CN104383427A - Preparation method and application of gallstone-dissolving cholagogue tablets - Google Patents

Preparation method and application of gallstone-dissolving cholagogue tablets Download PDF

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Publication number
CN104383427A
CN104383427A CN201410562859.1A CN201410562859A CN104383427A CN 104383427 A CN104383427 A CN 104383427A CN 201410562859 A CN201410562859 A CN 201410562859A CN 104383427 A CN104383427 A CN 104383427A
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preparation
extraction
radix
sal nitri
cholagogic tablet
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尤晓明
王显涛
李洋
迟文泉
邓世海
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Shandong Yongtai Chemical Group Co Ltd
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Shandong Yongtai Chemical Group Co Ltd
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Abstract

The invention belongs to the technical field of traditional Chinese medicines and particularly relates to a preparation method and application of gallstone-dissolving cholagogue tablets. The gallstone-dissolving cholagogue tablets are prepared from the drug substances by adopting supercritical extraction and microwave-assisted extraction, so that the content of hesperidin is greatly increased. The drug substances comprise 165 g of vinegar-processed radix bupleuri, 165 g of pericarpium citri reticulatae viride, 165 g of scutellaria baicalensis, 165 g of radices paeoniae alba, 66 g of rheum officinale, 165 g of radix curcumae, 165 g of desmodium, 165 g of lygodium japonicum, 165 g of heated endothelium corneum gigeriae galli, 165 g of oriental wormwood, 165 g of turmeric, 110 g of vinegar-processed trigone and 165 g of radix clematidis. The invention further provides the application of the gallstone-dissolving cholagogue tablets in preparing medicine for inhibiting cell proliferation of mouse anus sarcoma cell S-180.

Description

A kind of preparation method of Sal Nitri cholagogic tablet and application
Technical field
The invention belongs to technical field of Chinese medicines, be specifically related to a kind of preparation method of Sal Nitri cholagogic tablet and suppressing the application in mice anus sarcoma cell S-180 cell proliferation.
Background technology
Sal Nitri Lidan Capsule standard No. WS-11331 (ZD-1331)-2002, is recorded in national standard for traditional Chinese medicines compilation internal medicine taste fascicle.Be made up as crude drug of Radix Astragali 280g, fiber crops rare 80g, Radix Angelicae Sinensis 190g, Herba Ecliptae 220g, Rhizoma Atractylodis 190g, Flos Carthami 150g, Radix Paeoniae Rubra 140g, Semen Persicae 140g, Radix Achyranthis Bidentatae 150g, Rhizoma Chuanxiong 120g, Fructus Aurantii 70g, Radix Platycodonis 100g, there is depressed liver-energy dispersing and function of gallbladder promoting, promoting the circulation of QI to relieve pain, heat-clearing and toxic substances removing calculus removing effect, for syndrome after chronic cholecystitis, cholelithiasis, cholangitis, operation on gallbladder and biliary tract function of patients disease.
In prior art, Sal Nitri Lidan Capsule is not yet had to extract the report adopting supercritical and microwave technology in preparation, and volatile oil is drawn, the method of soak by water, technique is coarse, backward, and impurity is many, cause patient's consumption excessive, be inconvenient to take, had a strong impact on this product and applied clinically.
In prior art, each 3 of Sal Nitri Lidan Capsule, 3 times on the one.Sal Nitri Lidan Capsule dosage is large, and the heavy 0.5g of the every sheet of the Sal Nitri cholagogic tablet adopting the inventive method to be prepared into, only needs 1 at every turn, within 1st, take 3 times.Dose is greatly reduced under the condition with more active component.This conclusion can be proved by following test.And being prepared into tablet, patient swallows with water, and dosage is little and without bitterness, patient is easy to accept.
