CN1310029C - Method for preparing liangfuwan and method for controlling quality - Google Patents
Method for preparing liangfuwan and method for controlling quality Download PDFInfo
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- CN1310029C CN1310029C CNB2005102000350A CN200510200035A CN1310029C CN 1310029 C CN1310029 C CN 1310029C CN B2005102000350 A CNB2005102000350 A CN B2005102000350A CN 200510200035 A CN200510200035 A CN 200510200035A CN 1310029 C CN1310029 C CN 1310029C
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- liangfu
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- galangin
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- dropping pills
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- 238000000034 method Methods 0.000 title claims description 38
- VCCRNZQBSJXYJD-UHFFFAOYSA-N galangin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=CC=C1 VCCRNZQBSJXYJD-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000013558 reference substance Substances 0.000 claims abstract description 38
- 239000006187 pill Substances 0.000 claims abstract description 36
- CIPSYTVGZURWPT-UHFFFAOYSA-N galangin Natural products OC1=C(Oc2cc(O)c(O)cc2C1=O)c3ccccc3 CIPSYTVGZURWPT-UHFFFAOYSA-N 0.000 claims abstract description 35
- SUYJZKRQHBQNCA-UHFFFAOYSA-N pinobanksin Natural products O1C2=CC(O)=CC(O)=C2C(=O)C(O)C1C1=CC=CC=C1 SUYJZKRQHBQNCA-UHFFFAOYSA-N 0.000 claims abstract description 35
- 235000013421 Kaempferia galanga Nutrition 0.000 claims abstract description 28
- 244000062241 Kaempferia galanga Species 0.000 claims abstract description 28
- 238000003908 quality control method Methods 0.000 claims abstract description 20
- 238000004809 thin layer chromatography Methods 0.000 claims abstract description 11
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 9
- KUFXJZXMWHNCEH-DOMZBBRYSA-N (4as,7r)-1,4a-dimethyl-7-prop-1-en-2-yl-3,4,5,6,7,8-hexahydronaphthalen-2-one Chemical compound C1CC(=O)C(C)=C2C[C@H](C(=C)C)CC[C@]21C KUFXJZXMWHNCEH-DOMZBBRYSA-N 0.000 claims abstract 3
- KUFXJZXMWHNCEH-UHFFFAOYSA-N cyperone Natural products C1CC(=O)C(C)=C2CC(C(=C)C)CCC21C KUFXJZXMWHNCEH-UHFFFAOYSA-N 0.000 claims abstract 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 73
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 59
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- 238000012360 testing method Methods 0.000 claims description 28
- 238000002360 preparation method Methods 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 238000003556 assay Methods 0.000 claims description 3
- TXHIDIHEXDFONW-UHFFFAOYSA-N benzene;propan-2-one Chemical compound CC(C)=O.C1=CC=CC=C1 TXHIDIHEXDFONW-UHFFFAOYSA-N 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical group CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims 7
- 239000012085 test solution Substances 0.000 claims 5
- 239000000741 silica gel Substances 0.000 claims 3
- 229910002027 silica gel Inorganic materials 0.000 claims 3
- 239000012088 reference solution Substances 0.000 claims 2
- 241000234653 Cyperus Species 0.000 claims 1
- 239000012467 final product Substances 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 25
- 230000000694 effects Effects 0.000 abstract description 8
- 235000019439 ethyl acetate Nutrition 0.000 description 18
- 239000003814 drug Substances 0.000 description 15
- 239000000284 extract Substances 0.000 description 14
- 235000019441 ethanol Nutrition 0.000 description 12
- 229940079593 drug Drugs 0.000 description 11
- 239000000341 volatile oil Substances 0.000 description 11
- 239000000052 vinegar Substances 0.000 description 9
- 235000021419 vinegar Nutrition 0.000 description 9
- 239000002024 ethyl acetate extract Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 238000010992 reflux Methods 0.000 description 7
- 206010000087 Abdominal pain upper Diseases 0.000 description 6
- 238000004587 chromatography analysis Methods 0.000 description 6
- 239000006071 cream Substances 0.000 description 6
- 238000009472 formulation Methods 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000003810 ethyl acetate extraction Methods 0.000 description 5
