CN103751699B - A kind of preparation method of cholelithiasis treating Danshitongli tablet and the application in preparation inhibition breast tumor cell C127 cell proliferation medicine thereof - Google Patents
A kind of preparation method of cholelithiasis treating Danshitongli tablet and the application in preparation inhibition breast tumor cell C127 cell proliferation medicine thereof Download PDFInfo
- Publication number
- CN103751699B CN103751699B CN201310671280.4A CN201310671280A CN103751699B CN 103751699 B CN103751699 B CN 103751699B CN 201310671280 A CN201310671280 A CN 201310671280A CN 103751699 B CN103751699 B CN 103751699B
- Authority
- CN
- China
- Prior art keywords
- preparation
- cholelithiasis treating
- treating danshitongli
- application
- danshitongli tablet
- 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.)
- Expired - Fee Related
Links
Landscapes
- Medicinal Preparation (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to technical field of traditional Chinese medicines, be specifically related to a kind of preparation method and application of cholelithiasis treating Danshitongli tablet. The preparation method of cholelithiasis treating Danshitongli tablet of the present invention, made as bulk drug by desmodium 225g, oriental wormwood 225g, root tuber of aromatic turmeric 90g, dried orange peel 150g, root of large-flowered skullcap 45g, frankincense 35g, saltcake 80g, alum 35g, rheum officinale 45g, Rhizoma Sparganii 45g, cape jasmine 45g, Radix Glycyrrhizae 25g, myrrh 35g, adopt ultramicro grinding, supercritical extract, microwave abstracting and macroporous resin adsorption to be prepared from, content of hesperidin is improved a lot. The present invention also provides cholelithiasis treating Danshitongli tablet to suppress the application in mouse mammary tumor cell C127 cell proliferation medicine in preparation.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, be specifically related to a kind of preparation method of cholelithiasis treating Danshitongli tablet and suppress mouse breast in preparationApplication in adenoncus oncocyte C127 cell proliferation medicine.
Background technology
DanShiTongLi capsules standard No. WS-10324(ZD-0324)-2002, be recorded in national standard for traditional Chinese medicines compilation internal medicine liverCourage fascicle. By desmodium 225g, oriental wormwood 225g, root tuber of aromatic turmeric 90g, dried orange peel 150g, root of large-flowered skullcap 45g, frankincense 35g, saltcake80g, alum 35g, rheum officinale 45g, Rhizoma Sparganii 45g, cape jasmine 45g, Radix Glycyrrhizae 25g, myrrh 35g make as bulk drug, toolThere is clearing heat secreting bile, effect of stagnation resolvation row stone. For the acute and chronic cholecystitis due to liver and gallbladder damp-heat, gall stone etc.
In prior art, not yet there is DanShiTongLi capsules adopting ultramicro grinding, CO aspect extraction preparation2Supercritical extract, micro-The report that wave technology and macroporous adsorption resin technology extract, and Chinese medicine is directly beaten the method that powder is got, decocting boils, technique is coarse, fallAfter, impurity is many, causes patient's consumption excessive, is inconvenient to take, and has had a strong impact on this product and has applied clinically.
Summary of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of preparation method of cholelithiasis treating Danshitongli tablet.
Another object of the present invention is to provide a kind of cholelithiasis treating Danshitongli tablet to suppress mouse mammary tumor cell C127 cell in preparationApplication in propagation medicine.
The object of the invention is to realize by following scheme:
A preparation method for cholelithiasis treating Danshitongli tablet, by desmodium 225g, oriental wormwood 225g, root tuber of aromatic turmeric 90g, dried orange peel 150g, the root of large-flowered skullcap45g, frankincense 35g, saltcake 80g, alum 35g, rheum officinale 45g, Rhizoma Sparganii 45g, cape jasmine 45g, Radix Glycyrrhizae 25g, myrrh 35gMake as bulk drug, described preparation method is made up of the following step: saltcake, alum ultramicro grinding become particle size range 5-45The fine powder of μ m is for subsequent use; Get frankincense, myrrh, be ground into fine powder, join CO2In supercritical extract device, ethanol is as carrying secretlyAgent, the percent by volume that entrainer accounts for total extractant is 4-6%, extracting pressure 15-30MPa, temperature 30-50 DEG C, CO2StreamAmount l-3ml/g crude drug min, extraction time 180-220min, obtains supercritical extract, for subsequent use; Frankincense after extraction, do not haveMedicine residue and other nine tastes medicinal materials, pulverize, and adds 70% ethanol of 3.6L, and drop in microwave extracting apparatus and carry out microwave abstracting,Extraction power 600-800W, extracts 2 times, each 5-10 minute, and combining extraction liquid, concentrated, be added to DiaionHP-10 largeOn macroporous adsorbent resin post, 70% ethanol elution, collects 5 times of amount column volume eluents, and decompression recycling ethanol, concentrates and be dried,Obtain Microwave Extraction thing, the saltcake after ultramicro grinding, alum, supercritical extract, Microwave Extraction thing mixed and add starch,70% ethanol particle processed, dry, compressing tablet, makes 500, every heavy 0.3g.
