CN1509733A - Compound Qingdai agent for inflammatory intestinal diseases - Google Patents
Compound Qingdai agent for inflammatory intestinal diseases Download PDFInfo
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- CN1509733A CN1509733A CNA021569509A CN02156950A CN1509733A CN 1509733 A CN1509733 A CN 1509733A CN A021569509 A CNA021569509 A CN A021569509A CN 02156950 A CN02156950 A CN 02156950A CN 1509733 A CN1509733 A CN 1509733A
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Abstract
A compound Chinese medicine for treating the inflammatory enteropathy, such as ulcerative colitis, chronic colitis, and diarrhea is prepared from 5 Chinese-medicinal materials including natural indigo, baked alum, Sichuan phelloden dron bark, catechu and pearl through pulverizing them except Sichuan phellodendron bark, extracting from Sichuan phellodendron bark in alcohol, recovering alcohol, drying pulverizing, and proportionally mixing all together. Its advantages are high biologic utilization rate and easy absorption.
Description
Affiliated technical field the present invention relates to utilize the Chinese medicine compound compositions of natural plants preparation treatment inflammatory bowel, and preparation method thereof.
The background technology inflammatory bowel comprises ulcerative colitis (UC) and crohn (CD), they are a kind of intractable refractory diseases, its pathogenesis is still not fully aware of, most scholars think excessively relevant with the intestinal local immune response, the present clinical medicine that curative effect is relatively affirmed, toxic and side effects is little that lacks does not still have specific treatment way.Therefore, people have in the little anti-UC curative of Comprehensive Treatment effect and toxic and side effects in research, attach great importance to the development and utilization of Chinese medicine.The applicant's seminar is engaged in the Chinese medicine Indigo Naturalis, and to treat this disease existing for many years, and delivered monograph, application new drug lot number, apply for a patent (the Chinese medicine Pulvis Indigo Naturalis of CN1202361A treatment inflammatory bowel, 1997.6.18).The processing technique of former Pulvis Indigo Naturalis is with after the conventional pulverizing of each component drugs, crosses 120 mesh sieve mixings and makes powder, capsule and suspension liquor.Craft precision is not high, and drug particles is thicker, and the purity and the bioavailability of medicine are low.Along with going deep into of research, find that also the component compatibility of patent application formerly is not good enough yet.
Summary of the invention the purpose of this invention is to provide a kind of compound indigo agent for the treatment of inflammatory bowel and expands preparation method.The compound indigo agent is used for the diarrhoea that ulcerative colitis, chronic colitis, clone disease etc. cause, by the medicinal plants preparation, it is characterized in that the component weight proportion is as follows: Indigo Naturalis 554g, dried Alumen 185g, Cortex Phellodendri 308g, catechu 148g, Margarita powder 61g.
The method of the Chinese medicine compound Indigo Naturalis agent of preparation treatment inflammatory bowel comprises and makes different dosage form, it is characterized in that Indigo Naturalis, dried Alumen, catechu pulverize separately are become fine powder, and Indigo Naturalis contains indigo (C
16H
10N
2O
2) must not be less than 2.0%; The ultra-fine dry type of Margarita is ground into the micropowder of fineness of the particles 5-10 μ m; Cortex Phellodendri adopts ethanol extraction, reclaims ethanol, and drying gets dry extract, and is ground into fine powder; With the powder of the above-mentioned five tastes constituent mixing that sieves, total amount is divided into 250 parts.Get 1/250 part of preparation by the pharmaceutical dosage proportioning.
