CN102001997A - Method for refining dauricine - Google Patents
Method for refining dauricine Download PDFInfo
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- CN102001997A CN102001997A CN2010105202251A CN201010520225A CN102001997A CN 102001997 A CN102001997 A CN 102001997A CN 2010105202251 A CN2010105202251 A CN 2010105202251A CN 201010520225 A CN201010520225 A CN 201010520225A CN 102001997 A CN102001997 A CN 102001997A
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- dauricine
- chloroform
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention relates to a method for refining dauricine, which comprises the following steps of: supercritically extracting asiatic moonseed rhizome total alkaloids serving as raw materials for 2 to 6 hours in a CO2 solvent; dissolving an analytic substance by using acid aqueous solution, filtering, concentrating the filtrate, and adding ammonia water to regulate the pH value to be 8 to 10; adding chloroform for extraction, adding the chloroform extracting solution into an alumina medium-pressure short thick column, washing to neutral, and performing gradient elution by using the chloroform and methanol; performing thin-layer detection, collecting subsections with higher dauricine content, and recovering a reagent; and crystallizing and drying at low temperature so as to prepare high-content dauricine. In the method for producing the dauricine, the consumption of toxic reagent is lower, the purification degree is high, and the product quality is higher.
Description
Technical field:
The present invention relates to a kind of process for purification of dauricine, especially adopt supercritical CO
2Extraction and middle pressure alumina column chromatography are in conjunction with the method for purifying dauricine.
Background technology:
Dauricine has another name called dauricine, daurisoline.Belong to two benzyl tetrahydro isoquinoline Alkaloids.Molecular formula is C
38H
44N
2O
6Molecular weight is 624.76; Molecular structural formula is as follows:
Yellow parilla alkaloid (main component is dauricine Dau and daurisoline Ds) finds to have preferably the effect that resists myocardial ischemia, protect cerebral ischemia-reperfusion injury after deliberation, to effects such as human tumor cells PC-3, the value-added influences of BT5637, and side effect is little.Reports such as Zhou Jian, dauricine has significant concn dependency and restraining effect to adenosine diphosphate (ADP), suprarenin and collagen-induced extracorporeal platelet aggregation.The Zhang Changyuan experiment finds that Dau can be by alleviating the damage that the effect of rabbit Myocardial Lipid Peroxidation is caused, and enhance SOD activity improves oxygen radical removing ability, and the rabbit myocardial ischemia-reperfusion injury is had certain protective role.Dau can obviously suppress by MM-LDL, the increasing of MM-VLDL inductive vitro culture monocyte PDGF-B protein content, and its mechanism of action is unclear as yet.There are some researches show that Dau is a kind of neuron calcium channel blocker, can significantly suppress high K
+The emergence that depolarize causes " fast phase " Ca
2+Interior stream, but do not influence basic Ca
2+Interior stream.Find also that in recent years Dau has antitumor action, human nasopharyngeal epithelioma 1 had cytotoxicity, human leukemia cell HL60 and K526 there is obvious cytostatic effect, and be concentration dependent, the K562/ADM cell is reduced the IC50 of adriamycin and vincristine, the concentration of Zorubicin and daunorubicin raises in the cell, but to the amount of the glycoprotein P-170 of K562/ADM surface of cell membrane with distribute and do not change.
Existing technology has: Japanese scholar just obtains dauricine through alumina column chromatography, but the alumina column chromatography solvent-oil ratio is big, just is used for a small amount of separation; Shenyang Pharmaceutical University adopts anti-distributions partition method to prepare dauricine, and productive rate brings up to 0.43%, but condition is wayward, and solvent-oil ratio is big, complicated operation.
