Resin for separating and purifying tabersonine and applications thereof

A technology of other bonning and resin, which is applied in the field of extraction and separation of natural products, can solve the problems of low bonning recovery rate, large amount of resin consumption, and low bonning yield, so as to reduce the amount of solvent, increase the recovery rate, and reduce the amount of resin used Effect

Inactive Publication Date: 2014-02-05
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the patent US3758478, the extraction and separation method of Tabonin is reported, which uses organic solvent extraction, repeated acid water washing, alkalization, organic solvent extraction, recrystallization and other steps to separate and purify Tabonin. The operation process of this method is complicated. The yield is low, which is not conducive to industrial production, and toxic solvents such as benzene and chloroform are used, which will cause greater harm to production personnel
[0004] The publication number is CN101250188A, and the name

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Put the pretreated 150g D101 dry resin into the three-necked bottle, add 1000ml of dichloromethane to soak and swell for 24 hours, then add 200g of sodium chloride, 150g of zinc chloride, and 700ml of chloromethyl methyl ether respectively, at 50°C Reflux and stir under conditions for 15 hours, then wash with deionized water and methanol, and dry to obtain chloromethylated resin;

[0019] (2) Weigh 100g of chloromethylated resin into a three-necked bottle, then add 350ml of methanol to soak and swell for 12 hours. Add 72g of glycine and 75g of pyridine into 2000ml of aqueous solution, then add them into a three-necked flask, reflux and stir at 90°C for 24 hours, filter, wash, and dry to obtain a new resin modified with glycine;

[0020] (3) Take 100g of potato seeds and pulverize them, use 90% methanol solution 400ml reflux to extract five times, combine the extracts, concentrate and remove the alcohol solution; then add 250ml mass ratio to acidify with 1% hydrochlo...

Embodiment 2

[0024] (1) Add the pretreated 150g D101 dry resin into the three-necked bottle, add 800ml of dichloromethane to soak and swell for 24 hours, then add 150g of sodium chloride, 170g of zinc chloride, and 400ml of chloromethyl methyl ether respectively, at 50 Reflux and stir at ℃ for 20 hours, then wash with deionized water and methanol, and dry to obtain chloromethylated resin;

[0025] (2) Weigh 100g of chloromethylated resin into a three-necked bottle, add 350ml of methanol to soak and swell for 12 hours. Weigh 110g of valine and 70g of pyridine and add them to 1700ml of aqueous solution, then add them into a three-necked flask, reflux and stir at 90°C for 20 hours, filter, wash, and dry to obtain a novel resin modified by valine;

[0026] (3) take by weighing 100g potato seed pulverization, be 90% methanol solution 400ml reflux extraction five times with mass ratio, combine extract, concentrate and remove alcohol solution, add 250ml mass ratio and be 3% sulfuric acid solution...

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PUM

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Abstract

The invention relates to a resin for separating and purifying tabersonine and applications thereof. A novel resin can be obtained by performing chloromethylation based on a commercial resin as a starting resin, and then reacting with amino acid. The novel resin is extremely low in the capability of adsorbing the tabersonine in the acid liquor extracted from voacanga chalotiana pierre ex stapf seeds, and can selectively adsorb impurities in the extracted acid liquor; when the novel resin is used for separating and purifying tabersonine, the steps are as follows: firstly, pretreating and grinding voacanga chalotiana pierre ex stapf seeds, performing heating reflux extraction and acidification through organic solvent, purifying the acid liquor through the novel resin, enabling the target product tabersonine to be enriched remaining upper column liquor and washing liquor, alkalizing, extracting and concentrating the collecting liquor to obtain the product tabersonine. The novel resin is used for separating and purifying tabersonine, the recovery rate of the tabersonine can be improved, high-concentration alcohol washing is not required in the upper column purification process, and the production cost and the solvent usage amount can be reduced.

Description

technical field [0001] The invention relates to the technical field of extraction and separation of natural products, in particular to a resin for separation and purification and its application. Background technique [0002] Tabersonine, also known as Tabersonine (CAS NO.44289-63-4), is an important alkaloid in African potato fruit, with the molecular formula C 21 h 24 N 2 o 2 , the relative molecular mass is 336.42, and its chemical name is Aspidospermidine-3-carboxylic acid, 2,3,6,7-tetradehydro-(5α, 12β, 19α)-methylseter. Studies have shown that it has antihypertensive effect, and it is currently the main raw material for the synthesis of anticancer drug vinpocetine. [0003] In the patent US3758478, the extraction and separation method of Tabonin is reported, which uses organic solvent extraction, repeated acid water washing, alkalization, organic solvent extraction, recrystallization and other steps to separate and purify Tabonin. The operation process of this meth...

Claims

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Application Information

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IPC IPC(8): C08F8/32C08F8/24C07D471/20
Inventor 刘佳佳刘雄杨栋梁任娜王倩文
Owner CENT SOUTH UNIV
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