Though the compound indigo agent of treatment inflammatory bowel of the present invention is identical with former Pulvis Indigo Naturalis component, the proportioning difference.Particularly preparation method is to patent application Pulvis Indigo Naturalis preparation technology's further improvement formerly.It adopts micronizing and purifying technique respectively, makes drug particles thinner, and the dissolubility of medicine is bigger, and bioavailability is higher, easier absorption after the coloclysis.Dosage form has also increased emulsifiable concentrates, has improved the selectance of effective dose.The purify advantage of process for refining of the present invention is the effective ingredient that makes full use of medicine, and the Indigo Naturalis granule of prepared of the present invention is that each composition medicine is broken into fine grained (5-10 μ m) through superfine powder.For example the main component of Cortex Phellodendri is a berberine, alkaloid such as jateorhizine, magnoflorine and compositions such as obacunone, obakulactone in order to extract effective ingredient in the Cortex Phellodendri to greatest extent, adopt 50% ethanol extraction Cortex Phellodendri to purify through ethanol, fiber content obviously reduces, and has improved craft precision greatly., and conditions such as the principal element that influence is extracted such as solvent consumption, concentration of alcohol, extraction time adopt orthogonal test, are that index is carried out intuitive analysis and variance analysis with preferred optimum extraction condition with the berberine rate of transform in the Cortex Phellodendri.After process modification, existing 5.0 gram Pulvis Indigo Naturaliss are identical with 4.0 gram Indigo Naturalis granule effective ingredient, medicine can be made powder, granule, Emulsion, capsule etc.Particularly the purity of Emulsion medicine this moment, dissolubility, bioavailability etc. obviously improve, and because of fiber content is few, stimulation reduces to gastrointestinal, and the sense of discomfort during patient's medication alleviates, and the retention time of coloclysis obviously prolongs.And because of the raising of pharmaceutical purity, be more conducive to make capsule and be convenient to patient and carry, clinical efficacy also further improves.
Appended drawings 1 is the inventive method operation block diagram:
The Chinese medicine compound Indigo Naturalis agent of specific embodiment treatment inflammatory bowel by the medicinal plants preparation, is characterized in that the component weight proportion is as follows: Indigo Naturalis 554g dried Alumen 185g Cortex Phellodendri 308g catechu 148g Margarita powder 61g.
The method of the Indigo Naturalis agent of preparation treatment inflammatory bowel, comprise different dosage forms such as making emulsifying agent, capsule, suppository, pill, it is characterized in that Indigo Naturalis, dried Alumen, catechu choose, pulverize, sieve, remove impurity, fine hair respectively, make fine powder, be equivalent to the 120-200 order, Indigo Naturalis contains indigo (C
16H
10N
2O
2) must not be less than 2.0%; The ultra-fine dry type of Margarita is ground into the micropowder of fineness of the particles 5-10 μ m; Cortex Phellodendri is with 50% ethanol extraction three times, and Cortex Phellodendri is with 50% ethanol extraction three times, and 8 times of amounts were extracted 2 hours for the first time, and second and third time is 6 times of amounts and extracted 1 hour, collects three times extracting solution, filtration, and recovery ethanol, drying under reduced pressure is ground into fine powder.The powder of above-mentioned five tastes constituent is crossed sieve No. six, and mixing is divided into 250 parts with total amount.Each dosage form is as the criterion for 1/250 part to contain the compound indigo agent, and pharmaceutical technology adds excipient routinely.
Granule: adopt the dextrin slurry to granulate for binding agent, dextrin slurry concentration is 5%, and addition is that the 65-70% of above-mentioned medicine medicated powder amount is good, with 5% dextrin slurry system soft material, granulates, and through 80 ℃ of dryings, makes 1000g, and the granulate packing promptly.Every packed 4g contains 1/250 part of compound indigo agent.The one-pass finished rate can reach 80-85%.
With the compound indigo agent that the present composition and method make, pharmaceutical dosage is oral: adult's amount: at every turn contain 1/250 part of compound indigo agent, twice of every day; Coloclysis or suppository: at every turn with containing 1/250 part of compound indigo agent or two parts.
The Indigo Naturalis variet complexity is done assay with high performance liquid chromatography.Meeting pharmacopeia 〉=2.0% regulation can feed intake.It is raw material that the present invention builds black pigment used by women in ancient times to paint their eyebrows group authentic medicinal herbs with Fujian Province, contains indigo and reaches 2.4%.
[character] this product is the navy blue granule, bitter in the mouth.
[inspection] should meet the every regulation (appendix IB of Chinese Pharmacopoeia version in 2000) under the granule item.
[assay] measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler, and methanol-water (60: 40) is a mobile phase, and the detection wavelength is 604nm, flow velocity: 1.0ml/min, and number of theoretical plate calculates by indigo chromatographic peak, should be not less than 5000.