The comparison of content of hesperidin in Sal Nitri cholagogic tablet prepared by test one, distinct methods
L, instrument and reagent Sal Nitri cholagogic tablet of the present invention: by the preparation of embodiment 1 method, use 1991g crude drug, makes 333 through extracting, the heavy 0.5g of every sheet.Former Sal Nitri Lidan Capsule, prepares according to WS-11331 (ZD-1331)-2002 standard method.Agilent1200 high performance liquid chromatograph; METTLER AE240 electronic analytical balance; Hesperidin reference substance (Nat'l Pharmaceutical & Biological Products Control Institute).
2, method
Measure according to high performance liquid chromatography (Chinese Pharmacopoeia version in 2010 annex V D).
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filler; Methanol-water (25: 75) is mobile phase; Determined wavelength is 284nm.Number of theoretical plate calculates should be not less than 3000 by Hesperidin peak.
The preparation of reference substance solution gets Hesperidin reference substance in right amount, accurately weighed, adds methanol and makes the solution of every 1ml containing 0.2mg, to obtain final product.
Sal Nitri cholagogic tablet of the present invention is got in the preparation of product need testing solution of the present invention, porphyrize, get 0.33g, accurately weighed, put in tool plug conical flask, precision adds methanol 50ml, close plug, weighed weight, supersound process 45 minutes, let cool, weighed weight again, the weight of less loss is supplied with methanol, filter, precision measures subsequent filtrate 5ml, evaporate to dryness, add water and make dissolving in right amount, by D101 type macroporous adsorptive resins (internal diameter 1.5cm, long 9cm), use water and each 120ml eluting of 17% methanol solution respectively, discard eluent, use 2% piconol solution 120ml eluting again, collect eluent, evaporate to dryness, residue adds methanol makes dissolving, be transferred in 10ml measuring bottle, add methanol dilution to scale, shake up, filter, get subsequent filtrate, obtain.
The Sal Nitri Lidan Capsule of this contrast is got in the preparation of reference product need testing solution, porphyrize, get lg, accurately weighed, put in tool plug conical flask, precision adds methanol 50ml, close plug, weighed weight, supersound process 45 minutes, let cool, weighed weight again, the weight of less loss is supplied with methanol, filter, precision measures subsequent filtrate 5ml, evaporate to dryness, add water and make dissolving in right amount, by D101 type macroporous adsorptive resins (internal diameter 1.5cm, long 9cm), use water and each 120ml eluting of 17% methanol solution respectively, discard eluent, use 2% piconol solution 120ml eluting again, collect eluent, evaporate to dryness, residue adds methanol makes dissolving, be transferred in 10ml measuring bottle, add methanol dilution to scale, shake up, filter, get subsequent filtrate, obtain.
Algoscopy is accurate respectively draws reference substance solution 3 μ l and need testing solution 5 μ l, injection liquid chromatography, measures, to obtain final product.
3, result
Result shows, in Sal Nitri cholagogic tablet of the present invention, the content of Hesperidin is 9.5-19mg/ sheet; And the content of Hesperidin is 1.5mg/ grain in former Sal Nitri Lidan Capsule, the content of hesperidin each serving consumption 1 is 2-4 times of original capsule content, and when dose reduces, content of hesperidin improves a lot.
Above-mentioned research shows, adopts Sal Nitri cholagogic tablet prepared by preparation method of the present invention, Sal Nitri Lidan Capsule prepared by the method that active constituent content is recorded higher than WS-11331 (ZD-1331)-2002 standard far away.
Summary of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of preparation method of Sal Nitri cholagogic tablet.
Another object of the present invention is to provide a kind of Sal Nitri cholagogic tablet to suppress the application in mice anus sarcoma cell S-180 cell proliferation in preparation.
