Korean monkshood root diterpene total alkaloids and preparation method thereof

A technology of diterpenoids and total alkaloids, which can be used in pharmaceutical formulas, plant raw materials, medical preparations containing active ingredients, etc., and can solve problems such as low extraction efficiency, low alkaloid yield, and emulsification in extraction steps. To avoid severe emulsification, low solution viscosity, and less impurities in the extract

Active Publication Date: 2014-10-01
吉林敖东洮南药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction efficiency of the above-mentioned process is low, the emulsification of the extraction step is serious, and the extraction under acidic conditions causes a serious loss of alkaloids, and when the macroporous resin is adsorbed, the alkaloids will also be greatly lost, which also leads to a relatively low yield of total alkaloids

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] 5kg of Guanbaifu medicinal material, pulverized, extracted with supercritical carbon dioxide, adding methanol with a ratio of 1:10 to the medicinal material as an entrainer, the extraction pressure was 16MPa, the extraction temperature was 35°C, and supercritical CO 2 The flow rate is 40kg / h, the extraction time is 5 hours, the analytical pressure is 10MPa, and the analytical temperature is 60°C. Recover the solvent to obtain the extract, dissolve it with 10L of 1% hydrochloric acid, alkalinize the pH to 10 with concentrated ammonia water, extract 4 times with chloroform, 6L each time, combine the chloroform layers, wash 6 times with 5L ammonia water with pH 11, recover the chloroform, and remove the chloroform at 80 ℃ and dried under reduced pressure to obtain 262 g of total alkaloids of Guanbaifu, with a content of 52% in total alkaloids (calculated as Guanfu A).

Embodiment 2

[0068] Weigh 3 kg of Guanbaifu medicinal material, pulverize it, place it in an extraction kettle, and perform supercritical extraction with carbon dioxide. Add acetone with a ratio of 1:1.5 to the medicinal material as an entrainer. The extraction pressure is 50 MPa, the extraction temperature is 30 °C, and the supercritical CO 2 The flow rate is 30kg / h, the extraction time is 4 hours, the analytical pressure is 8MPa, and the analytical temperature is 50°C. Recover the solvent to obtain the extract, dissolve it with 6L 1% hydrochloric acid, alkalinize the pH to 10 with sodium carbonate, extract 5 times with 3L ethyl acetate, combine the ethyl acetate layers, wash twice with 30L aqueous sodium carbonate solution of pH 12, and recover acetic acid Ethyl ester was dried under reduced pressure at 80°C to obtain 168 g of total alkaloids of Guanbaifu, with a content of 57% in total alkaloids (calculated as Guanfu A).

Embodiment 3

[0070] Pulverize 6.5kg of Guanbai herb, extract with supercritical carbon dioxide in the extraction kettle, add ethanol with a ratio of 1:20 to the medicinal material as an entrainer, extract at a pressure of 25MPa, extract at a temperature of 70°C, and use supercritical CO 2 The flow rate is 45kg / h, the extraction time is 6 hours, the analytical pressure is 11MPa, and the analytical temperature is 45°C. Recover the solvent to obtain the extract, dissolve it with 6.5L 3% hydrochloric acid, alkalinize the pH to 10 with sodium hydroxide, extract 3 times with a mixed solvent of 13L dichloromethane and methanol (3:1), combine the organic layers, and use 8L pH9 hydrogen The sodium oxide aqueous solution was washed 3 times, the organic layer was recovered, and dried under reduced pressure at 80°C to obtain 355 g of total alkaloids of Guanbaifu, with a content of 50% in total alkaloids (calculated as Guanfu A).

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Abstract

The invention provides Korean monkshood root diterpene total alkaloids and a preparation method thereof and specifically discloses a method for preparing diterpene total alkaloids from Korean monkshood. According to the method, a CO2 supercritical extraction method is used to extract Korean monkshood root, then acidification-alkalization-extraction treatment is carried out, and obtained extract is washed with alkaline water. Specifically speaking, the method comprises the following steps: step 1, taking the medicinal material--the Korean monkshood root and subjecting the Korean monkshood root to supercritical extraction with CO2 as a solvent; step 2, dissolving the extract obtained in the step 1 with acid water, subjecting an obtained acid water solution to alkalization and then carrying out extraction with an organic solvent; and step 3, washing the organic solvent extract obtained in the step 2 with alkaline water so as to recover the organic solvent. The content of the total alkaloids is as high as more than 50%, and the content of the poisonous component--Guanfu base H is greatly decreased.

Description

technical field [0001] The invention relates to a method for preparing total diterpenoid alkaloids of Guanbaifu from Chinese herbal medicines, in particular, extracting, extracting and separating the root of Aconitum coreanum (Lévl.) Rapaics of the Ranunculaceae plant Method of Guanbaifu diterpenoid total alkaloids. Background technique [0002] The traditional Chinese medicine Aconitum coreanum (Lévl.) Rapaics is a medicinal plant mainly produced in northern my country, and its root is called Guanbaifu, which is one of the commonly used traditional Chinese medicines. The effect of reducing phlegm and relieving pain is good in folk medicine. Its chemical composition is mainly composed of Guanfu base G (GFG), Guanfu base A (GFA), Guanfu base I (GFI), Guanfu base I, Guanfu base , Guanfu Z, etc., are a series of new C20 diterpene alkaloids whose mother nucleus is Hetisine. Among them, Guanfu A is a new type of safe and effective broad-spectrum anti-arrhythmic drug discovered ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/714A61K125/00
Inventor 董秀华孙申国朱天全曾艳李娜吴丹刘巍程志国
Owner 吉林敖东洮南药业股份有限公司
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