In the preparation method of above-mentioned cholelithiasis treating Danshitongli tablet, described CO2In supercritical extract, entrainer accounts for the volume hundred of total extractantProportion by subtraction is 5%.
In the preparation method of above-mentioned cholelithiasis treating Danshitongli tablet, described CO2In supercritical extract, extracting pressure is 25MPa.
In the preparation method of above-mentioned cholelithiasis treating Danshitongli tablet, described CO2In supercritical extract, extraction temperature is 60 DEG C.
In the preparation method of above-mentioned cholelithiasis treating Danshitongli tablet, described CO2CO in supercritical extract2Flow 2ml/g crude drug min.
In the preparation method of above-mentioned cholelithiasis treating Danshitongli tablet, described CO2In supercritical extract, extraction time is 200min.
In the preparation method of above-mentioned cholelithiasis treating Danshitongli tablet, described microwave abstracting power is 700W.
In the preparation method of above-mentioned cholelithiasis treating Danshitongli tablet, the each extraction time of described microwave abstracting is 8 minutes.
Above-mentioned cholelithiasis treating Danshitongli tablet suppresses the application in mouse mammary tumor cell C127 cell proliferation medicine in preparation.
In prior art, DanShiTongLi capsules is oral, one time 5,3 times on the one. DanShiTongLi capsules dosage is large. AdoptEvery heavy 0.3g of cholelithiasis treating Danshitongli tablet that the inventive method is prepared into only needs 2 at every turn, within 1st, takes 3 times. Have moreUnder the condition of active component, greatly reduce dose. This conclusion can be by following evidence.
The comparison of content of hesperidin in cholelithiasis treating Danshitongli tablet prepared by test one, distinct methods
L, instrument and reagent cholelithiasis treating Danshitongli tablet of the present invention: press embodiment 1 method preparation, use 1080g bulk drug, through extractingMake 500, every heavy 0.3g. Former DanShiTongLi capsules, according to WS-10324(ZD-0324)-2002 standard method systemsStandby, in contrast. Agilent1200 high performance liquid chromatograph; AE240 electronic analytical balance; Aurantiamarin reference substance (ChinaPharmaceutical biological product calibrating institute).
2, method
Measure according to high performance liquid chromatography (annex VD of Chinese pharmacopoeia version in 2010).
Strong to close silica gel be filler by octadecylsilane for chromatographic condition and system suitability; Methanol-water (40: 60)For mobile phase; Detection wavelength is 284nm; Number of theoretical plate calculates and should be not less than 3000 by aurantiamarin peak.
It is appropriate that the preparation precision of reference substance solution takes aurantiamarin reference substance, and add methyl alcohol and make the solution of every 1ml containing 38 μ g,Obtain.
Cholelithiasis treating Danshitongli tablet of the present invention is got in the preparation of product need testing solution of the present invention, and porphyrize is got 0.06g,, accurate titleFixed, to put in tool plug conical flask, precision adds Diluted Alcohol 25ml, weighed weight, close plug, ultrasonic processing (power 250w, frequentlyRate 30kHz) 40 minutes, let cool, weighed weight, and supply the weight of less loss with Diluted Alcohol, and shake up, filter, get continuous filterLiquid, to obtain final product.
The DanShiTongLi capsules of this contrast is got in the preparation of reference substance need testing solution, mixes, and porphyrize, gets 0.15g, accurate titleFixed, to put in tool plug conical flask, precision adds Diluted Alcohol 25ml, weighed weight, close plug, ultrasonic processing (power 250w, frequentlyRate 30kHz) 40 minutes, let cool, weighed weight, and supply the weight of less loss with Diluted Alcohol, and shake up, filter, get continuous filterLiquid, to obtain final product.