The object of the invention is by following scheme realize:
A kind of preparation method of Sal Nitri cholagogic tablet, be made up as crude drug of Radix Bupleuri (processed with vinegar) 165g, Pericarpium Citri Reticulatae Viride 165g, Radix Scutellariae 165g, Radix Paeoniae Alba 165g, Radix Et Rhizoma Rhei 66g, Radix Curcumae 165g, Herba Lysimachiae 165g, Spora Lygodii 165g, boiling hot Endothelium Corneum Gigeriae Galli 165g, Herba Artemisiae Scopariae 165g, Rhizoma Curcumae Longae 165g, vinegar Rhizoma Sparganii 110g, Radix Clematidis 165g, described preparation method is made up of the following step: get Radix Bupleuri (processed with vinegar), Herba Artemisiae Scopariae, Radix Curcumae, Pericarpium Citri Reticulatae Viride, Rhizoma Curcumae Longae, Rhizoma Sparganii, join CO 2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 4-6%, extracting pressure 20-30MPa, temperature 30-50 DEG C, CO 2flow l-3ml/g crude drug min, extraction time 240-300min, obtains supercritical extract, for subsequent use; Get all the other Chinese medicines, pulverize, add 70% ethanol of 5L, drop in microwave extracting apparatus and carry out microwave extracting, extraction power 600-800W, extracts 2 times, each 5-10 minute, combining extraction liquid, concentrated, be added on Dl01 macroporous adsorptive resins, 70% ethanol elution, collect 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain microwave extraction thing, for subsequent use; By above-mentioned supercritical extract and the mixing of microwave extraction thing, add starch, 70% ethanol glue capsule, dry, tabletting, makes 333, the heavy 0.5g of every sheet.
In the preparation method of above-mentioned Sal Nitri cholagogic tablet, described CO 2in supercritical extraction, entrainer accounts for the percent by volume of total extractant is 5%.
In the preparation method of above-mentioned Sal Nitri cholagogic tablet, described CO 2in supercritical extraction, extracting pressure is 25MPa.
In the preparation method of above-mentioned Sal Nitri cholagogic tablet, described CO 2in supercritical extraction, extraction temperature is 40 DEG C.
In the preparation method of above-mentioned Sal Nitri cholagogic tablet, described CO 2cO in supercritical extraction 2flow 2ml/g crude drug min.
In the preparation method of above-mentioned Sal Nitri cholagogic tablet, described CO 2in supercritical extraction, extraction time is 270min.
In the preparation method of above-mentioned Sal Nitri cholagogic tablet, described microwave extracting power is 700W.
In the preparation method of above-mentioned Sal Nitri cholagogic tablet, each extraction time of described microwave extracting is 8 minutes.
Above-mentioned Sal Nitri cholagogic tablet suppresses the application in mice anus sarcoma cell S-180 cell proliferation in preparation.
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 the present invention, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following example, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
Get Radix Bupleuri (processed with vinegar) 165g, Pericarpium Citri Reticulatae Viride 165g, Radix Scutellariae 165g, Radix Paeoniae Alba 165g, Radix Et Rhizoma Rhei 66g, Radix Curcumae 165g, Herba Lysimachiae 165g, Spora Lygodii 165g, scald Endothelium Corneum Gigeriae Galli 165g, Herba Artemisiae Scopariae 165g, Rhizoma Curcumae Longae 165g, vinegar Rhizoma Sparganii 110g, Radix Clematidis 165g, by Radix Bupleuri (processed with vinegar), Herba Artemisiae Scopariae, Radix Curcumae, Pericarpium Citri Reticulatae Viride, Rhizoma Curcumae Longae, Rhizoma Sparganii, join CO 2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 5%, extracting pressure 25MPa, temperature 40 DEG C, CO 2flow 2ml/g crude drug min, extraction time 270min, obtains supercritical extract, for subsequent use; Get all the other Chinese medicines, pulverize, add 70% ethanol of 5L, drop in microwave extracting apparatus and carry out microwave extracting, extraction power 700W, extracts 2 times, each 8 minutes, combining extraction liquid, concentrated, be added on Dl01 macroporous adsorptive resins, 70% ethanol elution, collect 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain microwave extraction thing, for subsequent use; By above-mentioned supercritical extract and the mixing of microwave extraction thing, add starch, 70% ethanol glue capsule, dry, tabletting, makes 333, the heavy 0.5g of every sheet.
