Method for purifying dihydro Usambara mountain alkali

A purification method, the technology of dihydrousambala, which is applied in the fields of organic chemistry and bulk chemical production, can solve the problems of the undiscovered extraction and purification method of dihydrousanbara soda, and achieve short preparation cycle, low energy consumption, The effect of short extraction time

Inactive Publication Date: 2012-09-19
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] After searching the literature, no relevant reports on the extraction and purification methods of dihydrousambara sine have been found

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take the bark of 1kg MacBai hardwood, crush it, add 70% ethanol (ammonia water to adjust pH9) and soak for 3 hours, add it to the extraction kettle, use supercritical CO 2 For extraction, adjust extraction temperature to 40℃, extraction pressure to 40MPa, CO 2 The flow rate is 60L / h, the extraction is 3h, the extract is collected in the separation kettle, dissolved with 3% hydrochloric acid aqueous solution, filtered, and ammoniated to collect the precipitate, take petroleum ether, ethyl acetate, methanol, water, press (5:7: 12:3) Proportion mixing, the lower phase is the stationary phase, the upper phase is the mobile phase, the high-speed countercurrent chromatograph is turned on, the speed is adjusted to 900r / min, the ethyl acetate dissolved precipitate is injected into the chromatograph, and the dihydrousambara is collected The fraction of shannine was dried under reduced pressure to obtain 68mg of white dihydro-usambara mountainine. The content was 98.3% by high-phase...

Embodiment 2

[0017] Take the bark of 1kg MacBai hardwood, crush it, add 99% ethanol (ammonia water to adjust pH11) and soak for 8 hours, add it to the extraction kettle, use supercritical CO 2 Extraction, adjust extraction temperature to 65℃, extraction pressure to 25MPa, CO 2 The flow rate is 20L / h, the extraction is 1h, the extract is collected in the separation kettle, dissolved with 3% hydrochloric acid aqueous solution, filtered, and ammoniated to collect the precipitate, take petroleum ether, ethyl acetate, methanol, water, and press (5:3: 5: 3) Proportion mixing, the lower phase is the stationary phase, the upper phase is the mobile phase, turn on the high-speed countercurrent chromatograph, adjust the speed to 950r / min, take the ethyl acetate dissolved precipitate and inject it into the chromatograph, collect the dihydrousambala The fraction of shannine was dried under reduced pressure to obtain 39mg of white dihydrousambara mountainine, which was detected by high-phase liquid phase, ...

Embodiment 3

[0019] Take the bark of 1kg MacBai hardwood, crush it, add 80% ethanol (ammonia water to adjust pH 10) and soak it for 5 hours, add it to the extraction kettle, use supercritical CO 2 Extraction, adjust extraction temperature to 55℃, extraction pressure to 38MPa, CO 2 The flow rate is 40L / h, the extraction is 2h, the extract is collected in the separation kettle, dissolved with 3% hydrochloric acid aqueous solution, filtered, and ammoniated to collect the precipitate, take petroleum ether, ethyl acetate, methanol, water, press (5:6: 7:3) Proportion mixing, the lower phase is the stationary phase, the upper phase is the mobile phase, turn on the high-speed countercurrent chromatograph, adjust the speed to 850r / min, take the ethyl acetate dissolved precipitate and inject it into the chromatograph, and collect the dihydrousambala The fraction of shannine was dried under reduced pressure to obtain 85 mg of white dihydro-usambara mountainine. The content was 98.1% by high-phase liquid...

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Abstract

The invention provides a method for purifying dihydro Usambara mountain alkali. The method comprises the following steps of: crushing barks of apocynaceae plant aspidosperma marcgravianum wood as a raw material, adding alkali liquor and infiltrating for 3-8 hours; adding the infiltrated substance in an extraction kettle; extracting the product in the extraction kettle by adopting supercritical CO2; collecting the extract, dissolving the collected extract with acid water, filtering, aminating and precipitating; separating precipitate by adopting a high-speed countercurrent chromatography with petroleum ether, ethyl acetate, methanol and water as a solvent system; and carrying out drying under reduced pressure to obtain the dihydro Usambara mountain alkali with high content. The method is suitable for preparing the dihydro Usambara mountain alkali with the high content.

Description

Technical field [0001] The invention relates to a method for purifying dihydrousambara mountainine, in particular to an application of supercritical CO 2 A method for extraction and high-speed countercurrent chromatography to extract and purify dihydrousambara mountainine. Background technique [0002] Dihydrousambarashanine is a carboline alkaloid, molecular formula C 29 H 30 N 4 , Mp.143-145°C), [α]D+109.7°(chloroform). Dihydrousambarashanine has anti-Plasmodium falciparum activity with an IC50 of 0.023μM. Dihydrousambarashanine also has antibacterial activity and cytotoxic activity. At a concentration of 100 micrograms, its inhibitory zone diameter (mm) against Staphylococcus aureus, Mycobacterium smegmatis and Bacillus subtilis is 6 , 19, 19. [0003] Through literature search, no relevant reports on the extraction and purification methods of dihydrousambara mountainine have been found. Summary of the invention [0004] The technical problem to be solved by the present invent...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07D519/00
CPCY02P20/54
Inventor刘东锋杨成东
OwnerNANJING ZELANG MEDICAL TECH