Chinese patent application numbers 90102172.5 discloses a kind of " extracting dauricine technology from yellow parilla ", the employing acidleach is got, with the alkali alkalization, precipitation adds the benzene dissolving, extracts with alkali, add in the chloroform, after alkali cleaning, add the benzene dissolving again, recrystallization 2-3 time, add the acid dissolving, with the alkali alkalization, be washed to neutrality, low-temperature vacuum drying promptly gets product, the product purity that this method is extracted can reach 97%, but repeatedly use noxious solvents such as chloroform, benzene, seriously polluted, organic residual higher, the cost height is unfavorable for big production operation.
Chinese patent application numbers 99116493.8 discloses " application of yellow parilla extract and extraction process thereof and extract ", this invention obtains total alkali earlier from the yellow parilla rhizome, through alkalize slightly total alkali precipitation, get brown paste with the extraction using alcohol phenolic alkaloid again, alkali is molten, filters, tax reduction solution adds the acid neutralization, filter collection precipitation, drying gets the phenol thing.This method gained phenolic alkaloid is a mixture, and resulting dauricine content is low, uses soda acid repeatedly, and is bigger to the structural stability influence of compound.
Chinese patent application numbers 200910232812.8 discloses " a kind of preparation method of dauricine ", and this method adopts high performance counter current extraction process, this method mild condition, but preparation amount is low, has also used toxic reagents such as benzene.
Summary of the invention:
Technical problem to be solved by this invention provides a kind of small-scale operations that is beneficial to, product content height, the process for purification of the dauricine of production safety.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
A kind of process for purification of dauricine is characterized in that comprising following steps:
1) supercritical CO
2Extraction: the Rhizoma Menispermi total alkaloids is dropped in the extraction kettle, feed CO
2, ethanol is made entrainment agent, collects extract;
2) organic solvent extraction: above-mentioned extract is dissolved with acidic aqueous solution, filters, after filtrate concentrates, add ammonia soln and regulate pH to 8-10, add chloroform extraction 2-5 time, merge chloroform extraction liquid;
3) alumina column chromatography: above-mentioned chloroform extraction liquid recovery reagent is become the medicinal extract shape, add in the aluminum oxide and press short wide column, the chloroform-methanol gradient elution, thin layer detects, and collects dauricine high-content flow point section, reclaims reagent, gets the coarse-grain thing;
4) recrystallization: above-mentioned coarse-grain thing is added the saturated dissolving that refluxes of sherwood oil-alcohol mixed solution, and crystallization 2-5 time leaches cryodrying and promptly gets product.
The supercritical CO 2 extraction conditions is in the described step 1): the CO2 flow control is 30-40kg/h, extracts 40-50 ℃ of temperature, extracts pressure 26-44Mpa, and the extraction time is 2-6 hour, resolves pressure 4-8Mpa, and resolution temperature is 52-60 ℃.
The entrainment agent consumption is the 10-20% of material quantity in the described step 1).
Described step 2) acidic aqueous solution is that pH is a kind of in the hydrochloric acid, sulfuric acid, aqueous acetic acid of 1-3 in, consumption be 3-8 doubly.
Aluminum oxide is a 100-200 purpose alkali alumina in the described step 3), and blade diameter length ratio is 1: 3-1: 6.
The alumina column gradient elution is 3BV chloroform-methanol (0: 1) → 4-8BV chloroform-methanol (2: 1) mixing solutions → chloroform-methanol (9: 1) mixing solutions in the described step 3).
Ether-the alcohol mixed solution volume ratio is 1: 1-1: 3 in described step 4) PetroChina Company Limited..
