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Method for purifying vincoside lactam

A technology of higoside and camptotheca fruit, which is applied in the field of natural plant monomer purification, can solve the problems of large consumption of eluent, incapability of continuous automatic production and the like, and achieve the effect of reducing purification cost.

Active Publication Date: 2017-03-22
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing process for purifying citrus glycosides by column chromatography is a batch process, which consumes a lot of eluent and cannot be continuously and automatically produced

Method used

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  • Method for purifying vincoside lactam
  • Method for purifying vincoside lactam
  • Method for purifying vincoside lactam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 1. Preparation of crude extract of Camptotheca acuminata

[0058] Take 100g of crushed Camptotheca fruit raw material, add 1L of ethanol, ultrasonically extract twice at 60℃, each time for 60min to obtain the extract; then concentrate the extract to 75mL, add 25mLH 2 O, stand for stratification, remove the precipitate produced by the mixed solution, take the filtrate; dilute the filtrate with water-ethanol (volume ratio 5:5) to obtain the sample solution of the crude extract of camptotheca fruit, where the concentration of camptothecin is 0.56mg / mL, its chromatographic purity is 23.79%, see figure 1 .

[0059] 2. Use SMBC to purify camptoposide from the crude extract of Camptotheca fruit

[0060] 1) SMBC separation conditions are as follows:

[0061] Chromatographic column: 6 pieces, diameter 1cm, length 20cm;

[0062] Stationary phase: octadecylsilane bonded silica gel ODS, 20~30μm;

[0063] Operating mode: 1-3-2, that is, elution zone: 1 chromatographic column; refined zone: 3 ...

Embodiment 2

[0073] Except for the following content, other conditions and steps are the same as in Example 1;

[0074] Preparing the crude extract of Camptotheca acuminata fruit extract sample solution: After crushing 100g of camptotheca acuminata fruit, use a mixed solution of ethanol and water (volume ratio 7:3) to ultrasonically extract twice at 60°C, each ultrasonic extraction for 60 minutes. The liquid ratio is 1:15 to obtain the leaching solution; after the leaching solution is concentrated and dried, 100 mL of ethanol and water (volume ratio 7:3) are added to obtain a mixed solution, the precipitation of the mixed solution is removed, and the filtrate is taken; ethanol and water (volume Ratio 5:5) Dilute the filtrate to obtain a sample injection solution of the crude extract of Camptotheca fruit, in which the concentration of camptothecin is 1.14 mg / mL.

[0075] The citrinin extract was obtained from the outlet of SMBC extract E. The chromatographic purity and yield of citrinin were 91....

Embodiment 3

[0078] Except for the following content, other conditions and steps are the same as in Example 1;

[0079] Preparation of the crude extract of Camptotheca fruit sample injection solution: After crushing 100g of camptotheca fruit, it is leached twice with a mixed solution of ethanol and water (volume ratio 7:3), each time the ultrasonic leaching is 60min, the ratio of material to liquid is 1 :15 to obtain the leaching solution; after the leaching solution is concentrated and dried, add 150 mL of ethanol and water (volume ratio 6:4) to obtain a mixed solution, remove the precipitation of the mixed solution to obtain the filtrate; use ethanol and water (volume ratio 6:4) ) Dilute the filtrate to obtain the injection solution of the crude extract of Camptotheca fruit, wherein the concentration of camptothecin is 1.0 mg / mL.

[0080] Chromatographic column: 4, diameter 2cm, length 20cm;

[0081] Stationary phase: octadecylsilane bonded silica gel ODS, 30~40μm;

[0082] Operation mode: 1-1-...

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Abstract

The invention provides a method for purifying vincoside lactam and belongs to the technical field of purification of natural plant monomers. According to the method, firstly, a common camptotheca fruit is extracted with an ethanol water solution, a common camptotheca fruit crude extract is obtained, vincoside lactam in the common camptotheca fruit crude extract is purified by the aid of three-zone simulated moving bed chromatography separation, a vincoside lactam extracting liquid is obtained and then is treated after being concentrated and crystalized, and high-purity vincoside lactam is obtained. The method can be used for purifying vincoside lactam efficiently on a large scale, stable, continuous and automatic operation is realized in the simulated moving bed chromatography separation process, a solid phase and a mobile phase can be repeatedly utilized, and the purification cost is reduced.

Description

Technical field [0001] The invention belongs to the technical field of purification of natural plant monomers, and in particular relates to a method for purifying hiftoside. Background technique [0002] Camptotheca acuminata is the fruit of a unique tree species in my country. Camptotheca acuminata has been an important medicinal material in the folk since ancient times, and it can be used as a whole plant for the treatment of malignant drugs and tumors. The main chemical components in camptothecin include: camptothecin, 10-hydroxycamptothecin, 11-methoxycamptothecin, deoxycamptothecin, camptothecin, betulinic acid and camptothecin. Studies have found that camptothecin and camptothecin compounds have anti-cancer activity. Camptothecin also has antibacterial, antiviral, anti-inflammatory, painful, and antipyretic functions. [0003] The camptoposide extracted from Camptotheca fruit has important practical value. The current method for extracting and separating camptoside is mainl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/00C07H1/08
CPCC07H1/08C07H17/00
Inventor 王绍艳姚海旭张伟石爽魏伯峰李守江
Owner UNIV OF SCI & TECH LIAONING
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