- 239000000796 flavoring agent Substances 0.000 description 5
- 235000019634 flavors Nutrition 0.000 description 5
- 208000007107 Stomach Ulcer Diseases 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000003110 anti-inflammatory effect Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- 201000005917 gastric ulcer Diseases 0.000 description 4
- 239000000825 pharmaceutical preparation Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 230000006837 decompression Effects 0.000 description 3
- 238000012850 discrimination method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229960003511 macrogol Drugs 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 210000002784 stomach Anatomy 0.000 description 3
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 2
- 208000007882 Gastritis Diseases 0.000 description 2
- 230000036592 analgesia Effects 0.000 description 2
- 230000002467 anti-pepsin effect Effects 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007888 film coating Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000036407 pain Effects 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- YALFFHSIVPCNLF-QPSCCSFWSA-N Cyperolone Chemical compound C1[C@H](C(=C)C)CC[C@@]2(C)CC[C@H](O)[C@]21C(C)=O YALFFHSIVPCNLF-QPSCCSFWSA-N 0.000 description 1
- YALFFHSIVPCNLF-UHFFFAOYSA-N Cyperolone Natural products C1C(C(=C)C)CCC2(C)CCC(O)C21C(C)=O YALFFHSIVPCNLF-UHFFFAOYSA-N 0.000 description 1
- 241000699670 Mus sp. Species 0.000 description 1
- 208000008469 Peptic Ulcer Diseases 0.000 description 1
- 206010067171 Regurgitation Diseases 0.000 description 1
- 206010040007 Sense of oppression Diseases 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 210000001015 abdomen Anatomy 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 102000011759 adducin Human genes 0.000 description 1
- 108010076723 adducin Proteins 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 230000001760 anti-analgesic effect Effects 0.000 description 1
- 230000000767 anti-ulcer Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 239000012259 ether extract Substances 0.000 description 1
- OAYLNYINCPYISS-UHFFFAOYSA-N ethyl acetate;hexane Chemical class CCCCCC.CCOC(C)=O OAYLNYINCPYISS-UHFFFAOYSA-N 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- -1 flavone compound Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 230000030136 gastric emptying Effects 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 208000011906 peptic ulcer disease Diseases 0.000 description 1
- 230000003285 pharmacodynamic effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000011003 system suitability test Methods 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
- 229940098465 tincture Drugs 0.000 description 1
- 230000002110 toxicologic effect Effects 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
本发明公开了一种良附滴丸的质量控制方法。质量控制方法包含，以高良姜素为对照品，采用薄层色谱法对良附滴丸中高良姜进行定性鉴别；以α-香附酮为对照品，采用薄层色谱法对良附滴丸中香附进行定性鉴别；以高良姜素为对照品，采用高效液相色谱法对良附滴丸中高良姜素进行含量测定。本发明生产的良附滴丸，具有质量稳定、服用量小、疗效好的特点。同时也具有提取工艺高效可靠、质量控制手段先进的优点。The invention discloses a quality control method of Liangfu dripping pills. The quality control methods include, using galangin as reference substance, using TLC to qualitatively identify galangal in Liangfu dropping pills; using α-cyperone as reference substance, using TLC to identify Zhongxiangfu was qualitatively identified; galangin was used as a reference substance, and the content of galangin in Liangfu dripping pills was determined by high performance liquid chromatography. The Liangfu dripping pill produced by the invention has the characteristics of stable quality, small dosage and good curative effect. At the same time, it also has the advantages of efficient and reliable extraction process and advanced quality control means.
Description
Technical field
The present invention relates to a kind of Chinese medicine dripping pills formulation preparation method and method of quality control thereof for the treatment of epigastric pain, belong to technical field of medicaments.
