CN104327072A - Method for extraction and preparation of jatrorrhizine and application of jatrorrhizine in preparation of medicine for prevention and treatment of colon cancer - Google Patents
Method for extraction and preparation of jatrorrhizine and application of jatrorrhizine in preparation of medicine for prevention and treatment of colon cancer Download PDFInfo
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- CN104327072A CN104327072A CN201410685815.8A CN201410685815A CN104327072A CN 104327072 A CN104327072 A CN 104327072A CN 201410685815 A CN201410685815 A CN 201410685815A CN 104327072 A CN104327072 A CN 104327072A
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D455/00—Heterocyclic compounds containing quinolizine ring systems, e.g. emetine alkaloids, protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine
- C07D455/03—Heterocyclic compounds containing quinolizine ring systems, e.g. emetine alkaloids, protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine containing quinolizine ring systems directly condensed with at least one six-membered carbocyclic ring, e.g. protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine
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Abstract
The invention provides a method for extraction and preparation of jatrorrhizine from a traditional Chinese medicinal material and application of jatrorrhizine in preparation of medicine for prevention and treatment of colon cancer. The preparation method adopts an acid-base system solvent method and comprises the following steps: grinding the traditional Chinese medicinal material, adding an acidic (0.1%-2%) aqueous solvent for reflux extraction, recycling the solvent and carrying out an acid-base solvent method to obtain jatrorrhizine of which the purity is greater than 80%. Jatrorrhizine prepared by the method has the advantages of high purity, short period and low cost and the preparation method is friendly to the environment and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of method of utilizing soda acid solvent method to extract from Chinese medicine to prepare jateorhizine and the application in prevention and therapy colon cancer drug thereof.
Background technology
Jateorhizine (Jatrorrhizine) is protoberberine type isoquinoline alkaloid, and molecular formula is C20H20N04, and molecular weight is 338.39, reddish yellow needle crystal, fusing point 208-210 DEG C.There is physiologically active widely, comprise the functions such as antibacterial, analgesia, step-down, immunity moderation, be widely used at field of medicaments.
Stem of Leatherleaf mahonia, the coptis, golden cypress, herba fibraureae recisae, Root of Chinese Barberry are Chinese Pharmacopoeia version in 2010 medicinal material recorded, and all have heat-clearing and damp-drying drug, effect of eliminating fire and detoxication, cure mainly that damp-heat dysentery, jaundice urine red, conjunctival congestion with pain and swelling of the eye, sore furuncle carbuncle are swollen, dysentery and icterohepatitis etc.Modern pharmacological research shows that they all have antibacterial, antiulcer agent, the effect such as antimycotic.Wherein activeconstituents is isoquinoline alkaloid, all containing compositions such as Berberine, jateorhizine, palmatines.
In prior art, there is extraction from the medicinal materials such as Stem of Leatherleaf mahonia, the coptis, golden cypress, Root of Chinese Barberry to obtain Berberine, have no the research of extracting from the coptis, golden cypress, Root of Chinese Barberry and preparing jateorhizine.Patented technology (201210371939.X) has invented a kind of method preparing jateorhizine from Stem of Leatherleaf mahonia, saturated 1% ammoniacal liquor of main employing soaks, with 85-95% ethanolic soln for Extraction solvent, carry out homogenate extraction, adjust pH1-3, elimination insolubles, filtrate regulates pH8-9, upper macroporous resin column enrichment, 50% ethanol elution, and then adopt preparative liquid chromatography separation to obtain jateorhizine.But the method adopts the technology such as macroporous resin wash-out, preparative chromatography separation, and complicated operation, cost is high.Patented technology (200910167852.9) provides a kind of method extracted herba fibraureae recisae total alkaloids, be separated jateorhizine, wherein be separated the sulphuric acid soln that jateorhizine adopts 0.1%-1.0%, dipping, macroporous adsorbent resin, 10%-60% ethanol elution, hydrochloric acid adjusts pH to be 2, after saltouing, after upper silicagel column is refining, adds hydrochloric acid and adjust pH to be 2, dry jateorhizine.This method adopts macroporous resin wash-out, and silica gel chromatographic column band separating technology is more loaded down with trivial details, and the cycle is long, and cost is high, is not suitable for suitability for industrialized production.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of extraction from Chinese medicine and prepares the method for jateorhizine, and jateorhizine, jateorhizine composition are preparing the application in prevention and therapy colon cancer drug.It is simple to operate that the object of inventing is to provide a kind of extraction preparation method, and extraction efficiency is high, and the cycle is short, and cost is low, and purity is high, is applicable to the preparation method of the jateorhizine of suitability for industrialized production, and is applied to prepare prevention and therapy colon cancer drug.