Determination method is accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures,.
3, result
Result shows, in cholelithiasis treating Danshitongli tablet of the present invention, the content of aurantiamarin is 6-10mg/ sheet; And orange peel in former DanShiTongLi capsulesThe content of glycosides is 1.45mg/ grain, the 4-6 that every content of hesperidin is equivalent to original capsule content doubly, the feelings that reduce at doseUnder condition, content of hesperidin improves a lot.
Above-mentioned research shows, the cholelithiasis treating Danshitongli tablet that adopts preparation method of the present invention to prepare, and active constituent content is far away higher than WS-DanShiTongLi capsules prepared by the method that 10324(ZD-0324)-2002 standards are recorded.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described, so that those skilled in the art more understands thisBright, but this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following example, all based on foregoing of the present invention instituteThe technology realizing all belongs to scope of the present invention.
Embodiment 1
Get desmodium 225g, oriental wormwood 225g, root tuber of aromatic turmeric 90g, dried orange peel 150g, root of large-flowered skullcap 45g, frankincense 35g, saltcake 80g, whiteAlum 35g, rheum officinale 45g, Rhizoma Sparganii 45g, cape jasmine 45g, Radix Glycyrrhizae 25g, myrrh 35g: by saltcake, alum ultramicro grinding granulatingThe fine powder of degree scope 5-45 μ m is for subsequent use; Get frankincense, myrrh, be ground into fine powder, join CO2In supercritical extract device, ethanolAs entrainer, the percent by volume that entrainer accounts for total extractant is 5%, extracting pressure 25MPa, 40 DEG C of temperature, CO2StreamAmount 2ml/g crude drug min, extraction time 200min, obtains supercritical extract, for subsequent use; Frankincense after extraction, myrrh residueWith other nine tastes medicinal materials, pulverize, add 70% ethanol of 3.6L, drop in microwave extracting apparatus and carry out microwave abstracting, extraction meritRate 700W, extracts 2 times, and each 8 minutes, combining extraction liquid, concentrated, be added to DiaionHP-10 large pore resin absorption columnUpper, 70% ethanol elution, collects 5 times of amount column volume eluents, and decompression recycling ethanol, concentrates and be dried, and obtains Microwave ExtractionThing, mixes the saltcake after ultramicro grinding, alum, supercritical extract, Microwave Extraction thing to add starch, 70% ethanol systemGrain, dry, compressing tablet, makes 500, every heavy 0.3g.
After testing, in finished product, the content of aurantiamarin is 9.86mg/ sheet.
Embodiment 2
Get desmodium 225g, oriental wormwood 225g, root tuber of aromatic turmeric 90g, dried orange peel 150g, root of large-flowered skullcap 45g, frankincense 35g, saltcake 80g, whiteAlum 35g, rheum officinale 45g, Rhizoma Sparganii 45g, cape jasmine 45g, Radix Glycyrrhizae 25g, myrrh 35g: by saltcake, alum ultramicro grinding granulatingThe fine powder of degree scope 5-45 μ m is for subsequent use; Get frankincense, myrrh, be ground into fine powder, join CO2In supercritical extract device, ethanolAs entrainer, the percent by volume that entrainer accounts for total extractant is 4%, extracting pressure 30MPa, temperature 50 C, CO2StreamAmount 3ml/g crude drug min, extraction time 180min, obtains supercritical extract, for subsequent use; Frankincense after extraction, myrrh residueWith other nine tastes medicinal materials, pulverize, add 70% ethanol of 3.6L, drop in microwave extracting apparatus and carry out microwave abstracting, extraction meritRate 600W, extracts 2 times, and each 8 minutes, combining extraction liquid, concentrated, be added to DiaionHP-10 large pore resin absorption columnUpper, 70% ethanol elution, collects 5 times of amount column volume eluents, and decompression recycling ethanol, concentrates and be dried, and obtains Microwave ExtractionThing, mixes the saltcake after ultramicro grinding, alum, supercritical extract, Microwave Extraction thing to add starch, 70% ethanol systemGrain, dry, compressing tablet, makes 500, every heavy 0.3g.