Technical background
" Liang Fu Wan " is the good prescription that potion treatment cold obstruction causing qi stagnation causes epigastric pain.Liang Fu Wan comes from " good recipe collection armpit ", is made up of galangal and rhizoma cyperi two flavor medicines, has warm stomach and regulates the flow of vital energy, the effect of eliminating cold to stop pain.Modern all have very deep research to galangal and two single medicinal materials of rhizoma cyperi and perfect square.Single report that treatment gastritis, gastric ulcer are just arranged with galangal.Single just have the treatment alimentary canal with rhizoma cyperi, the report of hysterotrismus.Discover that the both is contained abundant volatile oil, the volatile oil of galangal accounts for 1.5% of crude drug, and Rhizoma Cyperi volatile oil accounts for 1.2% of crude drug, and the both has sure anti-inflammatory and analgesic effect.Wherein contain a large amount of Flavonoid substances in the galangal, proof has the effect of significant anti-inflammatory, analgesia, anti-peptic ulcer after deliberation.Britain will be wherein be used for the treatment of gastric ulcer with monomer component.The clinical literature report, the epigastric pain that Liang Fu Wan is used for cold obstruction causing qi stagnation has good curative effect.In addition, galangal and rhizoma cyperi all belong to large medicinal material kind, and galangal is extensively cultivated in Guangdong and Guangxi Provinces, and rhizoma cyperi distributes very wide, and the crude drug price is very cheap, is suitable for commercial production.Because the Liang Fu Wan curative effect is sure, definite, so in national standard has been listed it by country.Liang Fu Wan, former being stated from " 2000 editions one one of Pharmacopoeia of People's Republic of China ", former preparation technology be " above two the flavor, be ground into fine powder, sieve, mixing is used water pill, drying, promptly." water pill belongs to the Chinese medicine conventional dosage forms, though preparation is simple, has following shortcoming:
1. dose is big, Liang Fu Wan day dose be 6～12g, for modern preparation, dose is obviously bigger than normal.
2. microbiological manipulation difficulty, water pill can't effectively be controlled microorganism in whole process of preparation.
3. quality standard is low, and is wayward.
4, bioavilability is low.
Therefore, in order to bring into play the result of treatment of Liang Fu Wan better, it is carried out modified form be very important.
Summary of the invention
Liang Fu Wan is being carried out in the research of modified form, we have considered liquid preparation such as tincture aqua, oral liquid, solid pharmaceutical preparation such as capsule, dispersing tablet, a plurality of formulations such as dripping pill.Its purpose is to keep and to improve former side's curative effect, makes the formulation advanced person again, and the patient is easy to carry, and dose reduces, and is quality controllable.
Owing to contain more volatile effective component in this product prescription, select then poor stability of liquid preparation, and transportation, store and carry inconvenience, be appropriate so equally select solid pharmaceutical preparation with former side.In solid pharmaceutical preparation, dripping pill is compared with other solid pharmaceutical preparations such as common pill, tablet, capsules, and it is fast to have molten diffusing speed, and onset is rapid, and can effectively preserve volatile effective component wherein, has the advantage of better medicament stability.So finally selected pill.Pill belongs to a kind of quick releasing formulation, melts soon, and is scattered, is suitable for the intestines and stomach medication, avoided high-temperature operation on moulding process, and it is complete that volatile oil is kept, and dose is few.By prerun, with pharmacological screening, we find that the anti-inflammatory of Liang Fu Wan, analgesia, antiulcer effective constituent belong to liposoluble constituent more, are highly suitable for dropping pill formulation.
An object of the present invention is to provide a kind of preparation method of liangfuwan, another object of the present invention provides a kind of method of quality control of liangfuwan.Solve the problem that prior art exists.
The preparation method of liangfuwan of the present invention is as follows: galangal and rhizoma cyperi were mixed by weight 1: 1, the ethyl acetate that adds 8 times of weight, refluxing extraction, filter, merging filtrate, filtrate decompression is recycled to the clear cream of no ethyl acetate flavor, and clear cream is mixed by weight 1: 4 with Macrogol 6000, drips and makes dripping pill.
Among the above-mentioned liangfuwan preparation method, reasonable is that galangal is ground into meal, rhizoma cyperi is smashed, and mixes by weight 1: 1, adds 8 times of amount ethyl acetates, soaked refluxing extraction 2 times, each 1 hour 1 hour, filter, merging filtrate, filtrate decompression is recycled to no ethyl acetate and distinguishes the flavor of that density is the clear cream of 1.05-1.10 60 ℃ the time, clear cream and Macrogol 6000 are mixed in 1: 4 ratio, drip and make dripping pill, promptly.
Among the aforesaid liangfuwan preparation method, for fear of volatile ingredient wherein in storage life loss and reduce because the oral cavity sense of discomfort that volatile oil brings, described dripping pill is the dripping pill of bag film-coating.
