CN102988501A - Preparation method and application of Libiling tablet - Google Patents
Preparation method and application of Libiling tablet Download PDFInfo
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- CN102988501A CN102988501A CN2012103775328A CN201210377532A CN102988501A CN 102988501 A CN102988501 A CN 102988501A CN 2012103775328 A CN2012103775328 A CN 2012103775328A CN 201210377532 A CN201210377532 A CN 201210377532A CN 102988501 A CN102988501 A CN 102988501A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000003814 drug Substances 0.000 claims abstract description 21
- 229940079593 drug Drugs 0.000 claims abstract description 14
- 238000000874 microwave-assisted extraction Methods 0.000 claims abstract description 11
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 10
- VYQNWZOUAUKGHI-UHFFFAOYSA-N monobenzone Chemical compound C1=CC(O)=CC=C1OCC1=CC=CC=C1 VYQNWZOUAUKGHI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 201000001441 melanoma Diseases 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 55
- 238000000605 extraction Methods 0.000 claims description 19
- 239000000284 extract Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 6
- 229920002472 Starch Polymers 0.000 claims description 5
- 230000000274 adsorptive effect Effects 0.000 claims description 5
- 230000004663 cell proliferation Effects 0.000 claims description 5
- 229940126678 chinese medicines Drugs 0.000 claims description 5
- 230000006837 decompression Effects 0.000 claims description 5
- 239000003480 eluent Substances 0.000 claims description 5
- 238000010828 elution Methods 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 239000008107 starch Substances 0.000 claims description 5
- 235000019698 starch Nutrition 0.000 claims description 5
- 230000005764 inhibitory process Effects 0.000 claims description 3
- 230000035755 proliferation Effects 0.000 abstract 1
- 230000000452 restraining effect Effects 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 21
- ZSBXGIUJOOQZMP-UHFFFAOYSA-N Isomatrine Natural products C1CCC2CN3C(=O)CCCC3C3C2N1CCC3 ZSBXGIUJOOQZMP-UHFFFAOYSA-N 0.000 description 10
- ZSBXGIUJOOQZMP-JLNYLFASSA-N Matrine Chemical compound C1CC[C@H]2CN3C(=O)CCC[C@@H]3[C@@H]3[C@H]2N1CCC3 ZSBXGIUJOOQZMP-JLNYLFASSA-N 0.000 description 10
- 229930014456 matrine Natural products 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 239000013558 reference substance Substances 0.000 description 4
- 239000006144 Dulbecco’s modified Eagle's medium Substances 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000010261 cell growth Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000012531 culture fluid Substances 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 239000006285 cell suspension Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- WEEMDRWIKYCTQM-UHFFFAOYSA-N 2,6-dimethoxybenzenecarbothioamide Chemical compound COC1=CC=CC(OC)=C1C(N)=S WEEMDRWIKYCTQM-UHFFFAOYSA-N 0.000 description 1
- 206010000087 Abdominal pain upper Diseases 0.000 description 1
- 238000002965 ELISA Methods 0.000 description 1
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- 108090000631 Trypsin Proteins 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000010165 autogamy Effects 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- FCPVYOBCFFNJFS-LQDWTQKMSA-M benzylpenicillin sodium Chemical compound [Na+].N([C@H]1[C@H]2SC([C@@H](N2C1=O)C([O-])=O)(C)C)C(=O)CC1=CC=CC=C1 FCPVYOBCFFNJFS-LQDWTQKMSA-M 0.000 description 1
- 238000004113 cell culture Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010219 correlation analysis Methods 0.000 description 1
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- 230000035619 diuresis Effects 0.000 description 1
- 231100000673 dose–response relationship Toxicity 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
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- 238000002347 injection Methods 0.000 description 1
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- 230000031700 light absorption Effects 0.000 description 1
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- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- JWHHANVGNNWIRI-UHFFFAOYSA-N methanol phosphoric acid hydrate Chemical compound O.OC.OP(O)(O)=O JWHHANVGNNWIRI-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 1
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- 230000001737 promoting effect Effects 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
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- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000004759 spandex Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 229960002385 streptomycin sulfate Drugs 0.000 description 1
- 239000012588 trypsin Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention provides a preparation method of a libiling tablet which is prepared from crude drugs including 500g of radix sophorae flavescentis, 250g of radix paeoniae alba and 150g of radix aucklandiae through supercritical extraction and microwave extraction, so that the content of sophocarpidine is greatly improved. The invention also provides the application of the libiling tablet in preparing a medicine for restraining proliferation of human melanoma cell, MV3 cell.
