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Clean production method for extracting tabersonine from African machilus fruits

An African potato fruit and clean production technology, applied in the direction of organic chemistry, can solve the problems of flawed purity, inability to be called a clean process, inability to reflect, etc.

Inactive Publication Date: 2020-10-23
HUNAN HUACHENG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires expensive equipment such as ultrafine grinding and ultrasonic extraction, and the steps are cumbersome. There may be a large amount of TritonX-114 residues in the product, which is not suitable for industrial production.
In addition, this method uses concentrated hydrochloric acid and water, and there will inevitably be waste water discharge, which cannot be called a real "clean process"
In addition, the detection method of this patent is not the external standard method, but the normalization method
There are still many flaws in the normalization method to test the purity. Moisture, inorganic salts, and impurity components that cannot be displayed under liquid phase conditions cannot be reflected by the normalization method.
Therefore, the product obtained in this patented method has a purity of 99%, and the actual purity still has flaws.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Reflux extraction: take 100 kg of African potato seed raw material, crush it to a particle size of 1-2 mm, put it into an extraction tank, add a mixed solvent of petroleum ether and ethyl acetate, wherein petroleum ether: ethyl acetate=18 : 1, (V / V), wherein mixed solvent contains 0.8kg castor oil betaine, heating and reflux extracts twice (extracting the consumption of mixed solvent for the first time is 1000L, and the time of reflux is 3 hours; The consumption of solvent is 900L, the time of reflux is 1.5 hours), filter, combine two extracts, obtain mixed solvent extract.

[0045] (2) Silica gel chromatography column adsorption: the mixed solvent extract was passed through a silica gel chromatography column at a flow rate of 0.5 BV / hour (the amount of silica gel used for column chromatography was 30 L, and the height-to-diameter ratio of the silica gel chromatography column was 6:1). The effluent from the silica gel chromatography column was collected and concentr...

Embodiment 2

[0049] (1) Reflux extraction: Take 100kg of African potato seed raw material, crush it to a particle size of 1-2 mm, put it into the extraction tank, add a mixed solvent containing 6# solvent oil and ethyl acetate, 6# solvent oil: acetic acid Ethyl ester=20:1 (V / V), wherein containing 0.6kg castor oil betaine in the mixed solvent, heat reflux extraction twice (the consumption of extracting mixed solvent for the first time is 1000L, and the time of reflux is 2.5 hours; The consumption of extraction mixed solvent is 800L, and the time of reflux is 2 hours), filters, and merges twice extracting solution, obtains mixed solvent extracting solution.

[0050] (2) Silica gel chromatography column adsorption: the mixed solvent extract was passed through a silica gel chromatography column at a flow rate of 0.8 BV / hour (the amount of silica gel used for column chromatography was 25 L, and the height-to-diameter ratio of the silica gel chromatography column was 8:1). The effluent from the...

Embodiment 3

[0054] (1) Reflux extraction: get 100kg of African potato seed raw material, crush it to a particle size of 1 to 2mm, put it into the extraction tank, add a mixed solvent of cyclohexane and ethyl acetate, cyclohexane:ethyl acetate= 15:1, (V / V), wherein the mixed solvent contains 1kg castor oil betaine, heated and refluxed for extraction twice (the amount of mixed solvent for the first extraction is 900L, and the time of reflux is 3 hours; the first extraction mixed The consumption of solvent is 800L, the time of reflux is 2 hours), filter, combine two extracts, obtain mixed solvent extract.

[0055] (2) Silica gel chromatography column adsorption: the mixed solvent extract was passed through the silica gel chromatography column at a flow rate of 0.6BV / hour, the amount of silica gel used for column chromatography was 28L, and the height-to-diameter ratio of the silica gel chromatography column was 7:1. The effluent from the silica gel chromatography column was collected and con...

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PUM

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Abstract

The invention provides a clean production method for extracting tabersonine from African machilus fruits. The method comprises the following steps: (1) reflux extraction: crushing an African machilusfruit raw material, putting the crushed African machilus fruit raw material into an extraction tank, adding a mixed solvent of a lipophilic organic solvent containing a hydrophobic betaine derivativeand a medium-polarity organic solvent, carrying out heating reflux, and filtering to obtain a mixed solvent extracting solution; and (2) silica gel chromatographic column adsorption: enabling the mixed solvent extracting solution to pass through a silica gel chromatographic column, collecting silica gel chromatographic column effluent, and concentrating until no solvent exists so as to obtain a brownish yellow oily matter, namely the voacanga chaenomeles speciosa volatile oil; and (3) silica gel chromatographic column elution: eluting the silica gel chromatographic column with an eluent, collecting the eluent, and concentrating the eluent under reduced pressure, cooling the concentrated solution, stirring for crystallization, carrying out suction filtration, and drying to obtain the tabersonine finished product. According to the method, inorganic acid, alkali and water are not used, no sewage or waste gas is discharged, and the tabersonine finished product is high in content, high in yield, environmentally friendly and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for separating active components of African potato fruit, in particular to a clean production method for extracting tabonin from African potato fruit. Background technique [0002] African potato fruit (Voacanga Africana), also known as African Voacanga tree, is a perennial tree of the Apocynaceae family. It is mainly distributed in Africa from Senegal to Sudan and Angola, as well as in West Africa, Congo and Tanzania. African potato fruit has a long history of medicinal use in traditional medicine in Africa. The whole plant can be used as medicine and is often used to treat diseases such as leprosy, dysentery, malaria, generalized edema, epilepsy and convulsions in children. Pharmacological activity studies have shown that African potato fruit has anti-tumor, anti-bacterial, anti-inflammatory, anti-plasmodium, anti-angiogenesis, memory-improving, sedative-hypnotic and detoxification activities, and has extremely high ...

Claims

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Application Information

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IPC IPC(8): C07D471/20
CPCC07D471/20
Inventor 李伟黄华学
Owner HUNAN HUACHENG BIOTECH
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