For solving the problems of the technologies described above, technical scheme of the present invention is as follows:
From Chinese medicine, prepare a method for jateorhizine, its feature comprises the following steps:
Pulverizing medicinal materials is placed in extraction vessel, adds acidic aqueous, backflow, filter, recycling design, then uses adjusting PH with base, leaves standstill, and filters, and adjusts pH, adds the sodium-chlor of 5-30%, leave standstill, filter, obtain dry sediment after filtrate is concentrated with acid;
Dry sediment alkaline aqueous solvent redissolves, refluxing extraction, and filter, filtrate regulates pH with alkali, leaves standstill, and filter, filtrate concentrates rear acid for adjusting pH, adds the sodium-chlor of 5-30%, leaves standstill, and filters, drying precipitated; Repeatedly repeat above-mentioned steps, precipitation alkaline aqueous solvent redissolves, and refluxing extraction is filtered, obtained precipitation, precipitation alkaline aqueous solvent redissolves, and filter, filtrate concentrates, and adds the sodium-chlor of 0-30%, leave standstill, filter, drying precipitated, obtain the jateorhizine of content > 80%;
The preferred Stem of Leatherleaf mahonia of described medicinal material, golden cypress, herba fibraureae recisae, the coptis, Root of Chinese Barberry, Root of Hairystalk Tinospora;
Described Extraction solvent is acidic aqueous, the preferred 0.1%-2% of content of acid in solvent, aqueous solvent preferably water, ethanol, methyl alcohol, and acid is hydrochloric acid, sulfuric acid, acetic acid preferably;
Described redissolution solvent is alkaline aqueous solvent, the preferred 8-14 of pH of solvent, aqueous solvent preferably water, ethanol, methyl alcohol, the preferred ammoniacal liquor of alkali, liming, sodium hydroxide, potassium hydroxide;
Acidic conditions pH in described soda acid solvent systems is 0.5-7, and alkaline condition pH is 8-14, the preferred ammoniacal liquor of alkali, liming, sodium hydroxide, potassium hydroxide, and acid is hydrochloric acid, sulfuric acid, acetic acid preferably;
The application in prevention and therapy colon cancer drug prepared by described jateorhizine;
A kind of medicinal compositions, is characterized in that containing described jateorhizine, and containing pharmaceutically acceptable carrier;
Described jateorhizine and preparing the application in prevention and therapy colon cancer drug containing the composition of jateorhizine, is characterized in that described jateorhizine or medicinal compositions can be prepared into oral preparations, injection, suction preparation or external preparation.
The present invention finds that jateorhizine adopts 10mg/kg, 20mg/kg oral administration after further study, has and obviously suppress Apc compared with model group
min/+the size of tumour, the effect of tumour quantity in mice colon and small intestine, and can life cycle be extended.Therefore, available jateorhizine prevention and therapy colorectal carcinoma.
Jateorhizine involved in the present invention extracts preparation method, and adopt nontoxic, full solvent, material extraction to prepare, extraction yield is high, and the cycle is short, simple to operate, and cost is low, is more suitable for suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is that jateorhizine is to Apc
min/+the impact in Mice mouse survival cycle.
Further illustrate the present invention below in conjunction with specific embodiment, but the scope of protection of present invention is not limited to following embodiments.