Description
Technical field
The present invention relates to the Chinese medicine preparation technical field, be specifically related to a kind of preparation method and application of Libiling tablets.
Background technology
Libiling tablets is recorded in Ministry of Public Health standard WS3-B-0639-91, is made as crude drug by Radix Sophorae Flavescentis 500g, Radix Paeoniae Alba 250g, Radix Aucklandiae 150g, can clearing away heat-damp and promoting diuresis.Be used for hygropyretic dysentery, purge heat the diseases such as stomachache.
In the prior art, not yet there is Libiling tablets to adopt the report of supercritical and microwave technology aspect the preparation extracting, and adopts the method that powder and decocting boil of beating, technique is coarse, backward, and impurity is many, causes patient's consumption excessive, be inconvenient to take, had a strong impact on this product and used clinically.
Summary of the invention
Goal of the invention: in order to address the above problem, the object of the present invention is to provide a kind of preparation method of Libiling tablets.
Another object of the present invention is to provide the application of a kind of Libiling tablets in preparation inhibition human melanoma cell MV3 cell proliferation medicine.
Technical scheme: the objective of the invention is to realize by following scheme:
A kind of preparation method of Libiling tablets, made as crude drug by Radix Sophorae Flavescentis 500g, Radix Paeoniae Alba 250g, Radix Aucklandiae 150g, described method is comprised of the following step: get the Radix Aucklandiae, join in the CO2 supercritical extraction device, ethanol is as entrainer, the percent by volume that entrainer accounts for total extractant is 4-6%, extracting pressure 15-30MPa, temperature 30-50 ℃, CO2 flow 1-3m1/g crude drug min, extraction time 150-180min gets supercritical extract, and is for subsequent use; Get all the other Chinese medicines, pulverize, add 70% ethanol of 2L, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 400600W extracts 2 times, each 4-8 minute, combining extraction liquid, concentrated, be added on the D101 macroporous adsorptive resins, 50% ethanol elution is collected 5 times of amount column volume eluents, decompression recycling ethanol, concentrated and dry, get the microwave extraction thing, for subsequent use; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol granule processed, drying, tabletting is made 1600, every heavy 0.5g.
The preparation method of above-mentioned a kind of Libiling tablets, described CO
2The percent by volume that the supercritical extraction entrainer accounts for total extractant is 5%.
The preparation method of above-mentioned a kind of Libiling tablets, described microwave extracting power 500W extracts 6 minutes at every turn.
The preparation method of above-mentioned a kind of Libiling tablets, described CO
2The extracting pressure 20MPa of supercritical extraction, 40 ℃ of temperature, CO
2Flow 2ml/g crude drug min, extraction time 160min.
The application of above-mentioned Libiling tablets in preparation inhibition human melanoma cell MV3 cell proliferation medicine.
In the prior art, every 0.5g of Libiling tablets, each 8,3 times on the one, the every 0.5g of Libiling tablets that adopts the present invention to be prepared into only needs 4 at every turn, takes 2 times in 1st, has greatly reduced dose having under the condition of more active component.This conclusion can be by following evidence.
The comparison of matrine content in the Libiling tablets of test one, distinct methods preparation
1, instrument and reagent Libiling tablets of the present invention: press the preparation of embodiment 3 methods, use the 800g crude drug, make 1600 through extraction, every heavy 0.5g.Former Libiling tablets by the preparation of ministry standard method, uses the 800g crude drug, makes 1600 through extraction, every heavy 0.5g.Agilent 1200 high performance liquid chromatographs; The METTLERAE240 electronic analytical balance; Matrine reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute).