Among the aforesaid liangfuwan preparation method, rhizoma cyperi is a Rhizoma Cyperi (vinegar processed).
The method of quality control of liangfuwan of the present invention is as follows: be reference substance with the Galangin, adopt thin-layered chromatography that galangal in the liangfuwan is carried out qualitative identification; With α-cyperolone is reference substance, adopts thin-layered chromatography that rhizoma cyperi in the liangfuwan is carried out qualitative identification; With the Galangin is reference substance, adopts high performance liquid chromatography that Galangin in the liangfuwan is carried out assay.
In the method for quality control of aforesaid liangfuwan, the discrimination method of galangal is in the liangfuwan: get dripping pill 1g, put in the triangular flask, loose, be transferred in the separating funnel with hot water 15ml is molten, incorporate in the separating funnel with 10ml ethyl acetate washing triangular flask and with cleansing solution again, with ethyl acetate extraction 2 times (30ml, 20ml), divide and get the ethyl acetate layer, reclaim ethyl acetate to doing, residue adds absolute ethyl alcohol 3ml dissolving, as need testing solution; Other gets the Galangin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to the thin-layered chromatography test, draw need testing solution 2 μ l, reference substance solution 10 μ 1, put respectively on same block of silica GF254 thin layer plate, with volume ratio is that normal hexane-ethyl acetate-glacial acetic acid of 7: 1: 0.5 is a developping agent, launches, and takes out, dry, put under the 254nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the blackening point of same color
In the method for quality control of aforesaid liangfuwan, the discrimination method of rhizoma cyperi is in the liangfuwan: get α-cyperolone reference substance, add methyl alcohol and make the solution that every 1ml contains 1mg, in contrast product solution:, draw each 10 μ l of aforesaid need testing solution and reference substance solution according to the thin-layered chromatography test, put respectively on same block of silica GF254 thin layer plate, with volume ratio is that benzene-acetone of 25: 1 is developping agent, launches, and takes out, dry, put under the 254nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the blackening point of same color.
In the method for quality control of aforesaid liangfuwan, the content assaying method of Galangin is in the liangfuwan:
(1) according to high performance liquid chromatography, be filling agent with the octadecylsilane chemically bonded silica; With volume ratio is that acetonitrile-methyl alcohol-0.4% phosphoric acid of 20: 40: 40 is moving phase; Think that 266nm detects wavelength and detects;
(2) preparation of reference substance solution: it is an amount of to get the Galangin reference substance, and accurate the title decides, and uses dissolve with methanol, makes the solution that every 1ml contains 0.05mg, promptly;
(3) preparation of need testing solution: get the about 1.2g of this product, put in the 50ml measuring bottle, add methyl alcohol 40ml, dissolve in the tepidarium, put coldly, to scale, shake up, filter with methanol constant volume, accurate again the absorption in subsequent filtrate 1ml to the 5ml measuring bottle adds methyl alcohol and is diluted to scale, shakes up, promptly; Determination method, accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject high performance liquid chromatograph, measure.
In the method for quality control of aforesaid liangfuwan, every gram contains galangal with Galangin (C in the liangfuwan
15H
10O
5) meter, must not be less than 4.0mg.
In the method for quality control of aforesaid liangfuwan, every gram contains galangal with Galangin (C in the liangfuwan
15H
10O
5) meter, must not be less than 8.8mg.
In preparation method's process of determining liangfuwan, we utilize pharmacological screening to match, and in that effective constituent is kept under the complete prerequisite, have rationally reduced yield, have kept volatile oil, and the rate of transform that makes Galangin is about 80%.Determined advanced, easy, economic ethyl acetate extraction process.In 3 batches the trial production, produce controlled, good reproducibility, steady quality.
In order to finish the present invention, the applicant has done a large amount of extraction experiments and has researched and developed corresponding content assaying method and verified extracting result of experiment.
1, the investigation of Different Extraction Method
Known active component is Petroleum ether extraction part and the ethyl acetate extraction unit middle low polarity component that grades, and Petroleum ether extraction has partly been represented volatile oil component among the we.Extraction to them can be taked several different methods, has only they are screened, the extracting method that just can obtain carrying out suitability for industrialized production and can adapt to the galenic pharmacy requirement.
