CN102988545B - Preparation method and application of Yulian tablet - Google Patents
Preparation method and application of Yulian tablet Download PDFInfo
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- CN102988545B CN102988545B CN201210377488.0A CN201210377488A CN102988545B CN 102988545 B CN102988545 B CN 102988545B CN 201210377488 A CN201210377488 A CN 201210377488A CN 102988545 B CN102988545 B CN 102988545B
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- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 10
- 206010060862 Prostate cancer Diseases 0.000 claims abstract description 8
- 208000000236 Prostatic Neoplasms Diseases 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 7
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- 238000000605 extraction Methods 0.000 claims description 19
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- YBHILYKTIRIUTE-UHFFFAOYSA-N berberine Chemical compound C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 YBHILYKTIRIUTE-UHFFFAOYSA-N 0.000 abstract description 11
- 229940093265 berberine Drugs 0.000 abstract description 11
- QISXPYZVZJBNDM-UHFFFAOYSA-N berberine Natural products COc1ccc2C=C3N(Cc2c1OC)C=Cc4cc5OCOc5cc34 QISXPYZVZJBNDM-UHFFFAOYSA-N 0.000 abstract description 11
- 241000234314 Zingiber Species 0.000 abstract 1
- 235000006886 Zingiber officinale Nutrition 0.000 abstract 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 abstract 1
- 235000008397 ginger Nutrition 0.000 abstract 1
- 230000035755 proliferation Effects 0.000 abstract 1
- 230000000452 restraining effect Effects 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 21
- 238000002474 experimental method Methods 0.000 description 8
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- 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
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- 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
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- WEEMDRWIKYCTQM-UHFFFAOYSA-N 2,6-dimethoxybenzenecarbothioamide Chemical compound COC1=CC=CC(OC)=C1C(N)=S WEEMDRWIKYCTQM-UHFFFAOYSA-N 0.000 description 1
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- 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
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- JWHHANVGNNWIRI-UHFFFAOYSA-N methanol phosphoric acid hydrate Chemical compound O.OC.OP(O)(O)=O JWHHANVGNNWIRI-UHFFFAOYSA-N 0.000 description 1
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- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a preparation method of a Yulian tablet which is prepared from crude drugs including 210g of rhizoma coptidis dipped with ginger juice, 35g of fructus evodiae processed with salt and 70g of radix aucklandiae through supercritical extraction and microwave extraction, so that the content of berberine is greatly improved. The invention also provides the application of the Yulian tablet in preparing a medicine for restraining proliferation of human prostate cancer cell, PC-3 cell.
Description
Technical field
The present invention relates to the Chinese medicine preparation technical field, be specifically related to preparation method and the application in flakes of a kind of cornel.
Background technology
Cornel is recorded in Ministry of Public Health standard WS3-B-1019-91 in flakes, by Sucus Zingberis Rhizoma Coptidis 210g, salt process Fructus Evodiae 35g, Radix Aucklandiae 70g makes as crude drug, can pathogenic fire purging pain relieving, for abdominal and hypochondriac pain, belch acid regurgitation, stool diarrhea of heat type.。
In prior art, not yet there is cornel to adopt the report of supercritical and microwave technology extracting aspect preparation in flakes, and adopt 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 applied 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 cornel preparation method in flakes.
Another object of the present invention is to provide a kind of cornel to suppress the application in Human Prostate Cancer Cells PC-3 cell proliferation medicine in preparation in flakes.
Technical scheme: the objective of the invention is to realize by following scheme:
A kind of cornel preparation method in flakes, by Sucus Zingberis Rhizoma Coptidis 210g, salt process Fructus Evodiae 35g, Radix Aucklandiae 70g makes as crude drug, described method is comprised of the following step: get the Radix Aucklandiae, join in 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, obtain supercritical extract, standby; Get all the other Chinese medicines, pulverize, add 70% ethanol of 2L, drop in microwave extracting apparatus and carry out microwave extracting, extraction power 400600W, extract 2 times, each 4-8 minute, combining extraction liquid, concentrated, be added on the D101 macroporous adsorptive resins, 50% ethanol elution, collect 5 times of amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain the microwave extraction thing, standby; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol granule processed, drying, tabletting, make 1000, every heavy 0.5g.
Above-mentioned a kind of cornel preparation method in flakes, described CO
2the percent by volume that the supercritical extraction entrainer accounts for total extractant is 5%.
Above-mentioned a kind of cornel preparation method in flakes, described microwave extracting power 500W extracts 6 minutes at every turn.
Above-mentioned a kind of cornel preparation method in flakes, described CO
2the extracting pressure 20MPa of supercritical extraction, 40 ℃ of temperature, CO
2flow 2ml/g crude drug min, extraction time 160min.
Above-mentioned cornel suppresses the application in Human Prostate Cancer Cells PC-3 cell proliferation medicine in preparation in flakes.
