Process for extracting germacrone from rhododendron thymifolium leaf with silica gel method

A technology for Rhododendron rhododendron and gemmanone, which is applied in the field of extraction and separation of plant effective active components, can solve the problems of large amount of organic solvent, low yield of gemmanone, long preparation time and the like, and achieves low cost, simple preparation process and high product quality. high yield effect

Inactive Publication Date: 2016-01-13
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is complicated, the amount of organic solvent is large, the preparation time is long, the cost is high, and the yield of gemmacone is low (only 3.2g of gemmacone can be extracted from 40kg Xing’an Rhododendron leaves, and the yield is 0.008%)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Grind the leaves of Rhododendron Thyme Thyme, pass through a 40-mesh sieve, weigh 100g of Rhododendron Thyme Thyme Leaf powder, extract by steam distillation for 6 hours, and obtain 1.8mL of volatile oil;

[0016] (2) Add the volatile oil to a 40g silica gel column (160-200 mesh) after dehydration with anhydrous sodium sulfate, first elute with 500mL petroleum ether: ethyl acetate mixed solvent (180:1), and then use 1000mL petroleum ether : ethyl acetate mixed solvent (100:1) elution, petroleum ether: ethyl acetate (100:1) eluent recovery solvent;

[0017] (3) Filter the crystals, wash the crystals with petroleum ether, dissolve and recrystallize with petroleum ether, filter and wash to obtain 0.55 g of gemaconone.

[0018] Adopt high performance liquid chromatography analyzer to analyze its content: high performance liquid chromatography condition: chromatographic column is Kromasil-C18 column; Acetonitrile-water (80:20); Flow rate: 1.0mL min -1 ; Column temperatu...

Embodiment 2

[0021] (1) Grind the leaves of Rhododendron Thyme Thyme, pass through a 40-mesh sieve, weigh 100g of Rhododendron Thyme Thyme Leaf powder, extract by steam distillation for 8 hours, and obtain 2 mL of volatile oil;

[0022] (2) Dehydrate the volatile oil with anhydrous sodium sulfate and add it to a 40g silica gel column (160-200 mesh), first elute with 1000mL petroleum ether: ethyl acetate mixed solvent (150:1), and then use 500mL petroleum ether : ethyl acetate mixed solvent (100:1) elution, petroleum ether: ethyl acetate (100:1) eluent recovery solvent;

[0023] (3) Filter the crystals, wash the crystals with petroleum ether, dissolve and recrystallize with petroleum ether, filter and wash to obtain 0.60 g of gemaconone.

[0024] The content is analyzed by a high-performance liquid chromatography analyzer, and the purity of the obtained gemmaconone is 97%. The yield was 0.60%.

Embodiment 3

[0026] (1) Grind the leaves of Rhododendron Thyme Thyme, pass through a 40-mesh sieve, weigh 100g of Rhododendron Thyme Thyme Leaf powder, extract by steam distillation for 7 hours, and obtain 1.7mL of volatile oil;

[0027] (2) Dehydrate the volatile oil with anhydrous sodium sulfate and add it to a 35g silica gel column (160~200 mesh), first elute with 1000mL petroleum ether: ethyl acetate mixed solvent (150:1), then use 1000mL petroleum ether : ethyl acetate mixed solvent (80:1) eluting, petroleum ether: ethyl acetate (80:1) eluent recovery solvent;

[0028] (3) Filter the crystals, wash the crystals with petroleum ether, dissolve and recrystallize with petroleum ether, filter and wash to obtain 0.48 g of gemaconone.

[0029] The content is analyzed by a high-performance liquid chromatography analyzer, and the purity of the obtained gemmaconone is 97%. The yield was 0.48%.

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Abstract

The invention provides a method for extracting germacrone from rhododendron thymifolium leaf with a silica gel method, and relates to the technical field of plant effective active component extraction. According to the invention, rhododendron thymifolium leaf is crushed and is extracted with a steam distillation method, such that volatile oil is obtained; the volatile oil is dehydrated with anhydrous sodium sulfate, and is added into a silica gel column; elution is carried out with a mixed solvent of petroleum ether and ethyl acetate; part of the fraction is collected, crystallized and filtered; the crystals are washed with petroleum ether, and are dissolved with petroleum ether; recrystallization is carried out, and filtering and washing are carried out, such that high-purity germacrone is obtained. As a result of determination with high-performance liquid chromatography, the germacrone extracted and separated in the invention has a purity of 95-98% and a yield reaching 0.40-0.70%. The method provided by the invention has the advantage of simple process, low cost, high product yield and high product purity. The method is suitable for industrialized productions.

Description

technical field [0001] The invention relates to a method for extracting gemaconone from the leaves of Rhododendron thurium, in particular to a process for extracting gemaconone from the leaves of Rhododendron thurium through silica gel, and belongs to the technical field of extraction and separation of plant effective active ingredients. Background technique [0002] Gemma ketone is the main active ingredient in the traditional Chinese medicine Curcuma and Curcuma. Pharmacological experiments have proved that gemmacone has obvious anticancer activity. It has obvious inhibitory effect on the proliferation of human lung cancer A549 cells, and can induce apoptosis of human lung cancer A549 cells; it can also inhibit the proliferation of liver cancer Bel7402 cells in vitro; it also has anti-herpes simplex, amantadine-resistant strains, type B Activity of influenza virus strains and H3N2 subtype strains of influenza A virus (CN102274206B); gemmacone has good preventive and thera...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/607C07C45/78
CPCC07C45/78C07C49/607
Inventor 梁俊玉王文婷郑燕飞秦娟马英雄张继王俊龙孔维宝
Owner NORTHWEST NORMAL UNIVERSITY
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