1.1 the preparation of sample
One: 80% ethanol of method directly extracts
Take by weighing galangal, each 100g of rhizoma cyperi (vinegar system) (200g altogether), add 8 times of amounts of 80% ethanol, soaked 1 hour, heating and refluxing extraction 1 hour, cooling filters, get filtrate, in the dregs of a decoction, add 8 times of amount 80% ethanol again, refluxed 1 hour, cooling, filter, merge filtrate twice, reclaim ethanol and be concentrated into thick paste, get sample A32.4g, yield 16.2%.
Method two: ethyl acetate extracts
Take by weighing galangal, each 100g of rhizoma cyperi (vinegar system) (200g altogether), add 8 times of amounts of ethyl acetate, soaked 1 hour, heating and refluxing extraction 1 hour, cooling filters, get filtrate, in the dregs of a decoction, add 8 times of amount ethyl acetates again, refluxed 1 hour, cooling, filter, merge filtrate twice, reclaim ethyl acetate and be concentrated into thick paste, get sample B9.6g, yield 4.8%.
Method three: first water is carried and is collected volatile oil, uses 80% alcohol extract again
Take by weighing galangal, each 100g of rhizoma cyperi (vinegar system), add 12 times of water gagings and soaked 1 hour, extracted volatile oil 5 hours, collect volatile oil 2.4ml, cooling filters, and discards filtrate.Estimate water-intake rate 200%, add 95% ethanol 2133ml to determining alcohol 80%, reflux twice, each 1 hour, collect filtrate, reclaim ethanol and be condensed into thick paste, obtain sample C14.4g, yield 7.2%.
Four: 95% ethanol of method directly extracts
Take by weighing galangal, each 100g of rhizoma cyperi (vinegar system) (200g altogether), add 8 times of amounts of ethanol, soaked 1 hour, heating and refluxing extraction 1 hour filters, and gets filtrate, in the dregs of a decoction, add 8 times of amount ethanol again, refluxed 1 hour, cooling filters, merge filtrate twice, reclaim ethanol and be concentrated into thick paste, get sample D26.7g, yield 13.35%.
Method five: water directly extracts
Take by weighing galangal, each 100g of rhizoma cyperi (vinegar system) (200g altogether), add 12 times of water gagings, soaked 1 hour, decocted 1 hour, filter, get filtrate, add 12 times of water gagings again in the dregs of a decoction, decocted 1 hour, cooling filters, merge filtrate twice, be concentrated into thick paste, get sample E62.0g, yield 31%.
1.2 the investigation of Different Extraction Method
(1) measures the extraction ratio of Galangin by HPLC
HPLC chromatographic condition: enlightening horse diamond C
18Post (250 * 4.6mm, 5 μ m); Moving phase is methyl alcohol-0.4% phosphoric acid solution (60: 40); The detection wavelength is 360nm; 40 ℃ of column temperatures; Flow velocity is 1.30ml/ minute.
The preparation of reference substance solution: precision takes by weighing Galangin 4.81mg, puts in the 10ml volumetric flask, adds dissolve with methanol and constant volume, shakes up standby.Accurate again absorption 1ml puts in the 10ml volumetric flask, adds methanol constant volume, shakes up, and concentration is 0.0481mg/ml, in contrast product solution.
The preparation of need testing solution: it is an amount of to get medicinal extract, the accurate title, decide, and in the 100ml measuring bottle, adds methyl alcohol 80ml, sonicated (power is no less than 150W) 30 minutes, be diluted to scale with methyl alcohol, the jolting mixing is drawn in 2ml to the 5ml volumetric flask more respectively, methanol constant volume, take a morsel centrifugal (10000 rev/mins) 10 minutes, take out, get supernatant as need testing solution.
Sample determination: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly.This is tested, and Galangin content is 1.18% in the used galangal.The results are shown in following table
Different Extraction Method is to the influence of Galangin extraction ratio
| Numbering | Medicinal extract yield (%) | The content (%) of Galangin in medicinal extract | The content (mg/200g) of Galangin in the 200g crude drug medicinal extract | Galangin theoretical content (mg) in 200 crude drugs | Extraction ratio (%) |
| Method one method two method three methods four directions method five | 16.2 4.8 7.2 13.35 31.0 | 3.08 10.78 4.45 3.80 / | 997.92 1034.80 640.80 1014.60 / | 1180.0 1180.0 1180.0 1180.0 1180.0 | 84.57 87.69 54.30 85.98 / |
By above HPLC interpretation of result, Galangin content and extraction ratio are all the highest in the ethyl acetate extract (method two), and the medicinal extract yield is minimum, has obtained best extraction effect.
