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Method for preparing novel nicotianasesterpene H having antiviral activity with supercritical fluid chromatography

A supercritical fluid, sesquiterpene technology, applied in the field of tobacco chemistry, can solve the problem that the components have not been identified yet, etc.

Active Publication Date: 2015-12-23
CHINA TOBACCO YUNNAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Tobacco is the plant with the most complex chemical composition in the world, and its secondary metabolites are very rich. After decades of research, more than 3,000 monomeric chemical substances have been identified from tobacco, and many components have not yet been identified. come out

Method used

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  • Method for preparing novel nicotianasesterpene H having antiviral activity with supercritical fluid chromatography
  • Method for preparing novel nicotianasesterpene H having antiviral activity with supercritical fluid chromatography
  • Method for preparing novel nicotianasesterpene H having antiviral activity with supercritical fluid chromatography

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Experimental program
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Embodiment 1

[0024] Tobacco samples were from Yuxi, Yunnan, and the variety was Yuxi K326. 2.0kg of tobacco samples were pulverized and extracted with 95% methanol for 5 times, each extraction was 24h, the extracts were combined, filtered, and concentrated under reduced pressure to obtain an extract, 105g. The extract was dissolved in pure methanol with a weight ratio of 2.0 times, mixed with 120g of 100-mesh crude silica gel, and 0.4kg of 160-mesh silica gel was packed into a column for silica gel column chromatography. The volume ratio was 1:0, 20:1, Chloroform-acetone gradient elution of 9:1, 8:2, 7:3, 6:4, 1:1, 1:2, monitoring by thin layer chromatography (TLC) Identical fractions were pooled to give 8 fractions where the volume The chloroform-acetone elution fraction with a ratio of 8:2 was separated by water preparative chromatography with Waters SFC80Q supercritical fluid, with carbon dioxide / methanol as the mobile phase (88 / 12%, mass ratio), Silica2-EP (10mm×150mm, 5 μm) the prepa...

Embodiment 2

[0026]Tobacco samples are from Dali, Yunnan, the variety is Yunyan 200, 3.5kg of tobacco samples are chopped, extracted with 95% ethanol for 4 times, each extraction is 48h, the extracts are combined, filtered, and concentrated under reduced pressure to obtain an extract. 250g. The extract was dissolved in pure methanol with a weight ratio of 2.0 times, mixed with 250g of 80-mesh thick silica gel, and 0.5kg of 200-mesh silica gel was packed into a column for silica gel column chromatography. The volume ratio was 1:0, 20:1, 9:1, 8:2, 7:3, 6:4, 1:1, 1:2 chloroform-acetone gradient elution, TLC monitoring and merging the same fractions to obtain 8 fractions, wherein the volume ratio is 8: The chloroform-acetone elution part of 2 was separated by preparative chromatography with Waters SFC80Q supercritical fluid, carbon dioxide / methanol was used as the mobile phase (88 / 12%, mass ratio), and the Silica2-EP (10mm×150mm, 5μm) preparative column was The stationary phase, the flow rate...

Embodiment 3

[0028] Tobacco samples are from Kunming, Yunnan, the variety is Safflower Dajinyuan, 5kg of tobacco samples are pulverized, extracted 3 times by ultrasonic with 75% acetone, each extraction is 72h, the extracts are combined, filtered, and concentrated under reduced pressure into extract. Got extract 380g. The extract was dissolved in pure methanol with a weight ratio of 1.6 times, mixed with 400g of 90-mesh thick silica gel, and 2.4kg of 180-mesh silica gel was packed into a column for silica gel column chromatography. The volume ratio was 1:0, 20:1, 9:1, 8:2, 7:3, 6:4, 1:1, 1:2 chloroform-acetone gradient elution, TLC monitoring and merging the same fractions to obtain 8 fractions, wherein the volume ratio is 8: The chloroform-acetone elution part of 2 was separated by preparative chromatography with Waters SFC80Q supercritical fluid, carbon dioxide / methanol was used as the mobile phase (88 / 12%, mass ratio), and the Silica2-EP (10mm×150mm, 5μm) preparative column was The sta...

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Abstract

The invention discloses a sesquiterpenoids compound which is of a novel structure and found in tobacco. The compound is named nicotianasesterpene H, the molecular formula of the compound is C<15>H<20>O<3>, and the structural formula can be found in the specification. The invention further discloses the application of the compound. Activity tests indicate that the compound has a good inhibiting effect on rotavirus and can serve as a lead anti-rotavirus compound for being used in research and development of anti-rotavirus medicinal preparations.

Description

technical field [0001] The invention belongs to the technical field of tobacco chemistry, in particular to a sesquiterpenoid compound firstly extracted from tobacco. Meanwhile, the present invention also relates to the preparation method of the compound and its application in anti-rotavirus. Background technique [0002] Tobacco is the plant with the most complex chemical composition in the world, and its secondary metabolites are very rich. After decades of research, more than 3,000 monomeric chemical substances have been identified from tobacco, and many components have not yet been identified. come out. [0003] Supercritical fluid chromatography is based on supercritical fluids (such as CO 2 ) As a mobile phase chromatography method, supercritical fluid has both low viscosity and high diffusion coefficient of gas, which is about 10 to 100 times that of liquid, and has high density and strong solubility similar to liquid, so supercritical fluid chromatography has both ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/83C07C45/78C07C45/79A61P31/14
CPCC07C45/78C07C45/79C07C49/83Y02P20/54
Inventor 申钦鹏刘志华陈永宽赵伟刘春波王昆淼尚善斋王晋司晓喜杨光宇缪明明
Owner CHINA TOBACCO YUNNAN IND
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