There is following advantage in the present invention: supercritical extraction percentage extraction height, and solvent load is little, stable in properties, production safety, product purity height; The middle alumina column upper prop speed of pressing is fast, and applied sample amount is big, has shortened the production duration.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
Get Rhizoma Menispermi total bases 200g, drop into extraction column, sealing will be extracted temperature and be brought up to 48 ℃, and the knockout tower temperature transfers to 55 ℃, extract pressure 28Mpa, and parsing pressure is 6Mpa, with CO
2Gas is emitted from steel cylinder, is cooled to 0-5 ℃ in the liquefied pot again through behind the gas purifier, liquefaction.Enter storage tank with high-pressure metering pump with CO
2Send into preheater with 20ml ethanol, to assigned temperature and pressure, carry ethanol secretly by the extraction column bottom and enter together with material and contact by preheater, flow velocity 1.0L/min regulates the tower internal pressure, opens relief valve, by relief valve control above-mentioned parameter, dynamic extraction 4 hours.Emit extract after the shutdown; collect extract, add the aqueous hydrochloric acid dissolving of 8 times of pH2, filter; ammoniacal liquor is regulated pH to 8.5; add chloroform and stir extraction, extract the combined chloroform extraction liquid 3 times; reclaim chloroform and get concentrated solution; get alkali alumina (200 orders, consumption and concentrated solution ratio are 4: 1 (W/V)) dress post, concentrated solution is injected; pressurization; wash with water earlier to neutrality, get 3BV methyl alcohol more successively; 6BV chloroform-methanol (2: 1); chloroform-methanol (9: 1) wash-out, thin-layer chromatography detects; collect the high concentration flow segmentation; reclaim reagent, get the coarse-grain thing, add the dissolving of sherwood oil-ethanol (1: 2) reflux; cooling crystallization; recrystallization 3 times leaches; cryodrying gets dauricine, content 98.5%.
Embodiment 2:
Get Rhizoma Menispermi total bases 200g, drop into extraction column, sealing will be extracted temperature and be brought up to 42 ℃, the knockout tower temperature transfers to 58 ℃, extracts pressure 33Mpa, and parsing pressure is 4Mpa, CO2 gas is emitted from steel cylinder, be cooled to 0-5 ℃ in the liquefied pot again, liquefaction through behind the gas purifier.Enter storage tank and CO2 and 20ml ethanol are sent into preheater with high-pressure metering pump, arrive assigned temperature and pressure by preheater, carrying ethanol secretly by the extraction column bottom enters together with material and contacts, flow velocity 1.0L/min, regulate the tower internal pressure, open relief valve, by relief valve control above-mentioned parameter, dynamic extraction 5 hours.Emit extract after the shutdown; collect extract, add the aqueous hydrochloric acid dissolving of 8 times of pH2, filter; ammoniacal liquor is regulated pH to 9.0; add chloroform and stir extraction, extract the combined chloroform extraction liquid 5 times; reclaim chloroform and get concentrated solution; get alkali alumina (200 orders, consumption and concentrated solution ratio are 5: 1 (W/V)) dress post, concentrated solution is injected; pressurization; wash with water earlier to neutrality, get 3BV methyl alcohol more successively; 5BV chloroform-methanol (2: 1); chloroform-methanol (9: 1) wash-out, thin-layer chromatography detects; collect the high concentration flow segmentation; reclaim reagent, get the coarse-grain thing, add the dissolving of sherwood oil-ethanol (1: 2) reflux; cooling crystallization; recrystallization 5 times leaches; cryodrying gets dauricine, content 99.1%.
Embodiment 3:
Get Rhizoma Menispermi total bases 500g, drop into extraction column, sealing will be extracted temperature and be brought up to 46 ℃, and the knockout tower temperature transfers to 53 ℃, extract pressure 41Mpa, and parsing pressure is 8Mpa, with CO
2Gas is emitted from steel cylinder, is cooled to 0-5 ℃ in the liquefied pot again through behind the gas purifier, liquefaction.Enter storage tank with high-pressure metering pump with CO
2Send into preheater with 75ml ethanol, to assigned temperature and pressure, carry ethanol secretly by the extraction column bottom and enter together with material and contact by preheater, flow velocity 1.0L/min regulates the tower internal pressure, opens relief valve, by relief valve control above-mentioned parameter, dynamic extraction 3 hours.Emit extract after the shutdown; collect extract, add the aqueous hydrochloric acid dissolving of 8 times of pH2, filter; ammoniacal liquor is regulated pH to 8.5; add chloroform and stir extraction, extract the combined chloroform extraction liquid 3 times; reclaim chloroform and get concentrated solution; get alkali alumina (200 orders, consumption and concentrated solution ratio are 3: 1 (W/V)) dress post, concentrated solution is injected; pressurization; wash with water earlier to neutrality, get 3BV methyl alcohol more successively; 8BV chloroform-methanol (2: 1); chloroform-methanol (9: 1) wash-out, thin-layer chromatography detects; collect the high concentration flow segmentation; reclaim reagent, get the coarse-grain thing, add the dissolving of sherwood oil-ethanol (1: 2) reflux; cooling crystallization; recrystallization 4 times leaches; cryodrying gets dauricine, content 98.7%.