(2) by the TLC quality of Different Extraction Method relatively, each method all can wait the composition proposition with volatile ingredient such as α-rhizoma cyperi (vinegar system) ketone and Galangin (water carry except), but more with the ethyl acetate extract gained.
(3) TLC of ethyl acetate extract and system's extraction method different solvents extract investigates.(the test sample preparation: it is an amount of to get each extract medicinal extract, all adds methyl alcohol and makes the solution that is equivalent to 3.6g crude drug/ml, promptly to extraction method PetroChina Company Limited. of system ether extract, ethyl acetate extract, 80% ethanol extract, water extract and ethyl acetate extract.) compare by TLC, to investigate their difference on chemical constitution.
Analyzed as can be known by TLC, sherwood oil, ethyl acetate propose effective constituents such as Galangin substantially, and directly ethyl acetate extract also can propose compositions such as Galangin substantially.
With α-rhizoma cyperi (vinegar system) ketone is reference substance, is analyzed as can be known by TLC, and sherwood oil, ethyl acetate propose volatile effective components such as cyperolone substantially, and directly ethyl acetate extract also can propose above-mentioned volatile effective component substantially.
To sum up, method two (ethyl acetate extraction) has not only kept volatile oil component, and flavone compound maximum in the galangal can be proposed, and extraction ratio is the highest and yield is minimum, extracts with ethyl acetate so extraction process is definite.
Pharmacodynamics test shows, after Liang Fu Wan changes liangfuwan into, still have good anti-peptic gastric ulcer and antiinflammatory action, and when waiting dosage, both no significant differences, it is better than Liang Fu Wan in turning round the body number of times and promoting of minimizing acetic acid induced mice stomachache reaction aspect gastric emptying.Toxicological test shows that in 4 times of clinical cycles, obvious adverse reaction is not found in 100 times of human dose application and a maximal tolerance dose administration.The result shows that liangfuwan is a safety, effectively new formulation.
Clinical trial protocol according to the approval of national Bureau of Drugs Supervision, show through Sichuan Province's Hospital Affiliated To Chengdu Traditional Chinese Medicine Univ, Huaxi Hospital Attached to Sichuan Univ, the 288 routine liangfuwan treatment epigastric pain II clinical trial phase results of No.1 Hospital of Guiyang Traditional Chinese Medicine College: the clinical effective rate of liangfuwan treatment cold obstruction causing qi stagnation epigastric pain (comprising chronic superficial gastritis and gastric ulcer) is 88.9%, is higher than 5.6 percentage points of reference substance Liang Fu Wans.
Liangfuwan by the present invention produces has steady quality, little, the eutherapeutic characteristics of dose.Also has simultaneously extraction process high efficient and reliable, quality control method advanced person's advantage.
Embodiment
Embodiment 1.The preparation method of liangfuwan.With galangal 93.75g, rhizoma cyperi (vinegar system) 93.75g is raw material, and galangal is ground into meal, and rhizoma cyperi is smashed, add 8 times of amount ethyl acetates, soaked refluxing extraction 2 times 1 hour, each 1 hour, filter, merging filtrate, filtrate decompression is recycled to the clear cream of no ethyl acetate flavor, density is 1.07 in the time of 60 ℃, clear cream and Macrogol 6000 are mixed in 2: 8 ratios, drip and make 1000 of dripping pills, the bag film-coating promptly.The effect that finished product has warm stomach to regulate the flow of vital energy.Be used for the treatment of cold obstruction causing qi stagnation, the acid regurgitation of gastral cavity pain, fullness and oppression of chest and abdomen.The heavy 45mg of every ball, oral, a 0.75～1.5g, a twice-daily.
