick paste, drying under reduced pressure is ground into fine powder, add Radix Paeoniae Rubra fine powder mixing, make granule, add magnesium stearate, mixing incapsulates, promptly.
Embodiment 3:
(1) prescription: Cortex Phellodendri 200g Radix Paeoniae Rubra 200g Radix Salviae Miltiorrhizae 100g Semen Persicae 140g
Herba Lycopi 120g Radix Linderae 120g Semen Vaccariae 80g Radix Angelicae Dahuricae 80g
Starch 10g magnesium stearate 1.5g
More than make 1000.
(2) method for making: above eight flavors, getting Radix Paeoniae Rubra, to be ground into fine powder standby; Cortex Phellodendri powder is broken into coarse powder, adds to contain 1% tart 70% alcohol reflux three times, and the first time, 8 times of amounts were 1.5 hours, and 6 times of amounts of second and third time 1 hour filter, and merging filtrate reclaims ethanol, gets concentrated solution A; Radix Salviae Miltiorrhizae, the Radix Angelicae Dahuricae, the Radix Linderae add 60% alcohol reflux secondary, measure 2 hours for 8 times for the first time, measure 1 hour for 6 times for the second time, filter, and merging filtrate reclaims ethanol, gets concentrated solution B; Semen Vaccariae adds 8 times of water gagings and is heated to 80 ℃, adds Semen Persicae again, continues heating and decocts three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filters, and filtrate and above-mentioned concentrated solution merge, be condensed into thick paste, drying under reduced pressure is ground into fine powder, add Radix Paeoniae Rubra fine powder, starch mixing, make granule, drying, add the magnesium stearate mixing, incapsulate, promptly.
Embodiment 4:
(1) prescription: Cortex Phellodendri 200g Radix Paeoniae Rubra 200g Radix Salviae Miltiorrhizae 100g Semen Persicae 140g
Herba Lycopi 120g Radix Linderae 120g Semen Vaccariae 80g Radix Angelicae Dahuricae 80g
Microcrystalline Cellulose 40g
More than make 1000.
(2) method for making: above eight flavors, Cortex Phellodendri powder is broken into coarse powder, adds to contain 1% tart 70% alcohol reflux three times, and the first time, 8 times of amounts were 1.5 hours, and 6 times of amounts of second and third time 1 hour filter, and merging filtrate reclaims ethanol, gets concentrated solution A; Radix Salviae Miltiorrhizae, the Radix Angelicae Dahuricae, the Radix Linderae add 60% alcohol reflux secondary, measure 2 hours for 8 times for the first time, measure 1 hour for 6 times for the second time, filter, and merging filtrate reclaims ethanol, gets concentrated solution B; Radix Paeoniae Rubra, Semen Vaccariae add 8 times of water gagings and are heated to 80 ℃, add Semen Persicae again, continue heating and decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filters, and filtrate and above-mentioned concentrated solution merge, be condensed into thick paste, drying under reduced pressure is ground into fine powder, add the microcrystalline Cellulose mixing, make granule, incapsulate, promptly.
Quality Control Technology
[character] prostatitis-treating capsule is a capsule, and content is brown to tan granule; Mildly bitter flavor, puckery.
Prostatitis-treating capsule content 4g is got in [discriminating] (1), porphyrize, and the 20ml that adds diethyl ether, supersound process 20 minutes discards ether solution, and medicinal residues volatilize, and add methanol 20ml, and supersound process 20 minutes filters, and filtrate is concentrated into 2ml, as need testing solution.Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution (12: 6: 3: 3: 1) is developing solvent, put in the pre-saturated expansion cylinder of ammonia steam, launch, take out, dry.Put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(2) get prostatitis-treating capsule content 4g, porphyrize adds ethyl acetate 50ml, and reflux 1 hour filters, and filtrate is reclaimed ethyl acetate to doing, and residue adds ethanol 2ml makes dissolving, as need testing solution.Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid (40: 5: 10: 0.2) be developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing in 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-0.1% phosphoric acid (13: 87) is mobile phase; Detect wavelength 230nm.Number of theoretical plate calculates by the Hesperidin peak should be not less than 2500.
The preparation precision of reference substance solution takes by weighing that to put 36 hours peoniflorin reference substance of phosphorus pentoxide drying under reduced pressure an amount of, adds 50% methanol and makes the solution that every 1ml contains 40 μ g, and close plug shakes up, promptly.
The content under the content uniformity item is got in the preparation of need testing solution, and porphyrize is got about 0.5g, and accurate the title decides, add 50% methanol 30ml, supersound extraction 30 minutes filters, and filtrate is put evaporate to dryness in the water-bath, residue adds water 10ml gradation heating makes dissolving, filters, and filtrate is added on polyamide column (40 orders, the 4.0g that has handled well, post 1.8cm, dry column-packing) on, add water 50ml eluting, collect eluent, move in the 50ml measuring bottle, thin up is to scale, close plug shakes up, promptly.