After testing, in finished product, the content of Hesperidin is 18.9mg/ sheet.
Embodiment 2
Get Radix Bupleuri (processed with vinegar) 165g, Pericarpium Citri Reticulatae Viride 165g, Radix Scutellariae 165g, Radix Paeoniae Alba 165g, Radix Et Rhizoma Rhei 66g, Radix Curcumae 165g, Herba Lysimachiae 165g, Spora Lygodii 165g, scald Endothelium Corneum Gigeriae Galli 165g, Herba Artemisiae Scopariae 165g, Rhizoma Curcumae Longae 165g, vinegar Rhizoma Sparganii 110g, Radix Clematidis 165g, by Radix Bupleuri (processed with vinegar), Herba Artemisiae Scopariae, Radix Curcumae, Pericarpium Citri Reticulatae Viride, Rhizoma Curcumae Longae, Rhizoma Sparganii, join CO 2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 6%, extracting pressure 30MPa, temperature 30 DEG C, CO 2flow 3ml/g crude drug min, extraction time 300min, obtains supercritical extract, for subsequent use; Get all the other Chinese medicines, pulverize, add 70% ethanol of 5L, drop in microwave extracting apparatus and carry out microwave extracting, extraction power 800W, extracts 2 times, each 5 minutes, combining extraction liquid, concentrated, be added on Dl01 macroporous adsorptive resins, 70% ethanol elution, collect 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain microwave extraction thing, for subsequent use; By above-mentioned supercritical extract and the mixing of microwave extraction thing, add starch, 70% ethanol glue capsule, dry, tabletting, makes 333, the heavy 0.5g of every sheet.
After testing, in finished product, the content of Hesperidin is 14.9mg/ sheet.
Embodiment 3
Get Radix Bupleuri (processed with vinegar) 165g, Pericarpium Citri Reticulatae Viride 165g, Radix Scutellariae 165g, Radix Paeoniae Alba 165g, Radix Et Rhizoma Rhei 66g, Radix Curcumae 165g, Herba Lysimachiae 165g, Spora Lygodii 165g, scald Endothelium Corneum Gigeriae Galli 165g, Herba Artemisiae Scopariae 165g, Rhizoma Curcumae Longae 165g, vinegar Rhizoma Sparganii 110g, Radix Clematidis 165g, by Radix Bupleuri (processed with vinegar), Herba Artemisiae Scopariae, Radix Curcumae, Pericarpium Citri Reticulatae Viride, Rhizoma Curcumae Longae, Rhizoma Sparganii, join CO 2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 4%, extracting pressure 20MPa, temperature 50 C, CO 2flow lml/g crude drug min, extraction time 240min, obtains supercritical extract, for subsequent use; Get all the other Chinese medicines, pulverize, add 70% ethanol of 5L, drop in microwave extracting apparatus and carry out microwave extracting, extraction power 600W, extracts 2 times, each 10 minutes, combining extraction liquid, concentrated, be added on Dl01 macroporous adsorptive resins, 70% ethanol elution, collect 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain microwave extraction thing, for subsequent use; By above-mentioned supercritical extract and the mixing of microwave extraction thing, add starch, 70% ethanol glue capsule, dry, tabletting, makes 333, the heavy 0.5g of every sheet.
After testing, in finished product, the content of Hesperidin is 9.5mg/ sheet.
Embodiment 4: Sal Nitri cholagogic tablet suppresses the experimentation data of mice anus sarcoma cell S-180 cell proliferation
1. experiment material
1.1 experiment cell strains
Mice anus sarcoma cell S-180 cell, Shandong University's laboratory cell storehouse, DMEM+10%FBS cellar culture.
1.2 Experimental agents
Drugs: Sal Nitri cholagogic tablet of the present invention: prepare by embodiment 1 method.