The method of quality control of liangfuwan.Comprise discrimination method: step is; (1) gets dripping pill 1g, put in the triangular flask, loose with hot water 15ml is molten, be transferred in the separating funnel, incorporate in the separating funnel with 10ml ethyl acetate washing triangular flask and with cleansing solution again, with ethyl acetate extraction 2 times (30ml, 20ml), divide and get the ethyl acetate layer, reclaim ethyl acetate to doing, residue adds absolute ethyl alcohol 3ml dissolving, as need testing solution.Other gets the Galangin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; According to thin-layered chromatography (2000 editions one appendix VI B of Chinese Pharmacopoeia) test, draw need testing solution 2 μ l, reference substance solution 10 μ l, put respectively in same silica G F
254On the thin layer plate, be developping agent, launch, take out, dry, put under the 254nm ultraviolet lamp and inspect with normal hexane-ethyl acetates of 7: 1: 0.5-glacial acetic acid.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the blackening point of same color; (2) get α-cyperolone reference substance, add methyl alcohol and make the solution that every 1ml contains 1mg, in contrast product solution.According to thin-layered chromatography (2000 editions one appendix VI B of Chinese Pharmacopoeia) test, the need testing solution under absorption (1) item and above-mentioned each 10 μ l of reference substance solution put respectively in same silica G F
254On the thin layer plate, be developping agent, launch, take out, dry, put under the 254nm ultraviolet lamp and inspect with benzene-acetone of 25: 1; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the blackening point of same color.Also comprise content assaying method: according to high performance liquid chromatography (2000 editions appendix VID of Chinese Pharmacopoeia), chromatographic condition and system suitability test, octadecylsilane chemically bonded silica is a filling agent; With acetonitrile-methyl alcohol of 20: 40: 40-0.4% phosphoric acid is moving phase; The detection wavelength is 266nm; Number of theoretical plate calculates by the Galangin peak and is not less than 5000; The preparation of reference substance solution, it is an amount of to get the Galangin reference substance, and accurate the title, decide, and uses dissolve with methanol, makes the solution that every 1ml contains 0.05mg, promptly; The about 1.2g of this product is got in the preparation of need testing solution, puts in the 50ml measuring bottle, adds methyl alcohol 40ml, dissolves in the tepidarium, put coldly, to scale, shake up, filter with methanol constant volume, accurate again the absorption in subsequent filtrate 1ml to the 5ml measuring bottle adds methyl alcohol and is diluted to scale, shakes up, promptly; Determination method, accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing inject liquid chromatograph, measure, promptly; The every gram of this product contains galangal with Galangin (C
15H
10O
5) meter, must not be less than 8.8mg.
Claims (6)
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| CN101168008B (en) * | 2007-11-02 | 2011-03-23 | 陈勃 | Medicinal composition with tumor inhibition function and preparation method and application thereof |
| CN105136966B (en) * | 2015-06-29 | 2016-08-17 | 成都中医药大学 | A kind of quality determining method of Liang Fu Wan class preparation |
| CN105056059A (en) * | 2015-07-29 | 2015-11-18 | 王洪安 | Traditional Chinese medicine for treating gastropathy |
| CN108478740A (en) * | 2018-05-07 | 2018-09-04 | 张叶 | It is a kind of to treat Chinese medicine composition of gastrointestinal disease and preparation method thereof |
| CN109596765B (en) * | 2018-12-25 | 2021-02-26 | 贵州黄果树立爽药业有限公司 | Detection method of Liangfu dripping pills |
| CN114835582B (en) * | 2022-04-29 | 2024-03-15 | 贵州黄果树立爽药业有限公司 | Recycling method of Liangfu drop pill extract solvent |
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| CN1541669A (en) * | 2003-04-30 | 2004-11-03 | 天津药物研究院 | Prepared traditional Chinese drug Liangfu drop pills for treating epigastric pain |
| CN1557433A (en) * | 2004-02-06 | 2004-12-29 | 成都和康药业有限责任公司 | Chinese medicine for treating gastric disease |
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| CN1541669A (en) * | 2003-04-30 | 2004-11-03 | 天津药物研究院 | Prepared traditional Chinese drug Liangfu drop pills for treating epigastric pain |
| CN1557433A (en) * | 2004-02-06 | 2004-12-29 | 成都和康药业有限责任公司 | Chinese medicine for treating gastric disease |
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