A kind of separation and purification method of camptothecin

A technology for separation, purification and camptothecin, applied in the direction of organic chemistry, can solve the problems of large consumption of organic solvents, low selectivity, poor economy, etc., and achieve the effect of reducing the content of impurities, reducing the number of crystallization times, and increasing the service life.

Active Publication Date: 2017-10-20
HUNAN XINLI BIOLOGICAL SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problem that the selectivity of extraction and adsorption to the target substance is low, the purity of the prepared camptothecin is not high, and the method of repeated extraction and recrystallization consumes a lot of organic solvents, which is labor-intensive, time-consuming and economical. , high industrial production costs and serious environmental pollution

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  • A kind of separation and purification method of camptothecin

Examples

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Comparison scheme
Effect test

Embodiment 1

[0034] A method for separating and purifying camptothecin, characterized in that it consists of the following steps:

[0035] 1) The camptothecin solution is passed through diatomaceous earth to remove impurities

[0036] 1.1) 500 g of commercially available camptothecin extract (containing 10% camptothecin) is cut into small pieces, placed in a 5L beaker, the ratio of solid to liquid is 1: 6 (g: mL), and 3 L of 65% ethanol was stirred and dissolved for 5 hours;

[0037] 1.2) spread diatomaceous earth evenly in the Buchner funnel, its thickness is 2cm;

[0038] 1.3) Filter the dissolved camptothecin solution with a Buchner funnel, remove solid impurities therein, etc., to obtain filtrate A for subsequent use; collect the filter residue and mix and dissolve the next batch of camptothecin extract for filtration;

[0039] 2) Membrane separator removes impurities from camptothecin solution

[0040] The filtrate A obtained in step 1) is passed through a membrane separator, and a...

Embodiment 2

[0054] A method for separating and purifying camptothecin, characterized in that it consists of the following steps:

[0055] 1) The camptothecin solution is passed through diatomaceous earth to remove impurities

[0056] 1.1) 300g of commercially available camptothecin extract (containing 10% camptothecin) is cut into small pieces, placed in a 5L beaker, the ratio of solid to liquid is 1: 10 (g: mL), and 3 L of 95% ethanol was stirred and dissolved for 5 hours;

[0057] 1.2) spread diatomaceous earth evenly in the Buchner funnel, its thickness is 2cm;

[0058] 1.3) Filter the dissolved camptothecin solution with a Buchner funnel, remove solid impurities therein, etc., to obtain filtrate A for subsequent use; collect the filter residue and mix and dissolve the next batch of camptothecin extract for filtration;

[0059] 2) Membrane separator removes impurities from camptothecin solution

[0060] The filtrate A obtained in step 1) is passed through a membrane separator, and a...

Embodiment 3

[0074] A method for separating and purifying camptothecin, characterized in that it consists of the following steps:

[0075] 1) The camptothecin solution is passed through diatomaceous earth to remove impurities

[0076] 1.1) 300g of commercially available camptothecin extract (containing 10% camptothecin) is cut into small pieces, placed in a 5L beaker, the ratio of solid to liquid is 1: 10 (g: mL), and 3 L of 90% ethanol was stirred and dissolved for 5 hours;

[0077] 1.2) spread diatomaceous earth evenly in the Buchner funnel, its thickness is 2cm;

[0078] 1.3) Filter the dissolved camptothecin solution with a Buchner funnel, remove solid impurities therein, etc., to obtain filtrate A for subsequent use; collect the filter residue and mix and dissolve the next batch of camptothecin extract for filtration;

[0079] 2) Membrane separator removes impurities from camptothecin solution

[0080] The filtrate A obtained in step 1) is passed through a membrane separator, and a...

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Abstract

The purpose of the present invention is to disclose a camptothecin separation and purification method, particularly a technology for preparing high-purity camptothecin by using diatomaceous earth filtration, membrane separation technology, macroporous adsorption resin column chromatography adsorption and chromatography column preparation integration purification. With the method of the present invention, the problems that the selectivity of extraction and adsorption on the target compound is low, the purity of the prepared camptothecin is not high, and the multiple extraction-recrystallization way has disadvantages of high organic solvent consumption, labor consuming, time consuming, poor economy, high industrial production and serious environmental pollution are solved.

Description

technical field [0001] The present invention relates to the field of extraction and purification of plant effective components, specifically a technique for preparing high-purity camptothecin by utilizing diatomite filtration, membrane separation technology, macroporous adsorption resin column chromatography absorption, and preparation of chromatographic separation column integration and purification . Background technique [0002] Camptothecin is an indole alkaloid, which is generally extracted from camptothecin, and its chemical structure is as follows, with a molecular weight of 348.34 and a molecular formula: C 2 Oh 16 N 2 o 4 ; Pale yellow needle-like crystals, flaky crystals, melting point 264-266°C, slightly hygroscopic, showing blue fluorescence under ultraviolet light. Camptothecin is the only topoisomerase (Topoisomerase) inhibitor found so far, which has broad-spectrum anti-tumor activity. The World Health Organization has taken the research on camptothecin d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D491/22
CPCC07D491/22
Inventor 周志明李龙周小华张龙王康孟小庆陈尧辉吴琼王芳蒋金霞
Owner HUNAN XINLI BIOLOGICAL SCI & TECH
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