CN102836231A - Preparation method of aconitum episcopale levl. alkaloid - Google Patents
Preparation method of aconitum episcopale levl. alkaloid Download PDFInfo
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- CN102836231A CN102836231A CN 201210373348 CN201210373348A CN102836231A CN 102836231 A CN102836231 A CN 102836231A CN 201210373348 CN201210373348 CN 201210373348 CN 201210373348 A CN201210373348 A CN 201210373348A CN 102836231 A CN102836231 A CN 102836231A
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Abstract
The invention relates to a preparation method of an aconitum episcopale levl. alkaloid. The method comprises the following steps of: (1) smashing an aconitum episcopale levl. medicinal material, soaking with saturated limewater for 5-10 hours, drying in the air, smashing to 40-60 meshes, adding into an extracting tank, adding 80 percent ethanol serving as an entrainer, extracting with supercritical CO2, collecting an extraction liquid, and recovering ethanol to obtain an extract; 2, adding the extract into an acid aqueous solution of which the pH is 2.2-3.0, filtering, making a filtrate pass through a strongly acidic cation exchange resin, washing the resin with water till the water washing liquid becomes neutral, adding resin into alkaline water for alkalifying, and eluting with ethanol to obtain an ethanol eluent; and (3) concentrating the ethanol eluent to an alcohol-free state, passing through a macroporous adsorption resin column, eluting with water, eluting with ethanol, collecting an ethanol eluent, concentrating and drying to obtain a product. The method has the characteristics of high efficiency, low energy consumption, large preparation amount and the like, and is suitable for industrial production.
Description
Technical field
The present invention relates to the alkaloidal method for preparing of a kind of purple monkshood root, particularly relate to a kind of supercritical CO
2The alkaloidal method for preparing of extraction purple monkshood root.
Background technology
Purple monkshood root
Aconitum episcopaleLevl. be the Ranunculaceae aconitum plant, have another name called the Radix Arnebiae (Radix Lithospermi) crow, mainly be distributed in the northern and west and south, Sichuan, Yunnan, once be used to separate aconite poisoning, have function of promoting blood circulation to disperse blood clots.The fifties, isolation identification from purple monkshood root such as Zhu Renhong goes out delavaconitine and yunaconitine, and these two kinds of chemical compounds have tangible local anesthesia effect and certain analgesic effect.Employings such as Ding Lisheng 95% ethanol extraction, acid are dissolved, extracted with diethyl ether defat, ammonia ammonification, neutral alumina column chromatography and preparation of silica gel thin layer chromatography are isolated five diterpene alkaloids from purple monkshood root; Be respectively Deacetylheterophylloidine, Heterophylloidine, Songorine, Talatisamine, 14-Acetyltalaisamine; This method is used a large amount of toxic solvents, and environmental hazard is bigger.
Summary of the invention
The purpose of this invention is to provide the alkaloidal method for preparing of a kind of purple monkshood root, this method technology is simple, fast, favorable reproducibility, preparation amount be big.
The objective of the invention is to realize through following technical scheme:
The alkaloidal method for preparing of a kind of purple monkshood root is characterized in that comprising following steps:
1) gets the fragmentation of purple monkshood root medical material, soaked 5-10 hour, dry, be ground into the 40-60 order, add in the extractor, as entrainer, adopt supercritical CO with 80% alcoholic solution with saturated limewater
2Extract is resolved in extraction, reclaims ethanol, gets extract;
2) aqueous acid of above-mentioned extract adding pH2.2-3.0 dissolves, and filters, and the storng-acid cation exchange resin of filtrating, washed resin to water lotion are neutral, and resin adds aqueous alkali and alkalizes, and ethanol elution gets ethanol elution;
3) above-mentioned ethanol elution is concentrated into nothing alcohol, crosses macroporous adsorptive resins, earlier with water elution, the reuse ethanol elution is collected ethanol elution, concentrates, is drying to obtain product.
Supercritical CO in the said step 1)
2Extraction conditions is: extraction temperature 45-60 ℃, and extracting pressure 25-34Mpa, 2-3 hour dynamic extraction time, it is 6-8Mpa that separator I resolves pressure, resolution temperature 40-50 ℃, separator II resolves pressure 4-6Mpa, resolution temperature 35-45 ℃.
The said sour water of step (2) is hydrochloric acid, aqueous acetic acid.
The said storng-acid cation exchange resin of step (2) is 732, a kind of among the HZ002, HZ016, JK006.
The said macroporous adsorbent resin of step (3) is selected from nonpolar or low pole macroporous resins such as D180, HP10, SP-825, HPD400.
The said macroporous resin eluant of step (3) is selected the 50-75% ethanol elution for use, collects eluent.
Characteristics of the present invention are to adopt supercritical CO
2Extraction combines preparation purple monkshood root alkaloid with ion exchange resin, macroporous resin technology, product yield is high, and is with short production cycle, is easy to industrialization.
