Purification method of augustum alkaline

A purification method and technology of Augustus base, applied in the fields of organic chemistry, bulk chemical production, etc., can solve the problems of rare Augustus base research reports, etc., and achieve a short preparation cycle, short extraction time and high efficiency. Effect

Inactive Publication Date: 2012-09-12
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Augustine comes from Amaryllidaceae Augustus Manjusri (C rinum augustum Rox.) The whole plant of the plant, the research report of Augustine is rare in modern research, and the related research of this substance is still in its infancy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 1kg of the whole plant of Manjusri orchid Augustus, crush it, add 90% ethanol with pH 9 to infiltrate for 6 hours, add it to the extraction kettle, and use supercritical CO 2 Extraction, adjust the extraction temperature to 40°C, the extraction pressure to 38MPa, CO 2 The flow rate is 38L / h, extract for 3 hours, adjust the temperature of the separation kettle Ⅰ to 35°C, the pressure to 10MPa, the temperature of the separation kettle Ⅱ to 25°C, and the pressure to 6MPa, collect the extract in the separation kettle, dissolve it with 3% hydrochloric acid aqueous solution, and filter , the filtrate was adjusted to pH 9 with ammonia water, the precipitate was collected, carbon tetrachloride, methanol, and water were mixed according to the ratio (18:18:3), the following phase was the stationary phase, the upper phase was the mobile phase, and high-speed countercurrent chromatography was started instrument, adjust the rotating speed to 900r / min, take the dissolved precipi...

Embodiment 2

[0017] Take 1 kg of the whole plant of Manjusri orchid Augustus, crush it, add 99% ethanol with pH 12 to infiltrate for 2 hours, add it to the extraction kettle, and use supercritical CO 2 Extraction, adjust the extraction temperature to 60°C, the extraction pressure to 25MPa, CO 2 The flow rate is 20L / h, extract for 1h, adjust the temperature of the separation kettle Ⅰ to 45°C, the pressure to 18MPa, the temperature of the separation kettle Ⅱ to 35°C, and the pressure to 10MPa, collect the extract in the separation kettle, dissolve it with 3% hydrochloric acid aqueous solution, and filter , the filtrate was adjusted to pH 8 with ammonia water, the precipitate was collected, carbon tetrachloride, methanol, and water were mixed according to the ratio (18:20:2), the following phase was the stationary phase, the upper phase was the mobile phase, and high-speed countercurrent chromatography was started instrument, adjust the rotating speed to 950r / min, take the dissolved precipita...

Embodiment 3

[0019] Take 10kg of the whole plant of Manjusri orchid Augustus, crush it, add 95% ethanol with pH 10 to infiltrate for 4 hours, add it to the extraction kettle, and use supercritical CO 2 Extraction, adjust the extraction temperature to 50°C, the extraction pressure to 35MPa, CO 2 The flow rate is 35L / h, extract for 2 hours, adjust the temperature of the separation kettle Ⅰ to 38°C, the pressure to 15MPa, the temperature of the separation kettle Ⅱ to 28°C, and the pressure to 8MPa, collect the extract in the separation kettle, dissolve it with 3% hydrochloric acid aqueous solution, and filter , the filtrate was adjusted to pH 9 with ammonia water, the precipitate was collected, carbon tetrachloride, methanol, and water were mixed according to the ratio (18:17:2), the lower phase was the stationary phase, the upper phase was the mobile phase, and high-speed countercurrent chromatography was started Instrument, adjust the rotating speed to adjust 850r / min, take the dissolved pr...

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PUM

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Abstract

The invention provides a purification method of augustum alkaline. The method comprises enabling complete stool of Amaryllidaceae Crinum augustum Rox. to serve as a raw material and be ground, adding alkaline alcohol into the raw material and soaking for 2-8h, adding the raw material into an extraction kettle, utilizing supercritical CO2 to perform extraction, collecting extract, using acid water to dissolve the extract, filtering, using ammonia water to adjust the pH of filtrate to 8-10, utilizing carbon tetrachloride-methanol-water serving as a solvent system and adopting high-speed counter-current chromatographic instrument to separate sediments, and obtaining the high-purity augustum alkaline by drying under reduced pressure. The method is suitable for preparation of the high-purity augustum alkaline.

Description

technical field [0001] The present invention relates to a kind of purifying method of August base, particularly relate to a kind of application supercritical CO 2 Extraction and high-speed countercurrent chromatographic extraction and purification of Augustine. Background technique [0002] Augustine is an isoquinoline alkaloid with formula C 17 h 19 NO 4 , colorless prisms (benzene), mp.174-176°C. Augustine has cytotoxic activity against various cancer cells (BCA-1, HT-1080, LUC-1, MEL-2, COL-2, KB, P-388, A-431, LNCaP, ZR-75 -1, U-373) show cytotoxic activity; Plasmodium that is sensitive or resistant to chloroquine has antimalarial activity. [0003] Augustine comes from Amaryllidaceae Augustus Manjusri (C rinum augustum Rox.) The whole plant of the plant, the research report of Augustine is rare in modern research, and the related research of this substance is still in its infancy. Contents of the invention [0004] The technical problem to be solved by the pre...

Claims

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Application Information

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IPC IPC(8): C07D491/22
CPCY02P20/54
Inventor 刘东锋万冬梅
Owner NANJING ZELANG MEDICAL TECH
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