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Preparation method of sliver-white aglaione A

A technology for silver white milanone and silver white milanone A is applied in the field of preparation of silver white milanone A, which can solve the problems of complicated operation, low sample yield, small preparation amount, etc., and achieves high product purity and simple process. Easy to operate effect

Inactive Publication Date: 2013-12-18
NANJING TONGZE AGRI SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the complicated operation, small amount of preparation and low sample yield, it is difficult to realize industrial production

Method used

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  • Preparation method of sliver-white aglaione A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take silver white Mizilan leaves, dry them, crush them, weigh 10kg, add 8 times the amount of 90% ethanol solution, reflux and extract 3 times, the extract will shrink to no alcohol, add appropriate amount of water to dilute it, add it to D101 macroporous resin for adsorption, first use 7 times Column volume 50% ethanol solution to elute impurities, and then use 6 times column volume 80% ethanol solution to elute active ingredients, eluate to recover solvent and place precipitation, precipitate is filtered out and heated to dissolve with 95% ethanol, add appropriate amount of water to alcohol concentration 50%, add an equal volume of petroleum ether and stir thoroughly, collect the petroleum ether layer and filter with suction, collect the filter cake and dissolve the crystals with 80% ethanol solution for 3 times, dry to obtain 3g silver white mizalanone A, the content is 98.3% by HPLC detection.

Embodiment 2

[0015] Take silvery white Mizilan leaves, dry them, crush them, weigh 10kg, add 10 times the amount of 80% ethanol solution, and reflux for extraction twice. 10 times the column volume of 40% ethanol solution to elute the impurities, and then use 5 times the column volume of 90% ethanol solution to elute the active ingredient. Alcohol concentration 40%, add an equal volume of petroleum ether and stir thoroughly, collect the petroleum ether layer and filter with suction, collect the filter cake and dissolve the crystals with 90% ethanol solution for 3 times, dry to obtain 2.7g silver white mizalenone A, which is detected by HPLC. 97.2%.

Embodiment 3

[0017] Take silvery white Mizilan leaves, dry them, crush them, weigh 10kg, add 10 times the amount of 70% ethanol solution, reflux and extract twice, the extract will shrink to no alcohol, add appropriate amount of water to dilute it, then add it to HZ816 macroporous resin for adsorption, first use 7 times Column volume 60% ethanol solution to elute impurities, and then use 5 times column volume 80% ethanol solution to elute active ingredients, eluate to recover solvent and place precipitation, precipitate is filtered out and heated to dissolve with 90% ethanol, add appropriate amount of water to alcohol concentration 50%, add an equal volume of petroleum ether and stir thoroughly, collect the petroleum ether layer and suction filter, collect the filter cake and dissolve the crystals with 90% ethanol solution for 3 times, dry to obtain 3.5g silver white mizalenone A, the content is 97.8% by HPLC detection .

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Abstract

The invention discloses a preparation method of sliver-white aglaione. The preparation method comprises the following steps of drying and crushing sliver-white aglaia odorata leaves, adding 50%-99% ethanol liquor which is 5-10 times the amount of the sliver-white aglaia odorata leaves; carrying out reflux extraction for 2-3 times, concentrating extracting liquor until the liquor has no alcohol; adding into a macroporous resin for adsorption; carrying out gradient elution with the ethanol liquor, recycling a solvent from the eluant, placing for precipitating, and filtering out the precipitates for heating and dissolving by using 90%-95% ethanol; adding an appropriate amount of water until the alcohol concentration is 40%-70%; adding isopyknic petroleum ether for sufficiently stirring, collecting a petroleum ether layer for suction filtration; collecting a filter cake and dissolving and crystallizing 2-3 times using the ethanol liquor, and drying to obtain the sliver-white aglaione A. The preparation method of the sliver-white aglaione A is simple and convenient in process operation, and easily realizes industrial production.

Description

technical field [0001] The invention belongs to the field of biotechnology, in particular to a preparation method of mizalenone A silver white. Background technique [0002] Mizalenone A is a triterpenoid compound with insecticidal and cytotoxic activity, CAS No. 175673-63-9, molecular formula C30H46O4, molecular weight 470.68, and molecular structure as follows: [0003] [0004] Through literature search, the existing silver white mizalenone A preparation method is to adopt the silica gel separation method. Due to the complicated operation, small amount of preparation and low sample yield, it is difficult to realize industrial production. Contents of the invention [0005] The purpose of the present invention is to solve the deficiencies and defects of the prior art, and provide a method for preparing Mizilanone A silvery white with easy operation. [0006] In order to achieve the above object, the present invention adopts the following technical scheme: a kind of p...

Claims

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Application Information

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IPC IPC(8): C07J53/00
Inventor 杨存
Owner NANJING TONGZE AGRI SCI & TECH
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