2, method
Chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica; Methanol-water-phosphoric acid (40:60:0.2) is mobile phase; The detection wavelength is 280nm.Number of theoretical plate is pressed the matrine peak and is calculated, and should be not less than 3000.
The preparation of reference substance solution: precision takes by weighing at 4 hours matrine reference substance of 60 ℃ of drying under reduced pressure an amount of, adds methanol and makes the solution that every 1ml contains 18 μ g, and get final product.
The preparation of need testing solution: get Libiling tablets of the present invention and former Libiling tablets, porphyrize, mixing is got 1g, and is accurately weighed, the accurate 70% ethanol 20ml that adds, close plug, supersound process 10 minutes, centrifugal, get supernatant, and get final product.
Algoscopy is accurate reference substance solution and each 20 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product.
3, result
The result shows, the content of matrine is the 1.47mg/ sheet in the Libiling tablets of the present invention; And the content of matrine is the 0.35mg/ sheet in the former Libiling tablets, in the situation that dose reduces, matrine content improves a lot.
Above-mentioned studies show that, the Libiling tablets that adopts the present invention to prepare, active constituent content is higher than the standby Libiling tablets of ministry standard legal system.
The specific embodiment
Form by the following examples, foregoing of the present invention is described in further detail again, but this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following example, all technology that realizes based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
Get Radix Sophorae Flavescentis 500g, Radix Paeoniae Alba 250g, Radix Aucklandiae 150g, with the Radix Aucklandiae, join in the CO2 supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 4%, extracting pressure 15MPa, 30 ℃ of temperature, CO2 flow 1m1/g crude drug min, extraction time 150min, get supercritical extract, for subsequent use; Get all the other Chinese medicines, pulverize, add 70% ethanol of 2L, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 400W extracts 2 times, each 4 minutes, combining extraction liquid, concentrated, be added on the D101 macroporous adsorptive resins, 50% ethanol elution is collected 5 times of amount column volume eluents, decompression recycling ethanol, concentrated and dry, get the microwave extraction thing, for subsequent use; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol granule processed, drying, tabletting is made 1600, every heavy 0.5g.
After testing, the content of matrine is the 1.51mg/ sheet in the finished product.
Embodiment 2
Get Radix Sophorae Flavescentis 500g, Radix Paeoniae Alba 250g, Radix Aucklandiae 150g, with the Radix Aucklandiae, join CO
2In the supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 6%, extracting pressure 30MPa, temperature 50 C, CO
2Flow 3m1/g crude drug min, extraction time 180min gets supercritical extract, and is for subsequent use; Get all the other Chinese medicines, pulverize, add 70% ethanol of 2L, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 600W extracts 2 times, each 8 minutes, combining extraction liquid, concentrated, be added on the D101 macroporous adsorptive resins, 50% ethanol elution is collected 5 times of amount column volume eluents, decompression recycling ethanol, concentrated and dry, get the microwave extraction thing, for subsequent use; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol granule processed, drying, tabletting is made 1600, every heavy 0.5g.
After testing, the content of matrine is the 1.54mg/ sheet in the finished product.
Embodiment 3
Get Radix Sophorae Flavescentis 500g, Radix Paeoniae Alba 250g, Radix Aucklandiae 150g, with the Radix Aucklandiae, join CO
2In the supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 5%, extracting pressure 20MPa, 40 ℃ of temperature, CO
2Flow 2m1/g crude drug min, extraction time 160min gets supercritical extract, and is for subsequent use; Get all the other Chinese medicines, pulverize, add 70% ethanol of 2L, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 500W extracts 2 times, each 6 minutes, combining extraction liquid, concentrated, be added on the D101 macroporous adsorptive resins, 50% ethanol elution is collected 5 times of amount column volume eluents, decompression recycling ethanol, concentrated and dry, get the microwave extraction thing, for subsequent use; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol granule processed, drying, tabletting is made 1600, every heavy 0.5g.
After testing, the content of matrine is the 1.47mg/ sheet in the finished product.