In prior art, cornel is every 0.5g in flakes, each 5-8 sheet, and 3 times on the one, the cornel that adopts the present invention to be prepared into is every 0.5g in flakes, only needs 3 at every turn, within 1st, takes 3 times, has greatly reduced dose having under the condition of more active component.This conclusion can be by following evidence.
Cornel prepared by test one, distinct methods is the comparison of middle berberine content in flakes
1, instrument and reagent cornel of the present invention in flakes: press embodiment 3 method preparations, use the 315g crude drug, through extraction, make 1000, every heavy 0.5g.Former cornel in flakes, by the preparation of ministry standard method, is used the 315g crude drug, through extraction, makes 1000, every heavy 0.5g.Agilent 1200 high performance liquid chromatographs; The METTLERAE240 electronic analytical balance; Berberine reference substance (Nat'l Pharmaceutical & Biological Products Control Institute).
2, method
Chromatographic condition and system suitability: with octadecylsilane chemically bonded silica, be filler; Methanol-water-phosphoric acid (40:60:0.2) is mobile phase; The detection wavelength is 280nm.Number of theoretical plate is pressed the berberine peak and is calculated, and should be not less than 3000.
The preparation of reference substance solution: precision takes at 60 ℃ of drying under reduced pressure berberine reference substance of 4 hours appropriate, adds methanol and makes the solution of every 1ml containing 18 μ g, obtains.
The preparation of need testing solution: get cornel of the present invention in flakes with former cornel in flakes, porphyrize, mix, and gets 1g, accurately weighed, precision adds 70% ethanol 20ml, close plug, supersound process 10 minutes, centrifugal, get supernatant, obtain.
Algoscopy is accurate reference substance solution and each 20 μ l of need testing solution of drawing respectively, and the injection liquid chromatography, measure, and obtains.
3, result
Result shows, cornel of the present invention in flakes in the content of berberine be the 1.36mg/ sheet; And former cornel in flakes in the content of berberine be the 0.23mg/ sheet, in the situation that dose reduces, berberine content improves a lot.
Above-mentioned research shows, in flakes, the active constituent content cornel standby higher than the ministry standard legal system in flakes for the cornel that adopts the present invention to prepare.
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 to the scope of the above-mentioned theme of the present invention only limits to following example, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
Get Sucus Zingberis Rhizoma Coptidis 210g, salt is processed Fructus Evodiae 35g, Radix Aucklandiae 70g, by the Radix Aucklandiae, join in 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, obtain supercritical extract, standby; Get all the other Chinese medicines, pulverize, add 70% ethanol of 2L, drop in microwave extracting apparatus and carry out microwave extracting, extraction power 400W, extract 2 times, each 4 minutes, combining extraction liquid, concentrated, be added on the D101 macroporous adsorptive resins, 50% ethanol elution, collect 5 times of amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain the microwave extraction thing, standby; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol granule processed, drying, tabletting, make 1000, every heavy 0.5g.
After testing, in finished product, the content of berberine is the 1.43mg/ sheet.
Embodiment 2
Get Sucus Zingberis Rhizoma Coptidis 210g, salt is processed Fructus Evodiae 35g, Radix Aucklandiae 70g, by the Radix Aucklandiae, joins 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, obtain supercritical extract, standby; Get all the other Chinese medicines, pulverize, add 70% ethanol of 2L, drop in microwave extracting apparatus and carry out microwave extracting, extraction power 600W, extract 2 times, each 8 minutes, combining extraction liquid, concentrated, be added on the D101 macroporous adsorptive resins, 50% ethanol elution, collect 5 times of amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain the microwave extraction thing, standby; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol granule processed, drying, tabletting, make 1000, every heavy 0.5g.
After testing, in finished product, the content of berberine is the 1.42mg/ sheet.
Embodiment 3
Get Sucus Zingberis Rhizoma Coptidis 210g, salt is processed Fructus Evodiae 35g, Radix Aucklandiae 70g, by the Radix Aucklandiae, joins 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, obtain supercritical extract, standby; Get all the other Chinese medicines, pulverize, add 70% ethanol of 2L, drop in microwave extracting apparatus and carry out microwave extracting, extraction power 500W, extract 2 times, each 6 minutes, combining extraction liquid, concentrated, be added on the D101 macroporous adsorptive resins, 50% ethanol elution, collect 5 times of amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain the microwave extraction thing, standby; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol granule processed, drying, tabletting, make 1000, every heavy 0.5g.
After testing, in finished product, the content of berberine is the 1.36mg/ sheet.
Embodiment 4: cornel suppresses the experimentation data of PC-3 cell proliferation in flakes
1 experiment material
1.1 experiment cell strain
Human Prostate Cancer Cells PC-3 cell, Nanjing Zhengkuan Pharmaceutical Technology Co., Ltd.'s laboratory cell bank, DMEM+10%FBS cellar culture.
1.2 Experimental agents
Drugs: cornel of the present invention in flakes: press embodiment 3 methods preparations.