Embodiment
Embodiment 1:
Getting Stem of Leatherleaf mahonia medicinal powder 1kg adds in extraction vessel, adds 0.2% acid alcohol (50%) solution of 12L, backflow, merging filtrate, recycling design, concentrated medicament, and adjusting PH with base is 10, leaves standstill, and filters.Regulate pH to be 2 after filtrate is concentrated, add the sodium-chlor of 15%, leave standstill, filter.After drying precipitated, redissolve with the alkaline aqueous solution of 30 times of volumes, backflow, filtrate regulates pH to be 10, regulates pH to be 2, adds the sodium-chlor of 15%, leave standstill, filter after filtrate is concentrated.Drying precipitated.This precipitation redissolved with the alkaline aqueous solution of 20 times of volumes, backflow, filters.The aqueous solution precipitated with 9 redissolves, and filter, filtrate concentrates, and leaves standstill, and filter, obtain drying precipitated, it is 89.1% that HPLC method detects its content.
Embodiment 2:
Getting coptis medicinal powder 1kg adds in extraction vessel, adds 0.2% acetic acid alcohol (50%) solution of 12L, backflow, united extraction liquid, recycling design, and then concentrated medicament is 9 with adjusting PH with base, leaves standstill, filtration.Regulate pH to be 1 after filtrate is concentrated, add the sodium-chlor of 15%, leave standstill, filter.After drying precipitated, redissolve with the alkaline aqueous solution of 30 times of volumes, backflow, filters, and filtrate regulates pH9, leaves standstill, and filters, and regulates pH to be 1, adds the sodium-chlor of 15%, leave standstill, filter after filtrate is concentrated.Drying precipitated.This precipitation redissolved with the alkaline aqueous solution of 10 times of volumes, refluxing extraction 1 time, filters.The aqueous solution of precipitation pH9 redissolves, and filters, and filtrate concentrates, and leaves standstill, and filter, obtain drying precipitated, it is 91.3% that HPLC method detects its content.
Embodiment 3:
Getting golden cypress medicinal powder 1kg adds in extraction vessel, adds 0.2% acid alcohol (50%) solution of 12L, backflow, united extraction liquid, recycling design, and then concentrated medicament is 9 with adjusting PH with base, leaves standstill, filtration.Regulate pH to be 1 after filtrate is concentrated, add the sodium-chlor of 15%, leave standstill, filter.After drying precipitated, redissolve with the alkaline aqueous solution of 30 times of volumes, backflow, filters, and filtrate regulates pH9, leaves standstill, and filters, and regulates pH to be 1, adds the sodium-chlor of 15%, leave standstill, filter after filtrate is concentrated.Drying precipitated.This precipitation redissolved with the alkaline aqueous solution of 10 times of volumes, refluxing extraction 1 time, filters.The aqueous solution of precipitation pH9 redissolves, and filters, and filtrate concentrates, and leaves standstill, and filter, obtain drying precipitated, it is 85.1% that HPLC method detects its content.
Embodiment 4:
Apc
min/+mice mouse sub-cage rearing, freely drinks water, from Apc
min/+the birth of Mice mouse starts on the 8th week, administration group is the oral jateorhizine giving 10mg/kg, 20mg/kg respectively, and model group gives high lipid food, successive administration 40 weeks, measure tumor size in small intestine and colon, statistics tumour quantity (table 1) and life cycle (Fig. 1).
From table 1 and Fig. 1, jateorhizine high dose group obviously reduces Apc
min/+the size of Mice small intestine and colon tumor quantity, tumour, extends Apc
min/+the life cycle of Mice mouse.
Table 1. jateorhizine is to Apc
min/+the impact of Mice mouse
Claims (7)
1. from Chinese medicine, extract the method preparing jateorhizine, its feature comprises the following steps:
(1) pulverizing medicinal materials is placed in extraction vessel, adds acidic aqueous, backflow, filter, recycling design, then uses adjusting PH with base, leaves standstill, and filters, and adjusts pH, adds the sodium-chlor of 5-30%, leave standstill, filter, obtain dry sediment after filtrate is concentrated with acid;
(2) dry sediment alkaline aqueous solvent redissolves, refluxing extraction, and filter, filtrate regulates pH with alkali, leaves standstill, and filter, filtrate concentrates rear acid for adjusting pH, adds the sodium-chlor of 5-30%, leaves standstill, and filters, drying precipitated;
(3) repeating step (2) repeatedly, precipitation alkaline aqueous solvent redissolves, refluxing extraction, filter, must precipitate, precipitation alkaline aqueous solvent redissolves, and filters, filtrate concentrates, add the sodium-chlor of 0-30%, leave standstill, filter, drying precipitated, obtain the jateorhizine of content > 80%;
(4) the wherein preferred Stem of Leatherleaf mahonia of (1) Chinese medicinal materials, golden cypress, herba fibraureae recisae, the coptis, Root of Chinese Barberry, Root of Hairystalk Tinospora.