The preparation of reference substance solution: get indigo reference substance 3.50mg, accurate claim surely, put in the 50ml measuring bottle, add chloroform 40ml dissolving, supersound process made dissolving in 5 minutes, put coldly, added chloroform and was diluted to scale, shook up, and filtered and made the reference substance solution that every 1ml contains 0.07mg.
The preparation of need testing solution: get content uniformity and check item sample down, porphyrize is got 0.14g, porphyrize, the accurate title, decide, and puts in the flask, add chloroform 90ml, reflux, extract, 2 hours is put cold, filter, filtrate is put in the 100ml measuring bottle, adds chloroform and is diluted to scale, shakes up, filtrate filters through microporous filter membrane, gets subsequent filtrate as need testing solution.
Algoscopy: accurate reference substance solution and each 5 μ l of need testing solution of drawing, inject chromatograph of liquid, measure chromatographic peak area, calculate, promptly.
The every gram of this product contains Indigo Naturalis by indigo (C
10H
10N
2O
2) calculate, must not be less than 9mg.
[storage] sealing, shady and cool dry place.
The described Margarita micropowderization of the inventive method: pulverize with QLM-IV model airflow milling, adopt ultra-fine dry type to be ground into the micropowder of fineness of the particles 5-10 μ m Margarita.Compressed Gas is accelerated into supersonic airstream through jet pipe and injects pulverizing chamber, head-on collision is broken mutually after high velocity air quickens for material in the pulverizing chamber, material after the pulverizing is delivered to graded region by air-flow, sub-elect the powder of required fineness by grading wheel, the coarse powder of backlog demand returns milling zone to be continued to grind, fine powder enters catcher with air-flow and collects, and air filters and enters atmosphere.It is standby to collect 5-10 μ m micropowder.
Result of the test sees Table 1
Table 1
Margarita coarse granule (g) airflow milling model micropowder amount (g) level of residue (g) flour extraction (%)
1000??????QLM-IV??????965??????25??????96.5
1000??????QLM-IV??????960??????28??????96
1000??????QLM-IV??????975??????18??????97.5
Cortex Phellodendri of the present invention, select Cortex Phellodendri for use according to the clinical application experience, main component is a berberine in this medicine, alkaloid such as jateorhizine, magnoflorine and compositions such as obacunone, obakulactone, in order to extract effective ingredient in the Cortex Phellodendri to greatest extent, adopt ethanol extraction, and conditions such as the principal element that influence is extracted such as solvent consumption, concentration of alcohol, extraction time adopting orthogonal test, is that index is carried out intuitive analysis and variance analysis with preferred optimum extraction condition with the berberine rate of transform in the Cortex Phellodendri.
Table 9
| The airflow milling model | Granularity (μ m) | Flour extraction (%) | Minimum crushing quantity (kg) | Pulverizing speed (kg/h) | The place of production |
| ?QLM-IV | ?5-10 | ?95-98 | ?0.5 | ?1.5-2.0 | China Shenyang Aircraft Inst., powder body company |
(1) design of orthogonal table table is as table 2.
Experimental factor water-glass table 2
(2) test method, test data and result
Get Cortex Phellodendri 100g (known content of berberine 1.51%) respectively, press L for every part
9(3)
4Orthogonal table is tested extraction, reclaims the ethanol drying under reduced pressure, and dried cream is weighed, and measures content of berberine, calculates its rate of transform, result of the test, and the test data variance analysis sees Table 3 and table 4.
Test data table table 3
Berberine contains the real rate of transform of berberine reason berberine
Sequence number A B C dried cream heavy (g) amount (mg/g) stoichiometric (mg) is measured (mg) (%)
1?????1???1???1????16.14????????39.57???????1510???????638.66?????42.29
2?????1???2???2????20.26(+4)????38.04???????1510???????770.69?????51.04
3?????1???3???3????21.74(+6)????35.08???????1510???????762.56?????50.50
4????2????1????2????17.76???????46.23????1510?????821.08????54.38
5????2????2????3????16.18???????50.67????1510?????819.80????54.29
6????2????3????1????18.98(+4)???36.80????1510?????698.46????46.26
7????3????1????3????18.14???????50.96????1510?????924.41????61.22
8????3????2????1????17.82???????47.36????1510?????843.97????55.89
9????3????3????2????20.18(+4)???41.40????1510?????835.45????55.33
K
1?????143.83??????157.89??????144.44?????