Embodiment 4: Libiling tablets suppresses the experimentation data of MV3 cell proliferation
1 experiment material
1.1 experiment cell strain
Human melanoma cell MV3 cell, Nanjing Zhengkuan Pharmaceutical Technology Co., Ltd.'s laboratory cell bank, DMEM+10%FBS cellar culture.
1.2 Experimental agents
Drugs: Libiling tablets of the present invention: press the preparation of embodiment 3 methods.
The medicinal liquid liquid storage: take by weighing the 100mg Libiling tablets, be dissolved in the 5ml dehydrated alcohol, 0.2 μ m filter filters, and 500 μ ldoff manage packing ,-20 ℃ of storages, and 0.2 μ m filter filters dehydrated alcohol in order to the usefulness of matched group simultaneously.
1.3 experiment reagent
The Cat.No.12100-061Lot.No.758137 of DMEM(GIBCO company); Hyclone (Hangzhoupro, sky, Zhejiang bio tech ltd Lot.No.100419); NaHCO3(Shanghai hundred million chemical reagent company limited Cat.No.11810-033Lot.No.1088387 of a specified duration); Trypsin(AMRESCO company lot number: 2010/04); EDTA(AMRESCO company lot number: 2009/10); Penicillin G Sodium Salt(AMRESCO company lot number: 2010242); Streptomycin Sulfate(AMRESCO company lot number: 2010382); Dehydrated alcohol (Nanjing Chemistry Reagent Co., Ltd.'s lot number: 080310182); MTT (Biosharp lot number: 0793); The autogamy of PBS(laboratory);
1.4 experiment equipment
Lycra inverted microscope (German Leica model: DM1L); As seen-ultraviolet light microwell plate detector (U.S. MD company model: SPECTRAMAX 190); CO2 incubator (FORMA model: 3111); (safe and sound company of Su Jing group makes model to super-clean bench: SW-CJ-ZFD); Pure water instrument (U.S. Spring company model: S/N020579); Accurate pipettor (French Gilson Inc model: P2); Electronic balance (German Sai Duolisi company limited model: BT323S); Full-automatic high-pressure autoclave (Japanese SANYO company model: MLS-3020); Table electrothermal air dry oven (the accurate experimental facilities in Shanghai 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); 10cm culture dish (NEST company), 96 well culture plates (NEST company); Cell counting count board; Centrifuge tube, pipet, Tips are some.
2 experimental techniques
1) the MV3 cell carries out cellar culture (10cm culture dish) with DMEM+10%FBS in 37 ℃, 5%CO2, when Growth of Cells during to logarithmic (log) phase, collecting cell discards culture fluid, PBS fine laundering 3 times, add 3ml 0.25% trypsin-0.04%EDTA, behind 37 ℃ of digestion 2min, to wherein adding 5ml complete medium neutralization reaction, behind the piping and druming cell it is changed in the centrifuge tube, the centrifugal 5min of 1000rpm adjusts 3 * 104/ml of concentration of cell suspension.
2) the cell kind is entered in 96 well culture plates, every hole adds cell suspension 180 μ l, culture plate put into cell culture incubator (37 ℃, 5%CO2) cellar culture.
3) according to the Growth of Cells situation, generally grow to 50%-70%, add Libiling tablets solution, continue to cultivate 24h.
4) add 20 μ l MTT solution (5mg/ml, i.e. 0.5%MTT) behind the 24h, continue to cultivate 4h.
5) the buckle method is removed supernatant behind the 4h, pats dry gently with absorbent paper, and every hole adds 200 μ l dimethyl sulfoxide, puts low-speed oscillation 10min on the shaking table, and crystal is fully dissolved.Measure the light absorption value in each hole at enzyme-linked immunosorbent assay instrument 490nm place.
6) background (do not add cell, only add culture fluid) is set simultaneously, control wells (the medicine dissolution medium of cell, same concentrations, culture fluid, MTT, dimethyl sulfoxide) is set 6 multiple holes for every group.