The medicinal liquid liquid storage: take the 100mg cornel in flakes, be dissolved in the 5ml dehydrated alcohol, 0.2 μ m filter filters, 500 μ l doff pipe packing, and-20 ℃ of storages, 0.2 μ m filter filters the use of dehydrated alcohol in order to matched group simultaneously.
1.3 experiment reagent
The Cat.No.12100-061 Lot.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); Visible-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 manufactures model to super-clean bench: SW-CJ-ZFD); Pure water instrument (U.S. Spring company model: S/N 020579); 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 (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); 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 PC-3 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, discard culture fluid, PBS fine laundering 3 times, add 3ml 0.25% trypsin-0.04%EDTA, after 37 ℃ of digestion 2min, add wherein 5ml complete medium neutralization reaction, after the piping and druming cell, it is proceeded in centrifuge tube, the centrifugal 5min of 1000rpm, adjust 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 cornel solution in flakes, continue to cultivate 24h.
4) add 20 μ l MTT solution (5mg/ml, i.e. 0.5%MTT) after 24h, continue to cultivate 4h.
5) after 4h, the buckle method is removed supernatant, with absorbent paper, pats dry gently, and every hole adds 200 μ l dimethyl sulfoxide, puts low-speed oscillation 10min on 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), set 6 multiple holes for every group.
7) with medicine, the suppression ratio to cell means result:
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 mean with mean ± S.D..
4 experimental results
Statistical result showed after the mtt assay experiment, with matched group, compare, when dosage reaches 5mg/ml, to PC-3 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 cornel is in flakes on PC-3 cell inhibitory effect impact research
Annotate: compare * P<0.01 with matched group; * P<0.001
5 experiment conclusion
Cornel can suppress the PC-3 cell proliferation in flakes, reduces the Growth of Cells number of PC-3 cell, and this effect is dose dependent.
Claims (4)
1. a cornel suppresses the application in Human Prostate Cancer Cells PC-3 cell proliferation medicine in preparation in flakes, it is characterized in that cornel preparation method in flakes is as follows, by Sucus Zingberis Rhizoma Coptidis 210g, salt process Fructus Evodiae 35g, Radix Aucklandiae 70g makes as crude drug, 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, obtain supercritical extract, standby; Get all the other Chinese medicines, pulverize, add 70% ethanol of 2L, drop in microwave extracting apparatus and carry out microwave extracting, extraction power 400-600W, extract 2 times, each 4-8 minute, combining extraction liquid, concentrated, be added on the D101 macroporous adsorptive resins, 50% ethanol elution, collect 5 times of amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain the microwave extraction thing, standby; Above-mentioned supercritical extract and microwave extraction thing are mixed, add starch, 70% ethanol granule processed, drying, tabletting, make 1000, every heavy 0.5g.
2. a kind of cornel suppresses the application in Human Prostate Cancer Cells PC-3 cell proliferation medicine in preparation in flakes according to claim 1, it is characterized in that CO described in cornel preparation method in flakes
2the percent by volume that the supercritical extraction entrainer accounts for total extractant is 5%.
3. a kind of cornel suppresses the application in Human Prostate Cancer Cells PC-3 cell proliferation medicine in preparation in flakes according to claim 1, it is characterized in that microwave extracting power 500W described in cornel preparation method in flakes, extracts 6 minutes at every turn.
4. a kind of cornel suppresses the application in Human Prostate Cancer Cells PC-3 cell proliferation medicine in preparation in flakes according to claim 1, it is characterized in that CO described in cornel preparation method in flakes
2the extracting pressure 20MPa of supercritical extraction, 40 ℃ of temperature, CO
2flow 2ml/g crude drug min, extraction time 160min.
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| CN103768261A (en) * | 2013-12-06 | 2014-05-07 | 济南新起点医药科技有限公司 | Preparation method of Qingmei cold tablet and application of Qingmei cold tablet in drugs for inhibiting myeloma cell SP2/0 from cell proliferation |
| CN103751351B (en) * | 2013-12-06 | 2016-01-20 | 马燕 | A kind of preparation method of Armeniaca mume Sieb. common cold tablet and the application in suppression leydig cell tumor of testis cell MLTC-1 cell proliferation thereof |
| CN103800499A (en) * | 2013-12-10 | 2014-05-21 | 济南新起点医药科技有限公司 | Preparation method of Qingmei cold tablet and application of Qingmei cold tablet in drugs for inhibiting melanoma cell B16 from cell proliferation |
| CN110251647A (en) * | 2019-06-28 | 2019-09-20 | 四川省一直牛健康管理有限公司 | The fever paste for treating prostate and preparation method thereof of a fragrant plant compatibility |
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| CN102058702A (en) * | 2009-11-16 | 2011-05-18 | 中国中医科学院中药研究所 | Fructus evodiae and coptis chinensis hydrogel bapu paste preparation process and substrate |
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