K
2?????154.93??????161.22??????160.75
K
3?????172.44??????152.09??????166.01?????
????47.94???????52.63???????48.15???????CT＝24669.94
????51.64???????53.74???????53.58???????Q
A＝24808.64
R???????9.54????????3.04????????7.19????????Q
C＝24754.27
Annotate: the bracket content in the table 3 under the heavy item of dried cream is to add the dextrin amount, because extract is more sticking under this alcoholic degree, dry difficulty is so added a small amount of dextrin.
Berberine rate of transform analysis of variance table table 4
| Soruces of variation | Sum of deviation square | Degree of freedom | Mean square | The F value | The P value |
| S A | ??138.70 | ???2 | ??69.35 | ????9.8 | ????＞0.05 |
| S B | ??14.23 | ???2 | ??7.12 | ????1.0 | ????＞0.05 |
| S C | ??84.33 | ???2 | ??42.17 | ????5.9 | ????＞0.05 |
| S Mistake | ??14.14 | ???2 | ??7.07 | ||
| S Always | ??251.40 |
Above table 3, table 4 interpretation of result, from the factor A of R value maximum directly perceived with A
3For best, the factor of taking second place C with C
3Be the best, what the R value was minimum is that factor B numeric ratio is approaching with B
CBigger; From the variance analysis difference of seeing there are no significant, but its F value A＞C＞B is consistent with intuitive analysis.In sum, A
3, C
3Be optimum, the B of B factor
2Slightly good, but consider that extract is more sticking in preparation process, drying is difficulty, in addition with B
1The result is more approaching, so the B factor is selected B
1For suitable.
Therefore, the preferred optimum extraction condition of analysis-by-synthesis is A
3B
1C
3
That is: with 50% ethanol extraction three times, each 8,6,6 times of amounts were extracted 2.0,1.0,1.0 hours.
(3) demonstration test
In order to verify the A of above-mentioned selection
3B
1C
3The reliability of extraction conditions is carried out demonstration test, promptly gets Cortex Phellodendri 100g, presses A
3B
1C
3Condition is tested, and extracts dried cream and weighs, and assay calculates the rate of transform, the results are shown in Table 5.
Demonstration test tables of data table 5
| Dried cream heavy (g) | Content of berberine (mg/g) | Actual measurement total amount (mg) | Theoretical amount (mg) | The rate of transform (%) |
| ??18.09 | ????51.37 | ??929.28 | ??1510 | ??61.54 |
Above result and orthogonal experiments basically identical illustrate that test data is stable, reliable, and process conditions are feasible, can enter middle trial production.
(4) test apparatus, method and condition
Instrument: Tianjin, island CS-930 thin-layer chromatogram scanner
λ
S＝345nm??λ
R＝370nm???S
X＝3
Thin layer condition: silica gel G plate
Developing solvent: the developing solvent of Cortex Phellodendri.
------the dense ammoniacal liquor of isopropyl alcohol---methanol---(12: 6: 3: 3: 1) launches under the saturated ammonia steam ethyl acetate benzene
The preparation of need testing solution: get this product powder 0.1g, accurate claim surely, put in the 50ml volumetric bottle, add ethanol 40ml, supersound process (power 250W, frequency 33KHE) 20 minutes is put coldly, adds ethanol dilution to scale, shakes up.
The preparation of reference substance solution: berberine hydrochloride 11.32mg → 50ml (02264mg/ml).
Four, this product mostly is powder and is used as medicine, and diversity is strong, the cohesiveness extreme difference, and difficult forming, granule is frangible, carries out following test.