The specific embodiment:
To combine the specific embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment 1:
It is broken to get the purple monkshood root medical material, soaks 5 hours with saturated limewater, dries, and is ground into 60 orders; Take by weighing 5kg and add in the extractor sealing, opening device; Extraction temperature is transferred to 48 ℃, extracting pressure 28Mpa, it is 6Mpa that separator I resolves pressure; 43 ℃ of resolution temperatures, separator II resolves pressure 4Mpa, 40 ℃ of resolution temperatures.After reaching above-mentioned parameter, CO
2Gas is emitted from steel cylinder, through behind the gas purifier in liquefied pot, liquefaction, get into storage tank with high-pressure metering pump with CO
2Send into depurator, to assigned temperature and pressure, flow velocity 18kg/h opens pressure regulator valve through preheater; And carry dehydrated alcohol secretly, dynamic extraction 2 hours is resolved extract, reclaims ethanol; The aqueous acetic acid dynamic extraction of 5 times of amounts of extract adding pH3.0 3 times, each 1.5h, merge extractive liquid, concentrates extracting solution; Cross 732 storng-acid cation exchange resins, earlier with wash to water lotion be neutrality, in resin, add ammonia again and alkalize, after alkaloid is dissociated out; Use 85% ethanol elution, collect ethanol elution, being evaporated to does not have the alcohol flavor, crosses the D180 macroporous adsorptive resins; With water elution, reuse 50% ethanol elution is collected eluent earlier, and concentrated, drying obtains 7.8g purple monkshood root total alkaloids extract.
Embodiment 2:
It is broken to get the purple monkshood root medical material, soaks 8 hours with saturated limewater, dries, and is ground into 40 orders; Take by weighing 5kg and add in the extractor sealing, opening device; Extraction temperature is transferred to 53 ℃, extracting pressure 31Mpa, it is 8Mpa that separator I resolves pressure; 48 ℃ of resolution temperatures, separator II resolves pressure 6Mpa, 45 ℃ of resolution temperatures.After reaching above-mentioned parameter, CO
2Gas is emitted from steel cylinder, through behind the gas purifier in liquefied pot, liquefaction, get into storage tank with high-pressure metering pump with CO
2Send into depurator, to assigned temperature and pressure, flow velocity 20kg/h opens pressure regulator valve through preheater; And carry dehydrated alcohol secretly, dynamic extraction 2.5 hours is resolved extract, reclaims ethanol; The aqueous acetic acid dynamic extraction of 4 times of amounts of extract adding pH2.6 2 times, each 1.5h, merge extractive liquid, concentrates extracting solution; Cross the HZ002 storng-acid cation exchange resin, earlier with wash to water lotion be neutrality, in resin, add ammonia again and alkalize, after alkaloid is dissociated out; Use 85% ethanol elution, collect ethanol elution, being evaporated to does not have the alcohol flavor, crosses the HP10 macroporous adsorptive resins; With water elution, reuse 75% ethanol elution is collected eluent earlier, and concentrated, drying obtains the 8.1g total alkaloids extract.
Embodiment 3:
It is broken to get the purple monkshood root medical material, soaks 10 hours with saturated limewater, dries, and is ground into 60 orders; Take by weighing 5kg and add in the extractor sealing, opening device; Extraction temperature is transferred to 60 ℃, extracting pressure 25Mpa, it is 7Mpa that separator I resolves pressure; 50 ℃ of resolution temperatures, separator II resolves pressure 5Mpa, 38 ℃ of resolution temperatures.After reaching above-mentioned parameter, CO
2Gas is emitted from steel cylinder, through behind the gas purifier in liquefied pot, liquefaction, get into storage tank with high-pressure metering pump with CO
2Send into depurator, to assigned temperature and pressure, flow velocity 15kg/h opens pressure regulator valve through preheater; And carry dehydrated alcohol secretly, dynamic extraction 3 hours is resolved extract, reclaims ethanol; The aqueous hydrochloric acid solution dynamic extraction of 5 times of amounts of extract adding pH2.5 3 times, each 1.0h, merge extractive liquid, concentrates extracting solution; Cross the JK006 storng-acid cation exchange resin, earlier with wash to water lotion be neutrality, in resin, add ammonia again and alkalize, after alkaloid is dissociated out; Use 85% ethanol elution, collect ethanol elution, being evaporated to does not have the alcohol flavor, crosses the SP-825 macroporous adsorptive resins; With water elution, reuse 60% ethanol elution is collected eluent earlier, and concentrated, drying obtains the 7.4g total alkaloids extract.