Embodiment 4:
Get Rhizoma Menispermi total bases 500g, drop into extraction column, sealing will be extracted temperature and be brought up to 47 ℃, and the knockout tower temperature transfers to 56 ℃, extract pressure 36Mpa, and parsing pressure is 5Mpa, with CO
2Gas is emitted from steel cylinder, is cooled to 0-5 ℃ in the liquefied pot again through behind the gas purifier, liquefaction.Enter storage tank with high-pressure metering pump with CO
2Send into preheater with 100ml ethanol, to assigned temperature and pressure, carry ethanol secretly by the extraction column bottom and enter together with material and contact by preheater, flow velocity 1.0L/min regulates the tower internal pressure, opens relief valve, by relief valve control above-mentioned parameter, dynamic extraction 2 hours.Emit extract after the shutdown; collect extract, add the aqueous hydrochloric acid dissolving of 8 times of pH2, filter; ammoniacal liquor is regulated pH to 9.5; add chloroform and stir extraction, extract the combined chloroform extraction liquid 4 times; reclaim chloroform and get concentrated solution; get alkali alumina (200 orders, consumption and concentrated solution ratio are 2: 1 (W/V)) dress post, concentrated solution is injected; pressurization; wash with water earlier to neutrality, get 3BV methyl alcohol more successively; 4BV chloroform-methanol (2: 1); chloroform-methanol (9: 1) wash-out, thin-layer chromatography detects; collect the high concentration flow segmentation; reclaim reagent, get the coarse-grain thing, add the dissolving of sherwood oil-ethanol (1: 2) reflux; cooling crystallization; recrystallization 2 times leaches; cryodrying gets dauricine, content 98.2%.
Embodiment 5:
Get Rhizoma Menispermi total bases 1000g, drop into extraction column, sealing will be extracted temperature and be brought up to 41 ℃, and the knockout tower temperature transfers to 52 ℃, extract pressure 27Mpa, and parsing pressure is 7Mpa, with CO
2Gas is emitted from steel cylinder, is cooled to 0-5 ℃ in the liquefied pot again through behind the gas purifier, liquefaction.Enter storage tank with high-pressure metering pump with CO
2Send into preheater with 130ml ethanol, to assigned temperature and pressure, carry ethanol secretly by the extraction column bottom and enter together with material and contact by preheater, flow velocity 1.0L/min regulates the tower internal pressure, opens relief valve, by relief valve control above-mentioned parameter, dynamic extraction 5 hours.Emit extract after the shutdown; collect extract, add the aqueous hydrochloric acid dissolving of 8 times of pH2, filter; ammoniacal liquor is regulated pH to 10; add chloroform and stir extraction, extract the combined chloroform extraction liquid 3 times; reclaim chloroform and get concentrated solution; get alkali alumina (200 orders, consumption and concentrated solution ratio are 4: 1 (W/V)) dress post, concentrated solution is injected; pressurization; wash with water earlier to neutrality, get 3BV methyl alcohol more successively; 7BV chloroform-methanol (2: 1); chloroform-methanol (9: 1) wash-out, thin-layer chromatography detects; collect the high concentration flow segmentation; reclaim reagent, get the coarse-grain thing, add the dissolving of sherwood oil-ethanol (1: 2) reflux; cooling crystallization; recrystallization 4 times leaches; cryodrying gets dauricine, content 98.6%.