After testing, in finished product, the content of aurantiamarin is 6.42mg/ sheet.
Embodiment 3
Get desmodium 225g, oriental wormwood 225g, root tuber of aromatic turmeric 90g, dried orange peel 150g, root of large-flowered skullcap 45g, frankincense 35g, saltcake 80g, whiteAlum 35g, rheum officinale 45g, Rhizoma Sparganii 45g, cape jasmine 45g, Radix Glycyrrhizae 25g, myrrh 35g: by saltcake, alum ultramicro grinding granulatingThe fine powder of degree scope 5-45 μ m is for subsequent use; Get frankincense, myrrh, be ground into fine powder, join CO2In supercritical extract device, ethanolAs entrainer, the percent by volume that entrainer accounts for total extractant is 6%, extracting pressure 15MPa, 30 DEG C of temperature, CO2StreamAmount 1ml/g crude drug min, extraction time 220min, obtains supercritical extract, for subsequent use; Frankincense after extraction, myrrh residueWith other nine tastes medicinal materials, pulverize, add 70% ethanol of 3.6L, drop in microwave extracting apparatus and carry out microwave abstracting, extraction meritRate 800W, extracts 2 times, and each 10 minutes, combining extraction liquid, concentrated, be added to DiaionHP-10 large pore resin absorption columnUpper, 70% ethanol elution, collects 5 times of amount column volume eluents, and decompression recycling ethanol, concentrates and be dried, and obtains Microwave ExtractionThing, mixes the saltcake after ultramicro grinding, alum, supercritical extract, Microwave Extraction thing to add starch, 70% ethanol systemGrain, dry, compressing tablet, makes 500, every heavy 0.3g.
After testing, in finished product, the content of aurantiamarin is 8.26mg/ sheet.
Embodiment 4: cholelithiasis treating Danshitongli tablet suppresses the experimental study data of mouse mammary tumor cell C127 cell proliferation
1. experiment material
1.1 experiment cell lines
Mouse mammary tumor cell C127 cell, Shandong University's laboratory cell bank, DMEM+10%FBS cellar culture.
1.2 Experimental agents
Drugs: cholelithiasis treating Danshitongli tablet of the present invention: press embodiment 1 method preparation.
Liquid liquid storage: take 100mg cholelithiasis treating Danshitongli tablet, be dissolved in 5ml absolute ethyl alcohol, 0.2 μ m filter filters,500 μ ldoff pipe packing ,-20 DEG C of storages, 0.2 μ m filter filters the use of absolute ethyl alcohol in order to control group simultaneously.
1.3 experiment reagent
DMEM (Cat.No.12100-061Lot.No.758137 of GIBCO company); Hyclone (Hangzhoupro, sky, Zhejiang biotechnologyThe Lot.No.100419 of Co., Ltd); NaHCO3(Shanghai hundred million Cat.No.11810-033Lot.No. of chemical reagent Co., Ltd of a specified duration1088387); Trypsin(AMRESCO company); EDTA(AMRESCO company); PenicillinGSodiumSalt(AMRESCO company 1); StreptomycinSulfate (AMRESCO); Absolute ethyl alcohol (the limited public affairs of Zibo Ya Dulan economy and tradeDepartment); MTT (Biosharp lot number: 0793): PBS(laboratory autogamy);
1.4 experiment equipment
Lycra inverted microscope (German Leica model: DMIL); Visible-ultraviolet light microwell plate detector (MD company type of the U.S.Number: SPECTRAMAX190); CO2Incubator (FORMA model: 3111); Super-clean bench (safe and sound company of Su Jing group manufacture typeNumber: SW-CJ-ZFD); Pure water instrument (Sprlng company of U.S. model: S/N020579); (French gill is gloomy for accurate pipettorCompany's model: P2); Electronic balance (German Sai Duolisi Co., Ltd model: BT323S); Full-automatic high-pressure autoclave (dayThis SANYO company model: MLS-3020); Table electrothermal air dry oven (Shanghai accurate experimental facilities company model:DHG9123A); Refrigerator (Siemens Company's model: KG18V21TI); Liquid nitrogen container (CBS model: 2001); Low speed centrifuge(Anting Scientific Instrument Factory, Shanghai's model: KA-1000); 0.2 μ m filter (MILLIPORE model: SLGP033RB); 1cm trainingSupport ware (NEST company), 96 well culture plates (NEST company); Cell counting count board; Centrifuge tube, pipette, Tips are some.