Medicinal liquid liquid storage: take 100mg Sal Nitri cholagogic tablet, is dissolved in 5ml dehydrated alcohol, 0.2 μm of frit, 500 μ ldoff pipe subpackages ,-20 DEG C of storages, and simultaneously 0.2 μm of frit dehydrated alcohol is in order to the use of matched group.
1.3 experiment reagent
DMEM (GIBCO company Cat.No.12100-061Lot.No.758137); Hyclone (Tian Hang bio tech ltd, Zhejiang Lot.No.100419); NaHC0 3(Shanghai hundred million chemical reagent company limited Cat.No.11810-033Lot.No.1088387 of a specified duration); Trypsin (AMRESCO company); EDTA (AMRESCO company); Penicillin G Sodium Salt (AMRESCO company 1); Streptomycin Sulfate (AMRESCO); Dehydrated alcohol (Zibo Ya Dulan Trade Co., Ltd.); 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 of U.S. model: SPECTRAMAX 190); C0 2incubator (FORMA model: 3111); Super-clean bench (safe and sound Inc. of Su Jing group moulding number: SW-CJ-ZFD); Pure water instrument (Sprlng company of U.S. 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 (the accurate experimental facilities company in Shanghai 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 μm of filter (MILLIPORE model: SLGP033RB); 1cm culture dish (NEST company), 96 well culture plates (NEST company); Cell counting count board; Centrifuge tube, pipet, Tips are some.
2. experimental technique
1) S-180 cell DMEM+10%FBS is in 37 DEG C, 5%C0 2carry out cellar culture (10cm culture dish), when Growth of Cells is to logarithmic (log) phase, collecting cell, discards culture fluid, PBS fine laundering 3 times, add 3ml 0.25% trypsin-0.04%EDTA, after 37 DEG C of digestion 2min, add 5ml complete medium neutralization reaction wherein, proceeded in centrifuge tube after piping and druming cell, the centrifugal 5min of 1000rpm, adjustment concentration of cell suspension 3 × 10 4individual/ml.
2) enter in 96 well culture plates by cell kind, every hole adds cell suspension 180 μ l, culture plate put into cell culture incubator (37 DEG C, 5%C0 2) cellar culture.
3) according to cell growth status, generally grow to 50%-70%, add Sal Nitri cholagogic tablet solution, 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, buckle method removes supernatant, pats dry gently with absorbent paper, and every hole, as entered 200 μ l dimethyl sulfoxide, is put low-speed oscillation 10min on shaking table, crystal is fully dissolved.The light absorption value in each hole is measured at enzyme-linked immunosorbent assay instrument 490nm place.
6) background (do not add cell, only add culture fluid) is set, control wells (the medicine dissolution medium of cell, same concentrations, culture fluid, MTT, dimethyl sulfoxide) simultaneously, often organizes the multiple hole of setting 6.
7) result represents with the suppression ratio of medicine to cell: cell proliferation suppression ratio (%)=(control wells OD value-dosing holes OD value), control wells OD value × 100%.Experiment repetition 3 times.
3. statistical disposition
Adopt the correlation analysis in Microsoft Excel 2007 software and Student t to check, data represent with mean ± S.D..
4. experimental result
Statistical result showed after mtt assay experiment, compare with matched group, when dosage reaches 5mg/ml, to S-180 cell inhibitory effect variant (P<0.05), dosage this difference when 10mg/ml has significance (P<0.01), has pole significant difference (P<0.001) when dosage reaches 15-20mg/ml.
Table 1 Sal Nitri cholagogic tablet is to S-180 cell inhibitory effect influence research (X ± SD)
Group Drug level (mg/ml) Suppression ratio (%)
Matched group 0 0
1 5 9.52±5.44
2 10 17.31±10.07*
3 15 33.95±13.82**
4 20 45.27±16.99**
Note: compare with matched group, * P<O.01; * P<0.001.
