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Method for extracting cephalotaxine from cephalotaxus fortunei

A technology of harringtonine and harringtonine, which is applied in the field of separation of effective components of traditional Chinese medicine, can solve problems such as unsuitable for industrial production, incapable of large-scale production, lengthy synthetic route, etc., and achieve high efficiency and selectivity, strong selectivity, Simple operation effect

Inactive Publication Date: 2014-12-10
NANJING BIAOKE BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many synthetic literatures about harringtonine, such as the article "Synthesis and antitumor activity of harringtonine and oxoharringtonine derivatives" reported by Ye Xianrong. The synthetic route is lengthy and cannot be used for large-scale Production; while the literature and patents on the separation and purification of harringtonine from the harringtonine plant are few, and high-performance liquid phase preparative chromatographic separation is required, as well as toxic reagents such as chloroform and benzene, which are not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The branches and leaves of Chinese fir are crushed, passed through a 100-mesh sieve, 1 kg of coarse powder of Chinese fir is taken, 8 times of 70% ethanol solution is added, the pH value is adjusted to 3.0 with hydrochloric acid, placed in an ultrasonic-microwave extraction device, ultrasonic wave 600W (normally open) ), the microwave power is 400W, the extraction time is 90min, the extract is centrifuged, the supernatant is taken, the pH value is adjusted to 9 with sodium hydroxide, it is directly absorbed by the column of AlO3, eluted with ether, the flow rate is 10mL / min, to Concentrate the eluate until there is no alkaloid reaction in the eluate, extract three times with chloroform, dry over anhydrous sodium sulfate, concentrate under reduced pressure to obtain crude harringtonine, and recrystallize twice from absolute ethanol to obtain white crystal tertiary Taxoline 1.85g, after testing, the optical purity is 90.1%.

Embodiment 2

[0019] The branches and leaves of Chinese fir are crushed, passed through a 100-mesh sieve, 1 kg of coarse powder of Chinese fir is taken, 9 times of 80% ethanol solution is added, the pH value is adjusted to 4.0 with hydrochloric acid, placed in an ultrasonic-microwave extraction device, ultrasonic wave 600W (normally open) ), the microwave power is 450W, the extraction time is 110min, the extract is centrifuged, the supernatant is taken, the pH value is adjusted to 10 with sodium hydroxide, it is directly adsorbed by the column of aluminum oxide, and eluted with ether, the flow rate is 10mL / min, to Concentrate the eluate until there is no alkaloid reaction in the eluate, extract three times with chloroform, dry over anhydrous sodium sulfate, concentrate under reduced pressure to obtain crude harringtonine, and recrystallize twice from absolute ethanol to obtain white crystal tertiary Taxoline 1.90g, after testing, the optical purity is 93.2%.

Embodiment 3

[0021] Cedarwood branches and leaves are crushed, passed through a 100 mesh sieve, 1 kg of Cedarcus coarse powder is taken, 10 times of 75% ethanol solution is added, citric acid is adjusted to a pH value of 3.5, placed in an ultrasonic-microwave extraction device, ultrasonic wave 600W (usually On), the microwave power is 500W, the extraction time is 120min, the extract is centrifuged, the supernatant is taken, the pH value is adjusted to 11 with sodium hydroxide, and it is directly absorbed by the column of aluminum oxide, eluted with ether, and the flow rate is 10mL / min. Concentrate the eluate until there is no alkaloid reaction in the eluate, extract twice with chloroform, dry over anhydrous sodium sulfate, concentrate under reduced pressure to obtain crude harringtonine, recrystallize twice from absolute ethanol to obtain white crystals 1.86g of harringtonine, after testing, the optical purity is 92.5%.

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Abstract

The invention relates to a method for extracting cephalotaxine from cephalotaxus fortunei. The method comprises the following treatment steps of: a, pulverizing branches and leaves of cephalotaxus fortune and sieving with a 100-mesh sieve; b, carrying out ultrasonic-microwave-assisted extraction in an acidic ethanol solution; c, adjusting the pH value of the solution with an alkali and purifying and separating the solution by virtue of an aluminum trioxide column; d, extracting with chloroform for 2-3 times and carrying out reduced pressure concentration on the extract to obtain a crude product of cephalotaxine; and e, re-crystallizing the crude product of cephalotaxine with anhydrous ethanol twice to obtain a pure cephalotaxine. According to the method disclosed by the invention, the cephalotaxine is extracted by virtue of the modern extraction technology, namely, combined ultrasonic-microwave-assisted extraction method and the method has the advantages of simple process, high efficiency and low cost and the high-purity cephalotaxine is easily formed in an industrial production.

Description

technical field [0001] The invention relates to a method for extracting harringtonine from cephalotaxin, in particular to an ultrasonic-microwave extraction method for harringtonine, which belongs to the field of separation of effective components of traditional Chinese medicines. Background technique [0002] harringtonine, molecular formula C 18 h 21 NO 4 , white crystals, m.p132~133℃, widely present in the roots, stems, leaves, stems and fruits of the cloverleaf plants, accounting for 40~80% of the total alkaloids contained in the cloverleaf plants. It is the parent body of new anticancer drugs-harringtonine and homoharringtonine. Due to its unique five-membered fused ring structure, it has significant anticancer effects. The effective rate of clinical treatment of malignant tumors is 32.4% (especially chronic leukemia). [0003] At present, there are many synthetic literatures about harringtonine, such as the article "Synthesis and antitumor activity of harringtonine...

Claims

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Application Information

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IPC IPC(8): C07D491/20
CPCC07D491/20
Inventor 张金芳杨存
Owner NANJING BIAOKE BIO TECH
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