Embodiment 6:
Get Rhizoma Menispermi total bases 1000g, drop into extraction column, sealing will be extracted temperature and be brought up to 49 ℃, and the knockout tower temperature transfers to 57 ℃, extract pressure 26Mpa, and parsing pressure is 6Mpa, with CO
2Gas is emitted from steel cylinder, is cooled to 0-5 ℃ in the liquefied pot again through behind the gas purifier, liquefaction.Enter storage tank with high-pressure metering pump with CO
2Send into preheater with 140ml ethanol, to assigned temperature and pressure, carry ethanol secretly by the extraction column bottom and enter together with material and contact by preheater, flow velocity 1.0L/min regulates the tower internal pressure, opens relief valve, by relief valve control above-mentioned parameter, dynamic extraction 6 hours.Emit extract after the shutdown; collect extract, add the aqueous hydrochloric acid dissolving of 8 times of pH2, filter; ammoniacal liquor is regulated pH to 8.0; add chloroform and stir extraction, extract the combined chloroform extraction liquid 5 times; reclaim chloroform and get concentrated solution; get alkali alumina (200 orders, consumption and concentrated solution ratio are 5: 1 (W/V)) dress post, concentrated solution is injected; pressurization; wash with water earlier to neutrality, get 3BV methyl alcohol more successively; 6BV chloroform-methanol (2: 1); chloroform-methanol (9: 1) wash-out, thin-layer chromatography detects; collect the high concentration flow segmentation; reclaim reagent, get the coarse-grain thing, add the dissolving of sherwood oil-ethanol (1: 2) reflux; cooling crystallization; recrystallization 5 times leaches; cryodrying gets dauricine, content 99.4%.
Embodiment 7:
Get Rhizoma Menispermi total bases 2000g, drop into extraction column, sealing will be extracted temperature and be brought up to 45 ℃, and the knockout tower temperature transfers to 60 ℃, extract pressure 44Mpa, and parsing pressure is 8Mpa, with CO
2Gas is emitted from steel cylinder, is cooled to 0-5 ℃ in the liquefied pot again through behind the gas purifier, liquefaction.Enter storage tank with high-pressure metering pump with CO
2Send into preheater with 200ml ethanol, to assigned temperature and pressure, carry ethanol secretly by the extraction column bottom and enter together with material and contact by preheater, flow velocity 1.0L/min regulates the tower internal pressure, opens relief valve, by relief valve control above-mentioned parameter, dynamic extraction 4 hours.Emit extract after the shutdown; collect extract, add the aqueous hydrochloric acid dissolving of 8 times of pH2, filter; ammoniacal liquor is regulated pH to 9.5; add chloroform and stir extraction, extract the combined chloroform extraction liquid 3 times; reclaim chloroform and get concentrated solution; get alkali alumina (200 orders, consumption and concentrated solution ratio are 3: 1 (W/V)) dress post, concentrated solution is injected; pressurization; wash with water earlier to neutrality, get 3BV methyl alcohol more successively; 5BV chloroform-methanol (2: 1); chloroform-methanol (9: 1) wash-out, thin-layer chromatography detects; collect the high concentration flow segmentation; reclaim reagent, get the coarse-grain thing, add the dissolving of sherwood oil-ethanol (1: 2) reflux; cooling crystallization; recrystallization 4 times leaches; cryodrying gets dauricine, content 99.0%.