Accurate respectively reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of prostatitis-treating capsule contains Radix Paeoniae Rubra in peoniflorin (C23H28O11), must not be less than 1.0mg.
[function cures mainly] clearing away heat-damp and promoting diuresis, blood circulation promoting and blood stasis dispelling.Be used for syndrome of stagnant dampness-heat, disease is seen: frequent micturition, and urgent micturition, it is not smooth to urinate, lower abdominal distention pain etc.
[usage and dosage] is oral, one time 4～6,3 times on the one; Or follow the doctor's advice.
[specification] every dress 0.3g
[storage] sealing.
Claims (4)
1, prostatitis-treating capsule, crude drug is made up of Cortex Phellodendri, Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Semen Persicae, Herba Lycopi, the Radix Linderae, Semen Vaccariae, the Radix Angelicae Dahuricae, it is characterized in that:
(1) the formulation weight ratio is:
Cortex Phellodendri 200 Radix Paeoniae Rubra 200 Radix Salviae Miltiorrhizaes 100 Semen Persicaes 140
Herba Lycopi's 120 Radixs Linderae 120 Semen Vaccariae 80 Radixs Angelicae Dahuricae 80
(2) adjuvant comprises: starch, pregelatinized Starch, dextrin, microcrystalline Cellulose, calcium hydrogen phosphate, micropowder silica gel, Pulvis Talci, carboxymethyl starch sodium, magnesium stearate etc.
2, the preparation method of prostatitis-treating capsule according to claim 1 is characterized in that comprising:
Preparation method is 1.: Cortex Phellodendri powder is broken into fine powder, and is standby; Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add water and are heated to 60-90 ℃, add Semen Persicae again and decoct, and collecting decoction filters, and filtrate is condensed into thick paste, and drying under reduced pressure is ground into fine powder; Above-mentioned fine powder and pregelatinized Starch mixing are made granule, incapsulate, promptly;
Preparation method is 2.: above eight flavors, and getting Radix Paeoniae Rubra, to be ground into fine powder standby; Cortex Phellodendri powder is broken into coarse powder, adds alcohol reflux three times, filters, and merging filtrate reclaims ethanol, gets concentrated solution; Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add water and are heated to 60～90 ℃, add Semen Persicae again, continue heating and decoct three times, collecting decoction filters, and filtrate and above-mentioned concentrated solution merge, be condensed into thick paste, drying under reduced pressure is ground into fine powder, add Radix Paeoniae Rubra fine powder mixing, make granule, add magnesium stearate, mixing, incapsulate, promptly;
Preparation method is 3.: above eight flavors, and getting Radix Paeoniae Rubra, to be ground into fine powder standby; Cortex Phellodendri powder is broken into coarse powder, adds alcohol reflux three times, filters, and merging filtrate reclaims ethanol, gets concentrated solution A; Radix Salviae Miltiorrhizae, the Radix Angelicae Dahuricae, the Radix Linderae add the alcohol reflux secondary, filter, and merging filtrate reclaims ethanol, gets concentrated solution B; Semen Vaccariae adds water and is heated to 60～90 ℃, adds Semen Persicae again, continues heating and decocts three times, collecting decoction filters, and filtrate and above-mentioned concentrated solution merge, be condensed into thick paste, drying under reduced pressure is ground into fine powder, add Radix Paeoniae Rubra fine powder, starch mixing, make granule, drying adds the magnesium stearate mixing, incapsulate, promptly;
Preparation method is 4.: above eight flavors, Cortex Phellodendri powder is broken into coarse powder, adds to contain alcohol reflux three times, filters, merging filtrate reclaims ethanol, concentrated solution A; Radix Salviae Miltiorrhizae, the Radix Angelicae Dahuricae, the Radix Linderae add the alcohol reflux secondary, filter, and merging filtrate reclaims ethanol, gets concentrated solution B; Radix Paeoniae Rubra, Semen Vaccariae add water and are heated to 60～90 ℃, add Semen Persicae again, continue heating and decoct three times, and collecting decoction filters, filtrate and above-mentioned concentrated solution merge, and are condensed into thick paste, and drying under reduced pressure is ground into fine powder, add the microcrystalline Cellulose mixing, make granule, incapsulate, promptly.