(1) test method and experimental data
Condition of molding is carried out experimental study, the results are shown in Table 6 tables 6
| Inventory (g) | Select solvent and concentration consumption | Baking temperature | Drying time | Yield rate |
| The 100g powder | With 50% ethanol 59ml | ??80℃ | 4 hours | Granule is diffusing excessively |
| The 100g powder | With 30% ethanol 55ml | ??80℃ | 4 hours | Granule is diffusing excessively |
| The 100g powder | With 15% ethanol 55ml | ??80℃ | 4 hours | Granule is diffusing excessively |
| The 100g powder | Use aquae destillata 50ml | ??80℃ | 4 hours | Granule is diffusing excessively |
| The 100g powder | With 1% dextrin 71ml | ??80℃ | 4 hours | Yield rate 30% |
| The 100g powder | With 2% dextrin 71ml | ??80℃ | 4 hours | Yield rate 50% |
| The 100g powder | With 5% dextrin 72ml | ??80℃ | 4 hours | Yield rate 85% |
Relatively 1-2% granulates with 5% dextrin slurry, and the former yield rate is low, and shaped granule is in packing, and is frangible in the transportation, and the latter does not have this drawback, so adopt 5% dextrin to starch granulation, carries out 3 experiments with condition, and conditional stability, data are reliable.Granulate with medicinal powder among the present invention, the cohesiveness extreme difference, the granulating difficulty, granule is frangible, adopts the dextrin slurry to granulate for binding agent, through three batches of experiments, proves that dextrin slurry concentration is 5%, and addition is that the 65-70% of medicated powder amount is good, and the one-pass finished rate can reach 80-85%.
(2) pilot scale research
In front under the maturation condition, 3 batches of pilot scales, the every batch of Indigo Naturalis, Cortex Phellodendri, dried Alumen, catechu, Margarita, inventory is 12.56kg.The results are shown in Table 7.
Table 7
| Lot number | Medical material total amount (kg) | Medicated powder total amount (kg) | Dextrin slurry amount (ml/kg) | Output (kg) | Sieve leakage quantity (kg) | Yield rate (%) | Moisture (%) | Indigo content (mg/g) |
| ??981201 | ??12.56 | ??9.8 | ????650 | ????8.2 | ????1.6 | ???84 | ????4 | ????13 |
| ??981202 | ??12.56 | ??9.9 | ????680 | ????8.3 | ????1.6 | ???84 | ????4 | ????13 |
| ??981203 | ??12.56 | ??10.1 | ????700 | ????8.5 | ????1.6 | ???84 | ????4 | ????13 |
(3) the pilot scale controlled condition sees Table 8
Table 8
| Temperature (℃) | Grain thickness (cm) | Dextrin slurry consumption (ml%) | Drying time (h) |
| ??70-80℃ | ??1.5-2.5 | 65-70 | 4 |
(4) pilot scale conclusion
Through 3 batches of pilot plant tests 981201,981202,981203, prove that the concentration of dextrin slurry is 5%, addition is that the 65-70% of medicated powder amount is good, and the one-pass finished rate can reach 80-85%, and above structure shows that this technology is reasonable, can produce in batches.
Claims (6)
1, the compound indigo agent of treatment inflammatory bowel, be used for the diarrhoea that ulcerative colitis, chronic colitis, clone disease etc. cause, by the medicinal plants preparation, it is characterized in that component is as follows: Indigo Naturalis 554g dried Alumen 185g Cortex Phellodendri 308g catechu 148g Margarita powder 61g.
2, the method for the compound indigo agent of preparation treatment inflammatory bowel comprises and makes different dosage form, it is characterized in that right 1 described Indigo Naturalis, dried Alumen, catechu pulverize separately, sieves, removes impurity, fine hair, is ground into fine powder, and Indigo Naturalis contains indigo (C
16H
10N
2O
2) must not be less than 2.0%; The ultra-fine dry type of Margarita is ground into the micropowder of fineness of the particles 5-10 μ m; Cortex Phellodendri adopts ethanol extraction, and with 50% ethanol extraction three times, each 8,6,6 times of amounts were extracted 2.0,1.0,1.0 hours, recovery ethanol, and drying gets dry extract, and is ground into fine powder; With the powder of the above-mentioned five tastes component mixing that sieves, total amount is divided into 250 parts, gets 1/250 part of preparation by the pharmaceutical dosage proportioning.