5. experiment conclusion
Sal Nitri cholagogic tablet of the present invention can suppress S-180 cell proliferation, and reduce the Growth of Cells number of S-180 cell, this effect is dose dependent.

Claims (9)

1. the preparation method of a Sal Nitri cholagogic tablet, be made up as crude drug of Radix Bupleuri (processed with vinegar) 165g, Pericarpium Citri Reticulatae Viride 165g, Radix Scutellariae 165g, Radix Paeoniae Alba 165g, Radix Et Rhizoma Rhei 66g, Radix Curcumae 165g, Herba Lysimachiae 165g, Spora Lygodii 165g, boiling hot Endothelium Corneum Gigeriae Galli 165g, Herba Artemisiae Scopariae 165g, Rhizoma Curcumae Longae 165g, vinegar Rhizoma Sparganii 110g, Radix Clematidis 165g, it is characterized in that, described preparation method is made up of the following step: get Radix Bupleuri (processed with vinegar), Herba Artemisiae Scopariae, Radix Curcumae, Pericarpium Citri Reticulatae Viride, Rhizoma Curcumae Longae, Rhizoma Sparganii, join CO 2in supercritical extraction device, ethanol is as entrainer, and the percent by volume that entrainer accounts for total extractant is 4-6%, extracting pressure 20-30MPa, temperature 30-50 DEG C, CO 2flow l-3ml/g crude drug min, extraction time 240-300min, obtains supercritical extract, for subsequent use; Get all the other Chinese medicines, pulverize, add 70% ethanol of 5L, drop in microwave extracting apparatus and carry out microwave extracting, extraction power 600-800W, extracts 2 times, each 5-10 minute, combining extraction liquid, concentrated, be added on Dl01 macroporous adsorptive resins, 70% ethanol elution, collect 5 times amount column volume eluents, decompression recycling ethanol, concentrated and dry, obtain microwave extraction thing, for subsequent use; By above-mentioned supercritical extract and the mixing of microwave extraction thing, add starch, 70% ethanol glue capsule, dry, tabletting, makes 333, the heavy 0.5g of every sheet.
2. the preparation method of the Sal Nitri cholagogic tablet according to claim l, is characterized in that, described CO 2in supercritical extraction, entrainer accounts for the percent by volume of total extractant is 5%.
3. the preparation method of the Sal Nitri cholagogic tablet according to claim l, is characterized in that, described CO 2in supercritical extraction, extracting pressure is 25 MPa.
4. the preparation method of the Sal Nitri cholagogic tablet according to claim l, is characterized in that, described CO 2in supercritical extraction, extraction temperature is 40 DEG C.
5. the preparation method of the Sal Nitri cholagogic tablet according to claim l, is characterized in that, described CO 2cO in supercritical extraction 2flow 2ml/g crude drug min.
6. the preparation method of the Sal Nitri cholagogic tablet according to claim l, is characterized in that, described CO 2in supercritical extraction, extraction time is 270min.
7. the preparation method of the Sal Nitri cholagogic tablet according to claim l, is characterized in that, described microwave extracting power is 700W.
8. the preparation method of the Sal Nitri cholagogic tablet according to claim l, is characterized in that, each extraction time of described microwave extracting is 8 minutes.
9. the Sal Nitri cholagogic tablet described in claim l suppresses the application in mice anus sarcoma cell S-180 cell proliferation in preparation.
CN201410562859.1A 2014-10-21 2014-10-21 Preparation method and application of gallstone-dissolving cholagogue tablets Pending CN104383427A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103638450A (en) * 2013-11-22 2014-03-19 山东中大药业有限公司 Preparation method and application of banksia rose qi-rectifying tablet

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103638450A (en) * 2013-11-22 2014-03-19 山东中大药业有限公司 Preparation method and application of banksia rose qi-rectifying tablet

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
国家药品监督管理局: "《国家中成药标准汇编内科肝胆分册》", 31 December 2002 *

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