Claims (7)
1. the process for purification of a dauricine is characterized in that comprising following steps:
1) supercritical CO
2Extraction: the Rhizoma Menispermi total alkaloids is dropped in the extraction kettle, feed CO
2, ethanol is made entrainment agent, collects extract;
2) organic solvent extraction: above-mentioned extract is dissolved with acidic aqueous solution, filters, after filtrate concentrates, add ammonia soln and regulate pH to 8-10, add chloroform extraction 2-5 time, merge chloroform extraction liquid;
3) alumina column chromatography: above-mentioned chloroform extraction liquid recovery reagent is become the medicinal extract shape, add in the aluminum oxide and press short wide column, the chloroform-methanol gradient elution, thin layer detects, and collects dauricine high-content flow point section, reclaims reagent, gets the coarse-grain thing;
4) recrystallization: above-mentioned coarse-grain thing is added the saturated dissolving that refluxes of sherwood oil-alcohol mixed solution, and crystallization 2-5 time leaches cryodrying and promptly gets product.
2. press the process for purification of the described a kind of dauricine of claim 1, it is characterized in that the supercritical CO 2 extraction conditions is in the described step 1): the CO2 flow control is 30-40kg/h, extract 40-50 ℃ of temperature, extract pressure 26-44Mpa, the extraction time is 2-6 hour, resolve pressure 4-8Mpa, resolution temperature is 52-60 ℃.
3. by the process for purification of the described a kind of dauricine of claim 1, it is characterized in that the entrainment agent consumption is the 10-20% of material quantity in the described step 1).
4. by the process for purification of the described a kind of dauricine of claim 1, it is characterized in that described step 2) in acidic aqueous solution be that pH is a kind of in the hydrochloric acid, sulfuric acid, aqueous acetic acid of 1-3, consumption be 3-8 doubly.
5. by the process for purification of the described a kind of dauricine of claim 1, it is characterized in that aluminum oxide is a 100-200 purpose alkali alumina in the described step 3), blade diameter length ratio is 1: 3-1: 6.
6. by the process for purification of the described a kind of dauricine of claim 1, it is characterized in that the alumina column gradient elution is 3BV chloroform-methanol (0: 1) → 4-8BV chloroform-methanol (2: 1) mixing solutions → chloroform-methanol (9: 1) mixing solutions in the described step 3).
7. by the process for purification of the described a kind of dauricine of claim 1, it is characterized in that ether-the alcohol mixed solution volume ratio is 1: 1-1: 3 in described step 4) PetroChina Company Limited..
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105202251A CN102001997A (en) | 2010-10-26 | 2010-10-26 | Method for refining dauricine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105202251A CN102001997A (en) | 2010-10-26 | 2010-10-26 | Method for refining dauricine |
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| CN102001997A true CN102001997A (en) | 2011-04-06 |
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| CN2010105202251A Pending CN102001997A (en) | 2010-10-26 | 2010-10-26 | Method for refining dauricine |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044496A (en) * | 2012-12-13 | 2013-04-17 | 大兴安岭林格贝有机食品有限责任公司 | Novel technology method for extracting alkaloids from wild menispermum dauricum |
| CN104030982A (en) * | 2014-07-03 | 2014-09-10 | 王健 | Extraction method for dauricine |
| CN115006448A (en) * | 2022-05-30 | 2022-09-06 | 赣江中药创新中心 | High-content rhizoma Menispermi total alkaloid and preparation method thereof |
-
2010
- 2010-10-26 CN CN2010105202251A patent/CN102001997A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044496A (en) * | 2012-12-13 | 2013-04-17 | 大兴安岭林格贝有机食品有限责任公司 | Novel technology method for extracting alkaloids from wild menispermum dauricum |
| CN103044496B (en) * | 2012-12-13 | 2016-09-07 | 大兴安岭林格贝寒带生物科技股份有限公司 | A kind of novel technological method extracting alkaloid from wild Caulis menispermi |
| CN104030982A (en) * | 2014-07-03 | 2014-09-10 | 王健 | Extraction method for dauricine |
| CN115006448A (en) * | 2022-05-30 | 2022-09-06 | 赣江中药创新中心 | High-content rhizoma Menispermi total alkaloid and preparation method thereof |
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Application publication date: 20110406 |