2. experimental technique
1) C127 cell uses DMEM+10%FBS in 37 DEG C, 5%CO2Carry out cellar culture (10cm culture dish), when Growth of Cells extremelyWhen logarithmic phase, collecting cell, discards nutrient solution, and PBS fine laundering 3 times, adds 3ml0.25% trypsase-0.04%EDTA,After 37 DEG C of digestion 2min, add wherein 5ml complete medium neutralization reaction, after piping and druming cell, proceeded in centrifuge tube,The centrifugal 5min of 1000rpm, adjusts concentration of cell suspension 3 × 104Individual/ml.
2) cell kind is entered in 96 well culture plates, every hole adds cell suspension 180 μ l, and culture plate is put into cell culture incubator(37℃，5%CO2) cellar culture.
3) according to Growth of Cells situation, generally grow to 50%-70%, add cholelithiasis treating Danshitongli tablet solution, continue to cultivate 24h.
4) after 24h, add 20 μ lMTT solution (5mg/ml, i.e. 0.5%MTT), continue to cultivate 4h.
5) after 4h, buckle method is removed supernatant, pats dry gently with blotting paper, and, as entered 200 μ l dimethyl sulfoxide (DMSO)s, put on shaking table in every holeLow-speed oscillation 10min, fully dissolves crystal. Measure the light absorption value in each hole at enzyme-linked immunosorbent assay instrument 490nm place.
6) background (do not add cell, only add nutrient solution) is set simultaneously, (medicine dissolving of cell, same concentrations is situated between control wellsMatter, nutrient solution, MTT, dimethyl sulfoxide (DMSO)), set 6 multiple holes for every group.
7) result represents the inhibiting rate of cell with medicine: cell increment inhibiting rate (%)=(control wells OD value-dosing holes ODValue), control wells OD value × 100%. Experiment repeats 3 times.
3. statistical disposition
Adopt correlation analysis and Studentt inspection in MicrosoftExcel2007 software, data are with mean ± S.D.Represent.
4. experimental result
Statistical result showed after mtt assay experiment, with control group comparison, in the time that dosage reaches 5mg/ml, to C127 cell proliferationSuppress variant (P < 0.05), dosage this difference in the time of 10mg/ml has conspicuousness (P < 0.01), when dosage reaches 15-When 20mg/ml, there is utmost point significant difference (P < 0.001).
Table 1 cholelithiasis treating Danshitongli tablet is on C127 cell inhibitory effect impact research (X ± SD)
| Group | Drug concentration (mg/ml) | Inhibiting rate (%) |
| Control group | 0 | 0 |
| 1 | 5 | 8.84±6.98 |
| 2 | 10 | 15.26±7.68* |
| 3 | 15 | 27.43±11.52** |
| 4 | 20 | 38.20±12.95** |
Note: with control group comparison, * P < O.01; * P < 0.001.
5. experiment conclusion
Cholelithiasis treating Danshitongli tablet can suppress C127 cell proliferation, reduces the Growth of Cells number of C127 cell, and this effect is dosageDependence.
Claims (7)
1. a cholelithiasis treating Danshitongli tablet suppresses the application in mouse mammary tumor cell C127 cell proliferation medicine in preparation, it is characterized in that, described cholelithiasis treating Danshitongli tablet is made up as bulk drug of desmodium 225g, oriental wormwood 225g, root tuber of aromatic turmeric 90g, dried orange peel 150g, root of large-flowered skullcap 45g, frankincense 35g, saltcake 80g, alum 35g, rheum officinale 45g, Rhizoma Sparganii 45g, cape jasmine 45g, Radix Glycyrrhizae 25g, myrrh 35g, and concrete step prepared by described cholelithiasis treating Danshitongli tablet is: become the fine powder of particle size range 5-45 μ m for subsequent use saltcake, alum ultramicro grinding; Get frankincense, myrrh, be ground into fine powder, join in CO2 supercritical extract device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 4-6%, extracting pressure 15-30MPa, temperature 30-50 DEG C, CO2 flow 1-3ml/g crude drug min, extraction time 180-220min, obtain supercritical extract, for subsequent use;
Frankincense after extraction, myrrh residue and other nine tastes medicinal materials, pulverize, add 70% ethanol of 3.6L, drop in microwave extracting apparatus and carry out microwave abstracting, extraction power 600-800W, extract 2 times, each 5-10 minute, combining extraction liquid, concentrated, be added on DiaionHP-10 large pore resin absorption column, 70% ethanol elution, collect 5 times of amount column volume eluents, decompression recycling ethanol, concentrate and be dried, obtain Microwave Extraction thing, by the saltcake after ultramicro grinding, alum, supercritical extract, Microwave Extraction thing mixes and adds starch, 70% ethanol particle processed, dry, compressing tablet, make 500, every heavy 0.3g.