3, method according to claim 2, it is characterized in that Margarita adopts ultra-fine dry type to pulverize: Compressed Gas is accelerated into supersonic airstream through jet pipe and injects pulverizing chamber, head-on collision is broken mutually after high velocity air quickens for material in the pulverizing chamber, material after the pulverizing is delivered to graded region by air-flow, sub-elect the powder of required fineness by grading wheel, the coarse powder of backlog demand returns milling zone to be continued to grind, and fine powder enters catcher with air-flow and collects, and air filters and enters atmosphere.
4, the compound indigo agent that makes according to claim 1 and 2 is characterized in that pharmaceutical dosage is oral: adult's amount: at every turn contain compound indigo agent 1/250, twice of every day; Coloclysis or suppository: each with containing 1/250 part of compound indigo agent.
5, method according to claim 2 is characterized in that preparation can be made into granule: adopt the dextrin slurry to be binding agent, dextrin slurry concentration is 5%, addition is the 65-70% of above-mentioned medicated powder amount, and system soft material, granulation are through 80 ℃ of dryings, make 1000g, the one-pass finished rate can reach 80-85%; The granulate packing, every packed 4g contains 1/250 part of compound indigo agent.
6, method according to claim 2 is characterized in that the compound indigo agent also can be made into emulsifying agent, capsule, suppository, pill, and each dosage form is as the criterion for 1/250 part to contain the compound indigo agent, and pharmaceutical technology adds excipient routinely.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021569509A CN1316996C (en) | 2002-12-26 | 2002-12-26 | Compound Qingdai agent for inflammatory intestinal diseases |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021569509A CN1316996C (en) | 2002-12-26 | 2002-12-26 | Compound Qingdai agent for inflammatory intestinal diseases |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1509733A true CN1509733A (en) | 2004-07-07 |
| CN1316996C CN1316996C (en) | 2007-05-23 |
Family
ID=34236463
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021569509A Expired - Fee Related CN1316996C (en) | 2002-12-26 | 2002-12-26 | Compound Qingdai agent for inflammatory intestinal diseases |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104248713A (en) * | 2013-06-26 | 2014-12-31 | 天士力制药集团股份有限公司 | Purpose of traditional Chinese medicinal preparation to preparation of medicament for prevention and / or treatment of Crohn's disease |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2980667A1 (en) * | 2015-04-09 | 2016-10-13 | Galderma Sa | A pharmaceutical composition and the use thereof |
| JP2018510891A (en) | 2015-04-09 | 2018-04-19 | ガルデルマ・ソシエテ・アノニム | Antibacterial indigo naturalis or indigo-producing plant extract and use thereof |
| KR20170133497A (en) | 2015-04-09 | 2017-12-05 | 갈데르마 소시에떼아노님 | An extract from indigo naturalis and a process for preparing the same |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1202361A (en) * | 1997-06-18 | 1998-12-23 | 中国医科大学附属第一医院 | Traditional Chinese medicine natural indigo powder for curing inflammatory enteropathy |
-
2002
- 2002-12-26 CN CNB021569509A patent/CN1316996C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104248713A (en) * | 2013-06-26 | 2014-12-31 | 天士力制药集团股份有限公司 | Purpose of traditional Chinese medicinal preparation to preparation of medicament for prevention and / or treatment of Crohn's disease |
| WO2014206310A1 (en) * | 2013-06-26 | 2014-12-31 | 天士力制药集团股份有限公司 | Use of chinese medicine preparation in preparing drug for preventing and/or treating crohn's disease |
| CN104248713B (en) * | 2013-06-26 | 2018-04-03 | 天士力制药集团股份有限公司 | A kind of purposes of Chinese medicine preparation in the medicine for preparing prevention and/or treatment Crohn disease |
| RU2655797C2 (en) * | 2013-06-26 | 2018-05-29 | Тасли Фармасьютикал Груп Ко., Лтд. | Use of chinese medicine preparation in preparing drug for preventing and/or treating crohn's disease |
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|---|---|
| CN1316996C (en) | 2007-05-23 |
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