3, preparation method according to claim 2 is characterized in that its concrete steps are respectively:
Preparation method 1. concrete steps is: Cortex Phellodendri powder is broken into fine powder, and is standby; Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water gagings and are heated to 80 ℃, add Semen Persicae again, continue heating and decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filtered, filtrate is condensed into thick paste, and drying under reduced pressure is ground into fine powder; Above-mentioned fine powder and pregelatinized Starch mixing are made granule, incapsulate, promptly;
Preparation method 2. concrete steps is: above eight flavors, and getting Radix Paeoniae Rubra, to be ground into fine powder standby; Cortex Phellodendri powder is broken into coarse powder, adds to contain 1% tart 70% alcohol reflux three times, and the first time, 8 times of amounts were 1.5 hours, and 6 times of amounts of second and third time 1 hour filter, and merging filtrate reclaims ethanol, gets concentrated solution; Radix Salviae Miltiorrhizae, Herba Lycopi, the Radix Linderae, Semen Vaccariae and the Radix Angelicae Dahuricae add 8 times of water gagings and are heated to 80 ℃, add Semen Persicae again, continue heating and decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filters, and filtrate and above-mentioned concentrated solution merge, be condensed into thick paste, drying under reduced pressure is ground into fine powder, add Radix Paeoniae Rubra fine powder mixing, make granule, add magnesium stearate, mixing incapsulates, promptly;
Preparation method 3. concrete steps is: above eight flavors, and getting Radix Paeoniae Rubra, to be ground into fine powder standby; Cortex Phellodendri powder is broken into coarse powder, adds to contain 1% tart 70% alcohol reflux three times, and the first time, 8 times of amounts were 1.5 hours, and 6 times of amounts of second and third time 1 hour filter, and merging filtrate reclaims ethanol, gets concentrated solution A; Radix Salviae Miltiorrhizae, the Radix Angelicae Dahuricae, the Radix Linderae add 60% alcohol reflux secondary, measure 2 hours for 8 times for the first time, measure 1 hour for 6 times for the second time, filter, and merging filtrate reclaims ethanol, gets concentrated solution B; Semen Vaccariae adds 8 times of water gagings and is heated to 80 ℃, adds Semen Persicae again, continues heating and decocts three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filters, and filtrate and above-mentioned concentrated solution merge, be condensed into thick paste, drying under reduced pressure is ground into fine powder, add Radix Paeoniae Rubra fine powder, starch mixing, make granule, drying, add the magnesium stearate mixing, incapsulate, promptly;
Preparation method 4. concrete steps is: above eight flavors, and Cortex Phellodendri powder is broken into coarse powder, adds to contain 1% tart 70% alcohol reflux three times, and the first time, 8 times of amounts were 1.5 hours, and 6 times of amounts of second and third time 1 hour filter, and merging filtrate reclaims ethanol, gets concentrated solution A; Radix Salviae Miltiorrhizae, the Radix Angelicae Dahuricae, the Radix Linderae add 60% alcohol reflux secondary, measure 2 hours for 8 times for the first time, measure 1 hour for 6 times for the second time, filter, and merging filtrate reclaims ethanol, gets concentrated solution B; Radix Paeoniae Rubra, Semen Vaccariae add 8 times of water gagings and are heated to 80 ℃, add Semen Persicae again, continue heating and decoct three times, 2 hours for the first time, 1.5 hours for the second time, 1 hour for the third time, collecting decoction filters, and filtrate and above-mentioned concentrated solution merge, be condensed into thick paste, drying under reduced pressure is ground into fine powder, add the microcrystalline Cellulose mixing, make granule, incapsulate, promptly.
4, the method for quality control of prostatitis-treating capsule is characterized in that differentiating and measuring by following steps:
(1) qualitative identification
A, get prostatitis-treating capsule content 4g, porphyrize, the 20ml that adds diethyl ether, supersound process 20 minutes discards ether solution, and medicinal residues volatilize, and add methanol 20ml, and supersound process 20 minutes filters, and filtrate is concentrated into 2ml, as need testing solution; Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution (12: 6: 3: 3: 1) is developing solvent, put in the pre-saturated expansion cylinder of ammonia steam, launch, take out, dry; Put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
B, get prostatitis-treating capsule content 4g, porphyrize adds ethyl acetate 50ml, and reflux 1 hour filters, and filtrate is reclaimed ethyl acetate to doing, and residue adds ethanol 2ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid (40: 5: 10: 0.2) be developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing in 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) quantitative assay
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-0.1% phosphoric acid (13: 87) is mobile phase; Detect wavelength 230nm; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2500;
The preparation of reference substance solution: precision takes by weighing that to put 36 hours peoniflorin reference substance of phosphorus pentoxide drying under reduced pressure an amount of, adds 50% methanol and makes the solution that every 1ml contains 40 μ g, and close plug shakes up, promptly;