Embodiment 4:
It is broken to get the purple monkshood root medical material, soaks 6 hours with saturated limewater, dries, and is ground into 40 orders; Take by weighing 5kg and add in the extractor sealing, opening device; Extraction temperature is transferred to 45 ℃, extracting pressure 34Mpa, it is 6Mpa that separator I resolves pressure; 40 ℃ of resolution temperatures, separator II resolves pressure 5Mpa, 35 ℃ of resolution temperatures.After reaching above-mentioned parameter, CO
2Gas is emitted from steel cylinder, through behind the gas purifier in liquefied pot, liquefaction, get into storage tank with high-pressure metering pump with CO
2Send into depurator, to assigned temperature and pressure, flow velocity 18kg/h opens pressure regulator valve through preheater; And carry dehydrated alcohol secretly, dynamic extraction 2 hours is resolved extract, reclaims ethanol; The aqueous hydrochloric acid solution dynamic extraction of 4 times of amounts of extract adding pH2.2 3 times, each 1.5h, merge extractive liquid, concentrates extracting solution; Cross the HZ016 storng-acid cation exchange resin, earlier with wash to water lotion be neutrality, in resin, add ammonia again and alkalize, after alkaloid is dissociated out; Use 85% ethanol elution, collect ethanol elution, being evaporated to does not have the alcohol flavor, crosses the HPD400 macroporous adsorptive resins; With water elution, reuse 70% ethanol elution is collected eluent earlier, and concentrated, drying obtains the 7.6g total alkaloids extract.
Claims (6)
1. alkaloidal method for preparing of purple monkshood root is characterized in that comprising following steps:
1) gets the fragmentation of purple monkshood root medical material, soaked 5-10 hour, dry, be ground into the 40-60 order, add in the extractor, as entrainer, adopt supercritical CO with 80% alcoholic solution with saturated limewater
2Extract is resolved in extraction, reclaims ethanol, gets extract;
2) aqueous acid of above-mentioned extract adding pH2.2-3.0 dissolves, and filters, and the storng-acid cation exchange resin of filtrating, washed resin to water lotion are neutral, and resin adds aqueous alkali and alkalizes, and ethanol elution gets ethanol elution;
3) above-mentioned ethanol elution is concentrated into nothing alcohol, crosses macroporous adsorptive resins, earlier with water elution, the reuse ethanol elution is collected ethanol elution, concentrates, is drying to obtain product.
2. the alkaloidal method for preparing of a kind of according to claim 1 purple monkshood root is characterized in that supercritical CO in the said step 1)
2Extraction conditions is: extraction temperature 45-60 ℃, and extracting pressure 25-34Mpa, 2-3 hour dynamic extraction time, it is 6-8Mpa that separator I resolves pressure, resolution temperature 40-50 ℃, separator II resolves pressure 4-6Mpa, resolution temperature 35-45 ℃.
3. the alkaloidal method for preparing of a kind of according to claim 1 purple monkshood root is characterized in that the said sour water of step (2) is hydrochloric acid, aqueous acetic acid.
4. preparation technology according to claim 2 is characterized in that the said storng-acid cation exchange resin of step (2) is 732, a kind of among the HZ002, HZ016, JK006.
5. preparation technology according to claim 2 is characterized in that the said macroporous adsorbent resin of step (3) is selected from nonpolar or low pole macroporous resins such as D180, HP10, SP-825, HPD400.
6. preparation technology according to claim 2 is characterized in that the said macroporous resin eluant of step (3) selects the 50-75% ethanol elution for use, collects eluent.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103134871A (en) * | 2013-02-17 | 2013-06-05 | 四川省中医药科学院 | Preparation method of test solution for detecting aconitine-type alkaloids through high-efficiency liquid phase chromatography |
| CN103980196A (en) * | 2014-06-03 | 2014-08-13 | 海南师范大学 | Preparation method of Pollyalthia laui Merr roots |
| CN106668216A (en) * | 2016-08-17 | 2017-05-17 | 洪雅县瓦屋山药业有限公司 | Method for supercritical CO2 extraction of total alkaloids of radix coptidis deltoideae |
| CN113367242A (en) * | 2021-06-10 | 2021-09-10 | 中国农业科学院草原研究所 | Method for extracting alkaloid from nettle and application of alkaloid as growth promoting additive |
-
2012
- 2012-09-27 CN CN 201210373348 patent/CN102836231A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103134871A (en) * | 2013-02-17 | 2013-06-05 | 四川省中医药科学院 | Preparation method of test solution for detecting aconitine-type alkaloids through high-efficiency liquid phase chromatography |
| CN103980196A (en) * | 2014-06-03 | 2014-08-13 | 海南师范大学 | Preparation method of Pollyalthia laui Merr roots |
| CN106668216A (en) * | 2016-08-17 | 2017-05-17 | 洪雅县瓦屋山药业有限公司 | Method for supercritical CO2 extraction of total alkaloids of radix coptidis deltoideae |
| CN113367242A (en) * | 2021-06-10 | 2021-09-10 | 中国农业科学院草原研究所 | Method for extracting alkaloid from nettle and application of alkaloid as growth promoting additive |
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