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Technology for extracting Germacrone from Rhododendron thymifolium Maxim leaves with freezing 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 simple equipment, high purity and low cost. Effect

Inactive Publication Date: 2015-12-30
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

[0014] (1) Grind the leaves of Rhododendron Thyme Thyme and pass through a 40-mesh sieve; weigh 100g of Rhododendron Thyme Thyme Leaf powder, and extract it by steam distillation for 6 hours to obtain 1.8mL of volatile oil;

[0015] (2) Dehydrate the volatile oil with anhydrous sodium sulfate and place it in a refrigerator at 0°C to freeze to precipitate crystals;

[0016] (3) Filter the crystals, wash the crystals with ethanol, dissolve them in ethanol and recrystallize, filter and wash to obtain 0.45 g of gemaconone.

[0017] Adopt high performance liquid chromatography analyzer to analyze its content: high performance liquid chromatography condition: chromatographic column is Kromasil-C18 post; Acetonitrile-water (80:20); Flow rate: 1.0ml min -1 ; Column temperature: room temperature (25° C.); UV detection wavelength: 210 nm; injection volume: 20 μL.

[0018] The purity of the obtained gemacerone was 96%. The yield was 0.45%.

Embodiment 2

[0020] (1) Grind the leaves of Rhododendron japonica, pass through a 40-mesh sieve; weigh 100g, extract by steam distillation for 8 hours, and obtain 2mL of volatile oil;

[0021] (2) Dehydrate the volatile oil with anhydrous sodium sulfate and place it in a refrigerator at -10°C to freeze to precipitate crystals;

[0022] (3) The crystals were filtered and washed with ethanol, then dissolved in ethanol and recrystallized, filtered and washed to obtain 0.35 g of gemmaconone.

[0023] The purity of the obtained gemmaconone was 98% and the yield was 0.35% after analysis and determination by a high-performance liquid chromatography analyzer.

Embodiment 3

[0025] (1) Grind the leaves of Rhododendron japonica, pass through a 40-mesh sieve; weigh 100g, extract by steam distillation for 5 hours, and obtain 1.7mL of volatile oil;

[0026] (2) Dehydrate the volatile oil with anhydrous sodium sulfate and place it in a refrigerator at -20°C to freeze to precipitate crystals;

[0027] (3) The crystals were filtered and washed with ethanol, then dissolved in ethanol and recrystallized, filtered and washed to obtain 0.40 g of gemmaconone.

[0028] After analysis and determination by high-performance liquid chromatography analyzer, the purity of the obtained gemmacone is 97%. The yield was 0.40%.

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Abstract

The invention provides a technology for extracting Germacrone from Rhododendron thymifolium Maxim leaves with a freezing method and belongs to the technical field of extraction and separation of effective active ingredients of plants. The technology comprises steps as follows: the Rhododendron thymifolium Maxim leaves are smashed to form powder, and volatile oil is extracted with a vapor distillation method firstly; the volatile oil is dehydrated with anhydrous sodium sulfate and placed in a low-temperature environment for freezing, crystals are separated out and filtered, the crystals are dissolved with ethyl alcohol and recrystallized after being washed with ethyl alcohol, filtering and washing are performed again, and high-purity Germacrone is obtained. A high performance liquid chromatography analyzer determines that the purity of Germacrone extracted and separated with the technology is 95%-98%, the yield can be up to 0.20%-0.50%. The technology is simple, short in process, low in power consumption and cost and high in yield and product purity and requires simple equipment; water and ethyl alcohol are taken as solvents, so that the technology is environment-friendly and clean and has little pollution; industrial production can be realized.

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 by freezing, 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 therapeutic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/647C07C45/78C07C45/81C07C45/82
CPCC07C45/78C07C45/81C07C45/82C07C49/647
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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