The preparation of need testing solution: get the content under the content uniformity item, porphyrize is got about 0.5g, and accurate the title decides, add 50% methanol 30ml, supersound extraction 30 minutes filters, and filtrate is put evaporate to dryness in the water-bath, residue adds water 10ml gradation heating makes dissolving, filters, and filtrate is added on polyamide column (40 orders, the 4.0g that has handled well, post 1.8cm, dry column-packing) on, add water 50ml eluting, collect eluent, move in the 50ml measuring bottle, thin up is to scale, close plug shakes up, promptly;
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of prostatitis-treating capsule contains Radix Paeoniae Rubra with peoniflorin (C
23H
28O
11) meter, must not be less than 1.0mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100381545A CN100522198C (en) | 2006-01-28 | 2006-01-28 | Prostatitis-treating capsule and its preparing method and quality control method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100381545A CN100522198C (en) | 2006-01-28 | 2006-01-28 | Prostatitis-treating capsule and its preparing method and quality control method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1839982A true CN1839982A (en) | 2006-10-04 |
| CN100522198C CN100522198C (en) | 2009-08-05 |
Family
ID=37029285
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100381545A Expired - Fee Related CN100522198C (en) | 2006-01-28 | 2006-01-28 | Prostatitis-treating capsule and its preparing method and quality control method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100522198C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102526305A (en) * | 2012-02-14 | 2012-07-04 | 史志辉 | Chinese medicinal capsules for treating prostatitis and prostatic hyperplasia and preparation method for Chinese medicinal capsules |
| CN102805773A (en) * | 2012-08-27 | 2012-12-05 | 湖南华纳大药厂有限公司 | Qianlieantong capsule and preparation method thereof |
| CN107782816A (en) * | 2016-08-31 | 2018-03-09 | 天津中新药业研究中心 | A kind of detection method of clearing heat and detoxicating cool blood stranguria-treating drug |
-
2006
- 2006-01-28 CN CNB2006100381545A patent/CN100522198C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102526305A (en) * | 2012-02-14 | 2012-07-04 | 史志辉 | Chinese medicinal capsules for treating prostatitis and prostatic hyperplasia and preparation method for Chinese medicinal capsules |
| CN102805773A (en) * | 2012-08-27 | 2012-12-05 | 湖南华纳大药厂有限公司 | Qianlieantong capsule and preparation method thereof |
| CN107782816A (en) * | 2016-08-31 | 2018-03-09 | 天津中新药业研究中心 | A kind of detection method of clearing heat and detoxicating cool blood stranguria-treating drug |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100522198C (en) | 2009-08-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103784664A (en) | Dual-phase capsule for preventing and treating chronic pelvic inflammation and preparation method and detection method thereof | |
| CN101766771A (en) | Quality control method of medicine for gynecopathy treatment | |
| CN1806836A (en) | Chinese medicinal composition, its preparation process and quality control method | |
| CN100437112C (en) | Method for inspecting Chinese medicinal preparation quality in treatment of old man eyes dieases | |
| CN1839982A (en) | Prostatitis-treating capsule and its preparing method and quality control method | |
| CN1226033C (en) | Method for preparing traditional Chinese medicine concentrated pill | |
| CN1824239A (en) | Quality control method of kidney beneficial bone fortifying capsule | |
| CN1679811A (en) | Danshen root extract, production, medicine preparation and inspection thereof | |
| CN1879720A (en) | Blood platelet-increasing tablet, its preparation process and quality control method | |
| CN1907340A (en) | Quality checking and controlling method for renal stone removal preparation | |
| CN1840032A (en) | Granule for treating infant's rhinitis, its preparation method and quality control method | |
| CN1879850A (en) | Capsule with hairy vein agrimony and arenobufagin, its preparation process and quality control method | |
| CN102590423B (en) | Fingerprint spectrum determination method of ligusticum wallichii tea-blending granular preparation | |
| CN101647997B (en) | Influenza wind-dispelling capsule and preparation method and quality control method thereof | |
| CN1857445A (en) | Quality control method for Desheng preparation | |
| CN1879849A (en) | Compound capsule with pseudo-ginseng and Chinese fanpalm seed, its preparation process and quality control method | |
| CN107582639A (en) | A kind of vinegar corydalis tuber granule and preparation method thereof | |
| CN1943633A (en) | Pudilan antiphlogistic granules and its Pudilan antiphlogistic granules prepared by said method | |
| CN100518798C (en) | Dispersible tablet with gastrodia tuber for treating headache, and its testing method | |
| CN101711827A (en) | Traditional Chinese medicine preparation for clearing heat, cooling blood and nourishing yin and kidneys, preparation method and detection method thereof | |
| CN1857602A (en) | Quality control method for vatility source preparation | |
| CN101028474A (en) | Method for inspecting the quality of Chinese preparation with Yang-and kidney tonifying functions | |
| CN1923264A (en) | Capsule comprising artemisia capillaries and rhizoma imperatae for treating hepatitis | |
| CN1775240A (en) | Method for preparing Rukuaixiao Chewing tablet for eliminating mass of breast and its quality control technology | |
| CN1323676C (en) | Preparation method and quality control method of traditional Chinese medicine capsule for treating spleen and stomach weakness |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090805 Termination date: 20170128 |