2. the cholelithiasis treating Danshitongli tablet as described in claim l suppresses the application in mouse mammary tumor cell C127 cell proliferation medicine in preparation, it is characterized in that, in described CO2 supercritical extract, to account for the percent by volume of total extractant be 5% to entrainer.
3. the cholelithiasis treating Danshitongli tablet as described in claim l suppresses the application in mouse mammary tumor cell C127 cell proliferation medicine in preparation, it is characterized in that, in described CO2 supercritical extract, extracting pressure is 25MPa.
4. the cholelithiasis treating Danshitongli tablet as described in claim l suppresses the application in mouse mammary tumor cell C127 cell proliferation medicine in preparation, it is characterized in that CO2 flow 2ml/g crude drug min in described CO2 supercritical extract.
5. the cholelithiasis treating Danshitongli tablet as described in claim l suppresses the application in mouse mammary tumor cell C127 cell proliferation medicine in preparation, it is characterized in that, in described CO2 supercritical extract, extraction time is 200min.
6. the cholelithiasis treating Danshitongli tablet as described in claim l suppresses the application in mouse mammary tumor cell C127 cell proliferation medicine in preparation, it is characterized in that, described microwave abstracting power is 700W.
7. the cholelithiasis treating Danshitongli tablet as described in claim l suppresses the application in mouse mammary tumor cell C127 cell proliferation medicine in preparation, it is characterized in that, the each extraction time of described microwave abstracting is 8 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310671280.4A CN103751699B (en) | 2013-12-10 | 2013-12-10 | A kind of preparation method of cholelithiasis treating Danshitongli tablet and the application in preparation inhibition breast tumor cell C127 cell proliferation medicine thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310671280.4A CN103751699B (en) | 2013-12-10 | 2013-12-10 | A kind of preparation method of cholelithiasis treating Danshitongli tablet and the application in preparation inhibition breast tumor cell C127 cell proliferation medicine thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103751699A CN103751699A (en) | 2014-04-30 |
| CN103751699B true CN103751699B (en) | 2016-05-25 |
Family
ID=50519126
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310671280.4A Expired - Fee Related CN103751699B (en) | 2013-12-10 | 2013-12-10 | A kind of preparation method of cholelithiasis treating Danshitongli tablet and the application in preparation inhibition breast tumor cell C127 cell proliferation medicine thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103751699B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102988723A (en) * | 2012-10-08 | 2013-03-27 | 李正梅 | Preparation method and application of yin tonifying and calming tablet |
-
2013
- 2013-12-10 CN CN201310671280.4A patent/CN103751699B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102988723A (en) * | 2012-10-08 | 2013-03-27 | 李正梅 | Preparation method and application of yin tonifying and calming tablet |
Non-Patent Citations (1)
| Title |
|---|
| 胆石通利胶囊;国家药品监督管理局;《国家药品标准（试行）颁布件》;20021116;第2页"处方"和"制法" * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103751699A (en) | 2014-04-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103656493B (en) | A kind of preparation method of blood stasis dispelling stomach reinforcing sheet and application | |
| CN102988545A (en) | Preparation method and application of Yulian tablet | |
| CN103751699B (en) | A kind of preparation method of cholelithiasis treating Danshitongli tablet and the application in preparation inhibition breast tumor cell C127 cell proliferation medicine thereof | |
| CN102988611B (en) | Preparation method and application of antihypertension tablet | |
| CN103800816A (en) | Preparation method of Danshitongli tablet and application of Danshitongli tablet in preparing drugs for inhibiting stomach cancer cell MFC from cell proliferation | |
| CN103800818A (en) | Preparation method of Danshitongli tablet and application of Danshitongli tablet in preparing drugs for inhibiting myeloma cell FO from cell proliferation | |