7) result represents with the suppression ratio of medicine to cell:
Cell increment suppression ratio (%)=(control wells OD value-dosing holes OD value)/control wells OD value * 100%.Experiment repeats 3 times.
3 statistical dispositions
Adopt correlation analysis and Student t check in Microsoft Excel 2003 softwares, data represent with mean ± S.D..
4 experimental results
Statistical result showed after the mtt assay experiment, compare with matched group, when dosage reaches 5mg/ml, to MV3 cell inhibitory effect variant (P＜0.05), dosage this difference when 10mg/ml has significance (P＜0.01), and utmost point significant difference (P＜0.001) is arranged when dosage reaches 15-20mg/ml.
Table 1 Libiling tablets is on MV3 cell inhibitory effect impact research
Annotate: compare * P＜0.01 with matched group; * P＜0.001
5 experiment conclusion
Libiling tablets can suppress the MV3 cell proliferation, reduces the Growth of Cells number of MV3 cell, and this effect is dose dependent.
Claims (5)
1. the preparation method of a Libiling tablets is made as crude drug by Radix Sophorae Flavescentis 500g, Radix Paeoniae Alba 250g, Radix Aucklandiae 150g, it is characterized in that described method is comprised of the following step: get the Radix Aucklandiae, join CO
2In the supercritical extraction 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 ℃, CO
2Flow 1-3m1/g crude drug min, extraction time 150-180min gets supercritical extract, and is for subsequent use; Get all the other Chinese medicines, pulverize, add 70% ethanol of 2L, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 400-600W extracts 2 times, each 4-8 minute, combining extraction liquid, concentrated, be added on the D101 macroporous adsorptive resins, 50% ethanol elution is collected 5 times of amount column volume eluents, decompression recycling ethanol, concentrated and dry, get the microwave extraction thing, for subsequent use; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol granule processed, drying, tabletting is made 1600, every heavy 0.5g.
2. the preparation method of described a kind of Libiling tablets according to claim 1 is characterized in that described CO
2The percent by volume that the supercritical extraction entrainer accounts for total extractant is 5%.
3. the preparation method of described a kind of Libiling tablets according to claim 1 is characterized in that described microwave extracting power 500W, extracts 6 minutes at every turn.
4. the preparation method of described a kind of Libiling tablets according to claim 1 is characterized in that described CO
2The extracting pressure 20MPa of supercritical extraction, 40 ℃ of temperature, CO
2Flow 2ml/g crude drug min, extraction time 160min.
5. the according to claim 1 application of described a kind of Libiling tablets in preparation inhibition human melanoma cell MV3 cell proliferation medicine.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210377532.8A CN102988501B (en) | 2012-10-08 | 2012-10-08 | Preparation method and application of Libiling tablet |
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| CN201210377532.8A CN102988501B (en) | 2012-10-08 | 2012-10-08 | Preparation method and application of Libiling tablet |
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| CN102988501B CN102988501B (en) | 2014-01-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105596456A (en) * | 2016-03-01 | 2016-05-25 | 南京正亮医药科技有限公司 | Preparation method and application of spur pills |
| CN107243025A (en) * | 2017-06-26 | 2017-10-13 | 吉林大学 | A kind of plant drug composition for treating canine parvovirus disease |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102397451A (en) * | 2011-11-26 | 2012-04-04 | 苏州派腾生物医药科技有限公司 | Preparation method of cholagogic tablet |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102397451A (en) * | 2011-11-26 | 2012-04-04 | 苏州派腾生物医药科技有限公司 | Preparation method of cholagogic tablet |
Non-Patent Citations (1)
| Title |
|---|
| 中华人民共和国卫生部药典委员会: "《卫生部药品标准 中药成方制剂分册（第三册）》", 31 December 1991 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105596456A (en) * | 2016-03-01 | 2016-05-25 | 南京正亮医药科技有限公司 | Preparation method and application of spur pills |
| CN107243025A (en) * | 2017-06-26 | 2017-10-13 | 吉林大学 | A kind of plant drug composition for treating canine parvovirus disease |
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| CN102988501B (en) | 2014-01-01 |
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