2. according to claim 1, it is characterized in that Extraction solvent is acidic aqueous, the preferred 0.1%-2% of content of acid in solvent, aqueous solvent preferably water, ethanol, methyl alcohol, acid is hydrochloric acid, sulfuric acid, acetic acid preferably.
3. according to claim 1, it is characterized in that redissolution solvent is alkaline aqueous solvent, the preferred 8-14 of pH of solvent, aqueous solvent preferably water, ethanol, methyl alcohol, the preferred ammoniacal liquor of alkali, liming, sodium hydroxide, potassium hydroxide.
4. according to claim 1, it is characterized in that the acidic conditions pH in soda acid solvent systems is 0.5-7, alkaline condition pH is 8-14, the preferred ammoniacal liquor of alkali, liming, sodium hydroxide, potassium hydroxide, and acid is hydrochloric acid, sulfuric acid, acetic acid preferably.
5. the application in prevention and therapy colon cancer drug prepared by jateorhizine according to claim 1.
6. a medicinal compositions, is characterized in that containing jateorhizine according to claim 1, and containing pharmaceutically acceptable carrier.
7. preparing the application in prevention and therapy colon cancer drug described in claim 1 and 6, it is characterized in that described jateorhizine or medicinal compositions can be prepared into oral preparations, injection, suction preparation or external preparation.
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| CN201410685815.8A CN104327072A (en) | 2014-11-25 | 2014-11-25 | Method for extraction and preparation of jatrorrhizine and application of jatrorrhizine in preparation of medicine for prevention and treatment of colon cancer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105541831A (en) * | 2016-01-15 | 2016-05-04 | 辽宁中医药大学 | Medicine root berberrubine derived from amur cork-tree processed product and separation preparation method and application thereof |
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| CN101269132A (en) * | 2008-05-14 | 2008-09-24 | 西南大学 | Coptis chinensis total alkaloid extracting technique |
| CN101429197A (en) * | 2008-12-17 | 2009-05-13 | 西南大学 | Extraction method for joint production of coptis chinensis with coptis chinensis fibrous root as raw material |
| CN101695518A (en) * | 2009-10-10 | 2010-04-21 | 成都中医药大学 | Method for extracting total alkaloid of common fibraurea stems, separate fibriuretinin and jatrorrhizine |
| CN103393780A (en) * | 2013-08-16 | 2013-11-20 | 西南大学 | Extraction method of high-purity coptis total alkaloid |
| CN103450186A (en) * | 2013-07-30 | 2013-12-18 | 西南交通大学 | Method for extracting fibrauretine from berberine production waste fluid |
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2014
- 2014-11-25 CN CN201410685815.8A patent/CN104327072A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101269132A (en) * | 2008-05-14 | 2008-09-24 | 西南大学 | Coptis chinensis total alkaloid extracting technique |
| CN101429197A (en) * | 2008-12-17 | 2009-05-13 | 西南大学 | Extraction method for joint production of coptis chinensis with coptis chinensis fibrous root as raw material |
| CN101695518A (en) * | 2009-10-10 | 2010-04-21 | 成都中医药大学 | Method for extracting total alkaloid of common fibraurea stems, separate fibriuretinin and jatrorrhizine |
| CN103450186A (en) * | 2013-07-30 | 2013-12-18 | 西南交通大学 | Method for extracting fibrauretine from berberine production waste fluid |
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| CN105541831A (en) * | 2016-01-15 | 2016-05-04 | 辽宁中医药大学 | Medicine root berberrubine derived from amur cork-tree processed product and separation preparation method and application thereof |
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