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Preparation method of clerodendrin B

A technology of rhizinin and leaves, which is applied in the field of preparation of rhinbinoside B, can solve the problems that high content of rhinbinoside B has not been found, and achieve the effect of simple process, good product quality and improved separation efficiency

Inactive Publication Date: 2012-02-15
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After searching the literature, no reports on the methods for preparing large amounts of rhizin B in large quantities have been found.

Method used

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  • Preparation method of clerodendrin B

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Take 3 kg of dried kulang leaves and use 8 times the amount of water-containing acetone to reflux extract twice, extract 3 hours each time, and concentrate to obtain kulang leaves extract, add water to disperse and dissolve through the AB-8 macroporous adsorption resin column, first use water Elute until the color becomes lighter, then elute with 70% ethanol, collect the ethanol eluate, pass it through a D941 decolorization resin column, collect the injection liquid, concentrate under reduced pressure to obtain the extract, mix the extract with an appropriate amount of silica gel, and use Pack silica gel and magnesium oxide (10:1) equivalent to 6 times the amount of the extract into the column, place the mixed silica gel on the top of the column, and elute with ethyl acetate-acetone 15:1 at a flow rate of 5ml / min, TLC Monitoring, collecting the fractions containing rhizin B, concentrating the fractions until a small amount of crystals are precipitated, and placing them i...

Embodiment 2

[0022] Take 3 kg of dried kulang leaves and use 6 times the amount of water-containing acetone to reflux extract twice, extract 4 hours each time, and concentrate to obtain kulang leaves extract, add water to disperse and dissolve, pass through HPD100 macroporous adsorption resin column, and first elute with water When the color becomes lighter, elute with 95% ethanol, collect the ethanol eluate, pass it through a D941 decolorization resin column, collect the infusion solution, concentrate under reduced pressure to obtain the extract, mix the extract with an appropriate amount of silica gel, and use an equivalent Pack silica gel and magnesium oxide (10:1) 6 times the amount of the extract into the column, place the mixed sample silica gel on the top of the column, and elute with ethyl acetate-acetone 10:1, the flow rate is 5ml / min, TLC tracking monitoring, Collect the fractions containing rhinbinoside B, concentrate the fractions until a small amount of crystals are precipitate...

Embodiment 3

[0024] Take 3 kg of dried kulang leaves and use 10 times the amount of water-containing acetone to reflux extract 3 times, extract 2 hours each time, and concentrate to obtain kulang leaves extract, add water to disperse and dissolve, pass through a D101 macroporous adsorption resin column, and first elute with water When the color becomes light, then elute with 85% ethanol, collect the ethanol eluate, pass it through a D941 decolorization resin column, collect the infusion solution, concentrate under reduced pressure to obtain the extract, mix the extract with an appropriate amount of silica gel, and use an equivalent Pack silica gel and magnesium oxide (10:1) 6 times the amount of the extract into the column, place the mixed sample silica gel on the top of the column, and elute with ethyl acetate-acetone 10:1, the flow rate is 5ml / min, TLC tracking monitoring, Collect the fractions containing rhinbinoside B, concentrate the fractions until a small amount of crystals are preci...

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Abstract

The invention discloses a preparation method of clerodendrin B. The specific method comprises the following steps: extracting Seaside clerodendrum leaves with hydrous ethanol or hydrous acetone, concentrating the extract to obtain Seaside clerodendrum leaf extract; adding the Seaside clerodendrum leaf extract in a macroporous adsorption resin column, eluting with water first, then eluting with 70-95% ethanol, adding the eluent in a D941 decoloring resin column, performing lower liquid injection and upper concentration, adopting the silica gel-magnesium oxide mixed short wide column chromatography to separate and elute while using an ethyl acetate-acetone solution as the elution solution, and performing supercritical CO2 anti-solvent crystallization on eluent concentrated solution to obtain clerodendrin B monomer of which the purity is up to 98%. The separation and preparation method is simple, has low cost and high product purity, and can realize industrial application easily.

Description

technical field [0001] The invention belongs to the field of separation and preparation of effective components of traditional Chinese medicines, and relates to a preparation method of rhizin B. Background technique [0002] Clerodendrin B (Clerodendrin B) is a diterpenoid compound with the molecular formula C 31 h 44 o 12 , molecular weight 608.68, colorless prisms (hexane-ethyl acetate, 3:2), mp.228-230℃. Mainly found in Verbenaceae Kulangshu Clerodendron inerme Gaerth. Ye and Haizhou Changshan Clerodendron trichotomum (Thunb.) Nakai. Its molecular structural formula is as follows: [0003] [0004] Pharmacological studies have shown that rutinin B is an insect growth inhibitor and antifeedant, it is a feeding inhibitor for tobacco night thief larvae, and a feeding accelerator for turnip sawfly adults. According to the literature search, there is no report on the method of preparing a large amount of rutinin B with high content. Contents of the invention [0...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCY02P20/54
Inventor 刘东锋郭琴
Owner NANJING ZELANG MEDICAL TECH
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