| CN103768513B (en) | A kind of preparation method of cholelithiasis treating Danshitongli tablet and the application in preparation inhibition teratocarcinoma cell P19 cell proliferation medicine thereof | |
| CN103784872B (en) | A kind of preparation method of cholelithiasis treating Danshitongli tablet and the application in preparation suppression Ascitic Tumor Cells SAC-II C3 cell proliferation thereof | |
| CN103751698B (en) | The preparation method of a kind of cholelithiasis treating Danshitongli tablet and the application in preparation suppression prostate gland cancer cell RM-1 cell proliferation thereof | |
| CN103800498A (en) | Preparation method of Qingmei cold tablet and application of Qingmei cold tablet in drugs for inhibiting mouse prostate cancer cell RM-1 from cell proliferation | |
| CN103768267A (en) | Preparation method of Qingmei cold tablet and application of Qingmei cold tablet in drugs for inhibiting lung cancer cell H22 from cell proliferation | |
| CN103768211A (en) | Preparation method of Qingmei cold tablet and application of Qingmei cold tablet in drugs for inhibiting lymphomata cell EL4 from cell proliferation | |
| CN103768266A (en) | Preparation method of Qingmei cold tablet and application of Qingmei cold tablet in drugs for inhibiting mouse leukaemia cell L6565 from cell proliferation | |
| CN103768517A (en) | Preparation method of Danshitongli tablet and application of Danshitongli tablet in preparing drugs for inhibiting mouse lung cancer cell LLC from cell proliferation | |
| CN103768514A (en) | Preparation method of Danshitongli tablet and application of Danshitongli tablet in preparing drugs for inhibiting myeloma cell SP2/0 from cell proliferation | |
| CN103751701B (en) | A kind of preparation method of cholelithiasis treating Danshitongli tablet and the application in preparation suppression lymphoma cell YAC-1 cell proliferation thereof | |
| CN103751700A (en) | Danshilitong tablet preparation method and application of Danshilitong tablets in preparation of lymphoid neoplasm cell P388D1 proliferation inhibition drugs | |
| CN103768516A (en) | Preparation method of Danshitongli tablet and application of Danshitongli tablet in preparing drugs for inhibiting stomach cancer cell MFC from cell proliferation | |
| CN103768208B (en) | A kind of preparation method of green plum common cold tablet and the application in inhibition lymph sample oncocyte P388D1 cell proliferation medicine thereof | |
| CN104161852A (en) | Preparation method for nine-composition hemorrhoid tablet and application thereof to medicines inhibiting cell proliferation of prostate cancer cell RM-1 | |
| CN103768207A (en) | Preparation method of Qingmei cold tablet and application of Qingmei cold tablet in drugs for inhibiting lung cancer cell Hepa1-6 from cell proliferation | |
| CN103768265A (en) | Preparation method of Qingmei cold tablet and application of Qingmei cold tablet in drugs for inhibiting lung cancer cell LLC from cell proliferation | |
| CN103768212A (en) | Preparation method of Qingmei cold tablet and application of Qingmei cold tablet in drugs for inhibiting stomach cancer cell MFC from cell proliferation | |
| CN103768264A (en) | Preparation method of Qingmei cold tablet and application of Qingmei cold tablet in drugs for inhibiting teratoma cell P19 from cell proliferation | |
| CN103751425A (en) | Preparation method of Qingmei cold-treatment tablet and use of Qingmei cold-treatment tablet in drug for inhibiting breast tumor cell C127 proliferation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| CB03 | Change of inventor or designer information |
Inventor after: Hou Hong Inventor after: Yu Xi Inventor after: Fang Kun Inventor after: Li Zhenfeng Inventor before: Sun Bo |
|
| COR | Change of bibliographic data | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20160413 Address after: Qingdao City, Shandong province 266000 four Road No. 127 Applicant after: Zhongxin Hospital, Qingdao Address before: 250001 Shandong Province, Ji'nan City District Court building 2303 No. 288 Applicant before: JINAN XINQIDIAN MEDICINE SCIENCE & TECHNOLOGY CO., LTD. |
|
| 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: 20160525 Termination date: 20171210 |