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Preparation method and application of a kind of benzolactone compound in tobacco

A technology of benzolides and compounds, applied in the fields of tobacco, application, and treatment of tobacco, etc., to achieve the effect of improving oral moisturization, simple structure, and increasing fineness

Active Publication Date: 2017-09-26
CHINA TOBACCO YUNNAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The present invention separates and obtains a benzolide compound with the function of improving the smoking quality of cigarettes from tobacco, which has not been reported so far

Method used

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  • Preparation method and application of a kind of benzolactone compound in tobacco
  • Preparation method and application of a kind of benzolactone compound in tobacco
  • Preparation method and application of a kind of benzolactone compound in tobacco

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Preparation of benzolide compound C 12 h 12 o 4 , including extracting extract, silica gel column chromatography, and high-pressure liquid chromatography separation, specifically adopting the following steps:

[0031] Step (1), extraction of extract: take tobacco leaves and pulverize them, use high-concentration methanol (w%: 90%) or high-concentration ethanol (w%: 95%) or high-concentration acetone (w%: 75%) as the extraction solvent, Extraction solvent: Tobacco (weight ratio) = 3:1, soak for 54 hours, extract 4 times, combine extracts, filter and concentrate to obtain extract.

[0032] Step (2), silica gel column chromatography: after dissolving the extract obtained in step (1) with 3 times the amount of pure methanol, pure ethanol or pure acetone, use 80-100 mesh silica gel with 2.5 times the weight of the extract Mix the sample, and at the same time, carry out silica gel column chromatography with a 250-mesh silica gel dry-packed column whose weight is 2.5 times ...

Embodiment 2

[0037] The tobacco samples were from Yuxi, Yunnan, and the variety was Yuxi K326. Sampling 2.0 kg of tobacco and pulverizing it with 95% methanol soaking and extracting for 5 times, each extraction for 24 hours, the weight ratio of extraction solvent:tobacco leaves=2:1, the extracts were combined, filtered, and concentrated under reduced pressure to obtain extractum 105g . After dissolving the extract with 2.0 times the amount of pure methanol, mix the sample with 120 g of 100 mesh thick silica gel, pack 0.6 kg of 160 mesh silica gel into a column, and perform silica gel column chromatography, using a volume ratio of 1:0, 20:1, 9:1, 8:2, 7:3, 6:4, 1:1, 1:2 chloroform-acetone gradient elution, TLC monitoring The same parts were combined and concentrated to obtain 8 parts, of which The part obtained by elution and concentration with chloroform-acetone with a volume ratio of 7:3 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 35% metha...

Embodiment 3

[0040] The tobacco sample comes from Dali, Yunnan, and the variety is Yunyan 200. The tobacco sample 3.5kg is cut into small pieces, soaked and extracted with 95% ethanol for 4 times, each extraction is 48h, the extraction solvent:tobacco leaf weight ratio=4:1, the extract Combined, filtered, and concentrated under reduced pressure to form an extract, 250 g of extract was obtained. After dissolving the extract with 2.0 times its weight of pure methanol, mix the sample with 250g of 80-mesh silica gel, pack 1kg of 200-mesh silica gel into a column, and perform silica gel column chromatography. The volume ratio is 1:0, 20 :1, 9:1, 8:27:3, 6:4, 1:1, 1:2 chloroform-acetone gradient elution, TLC monitoring The same fractions were combined and concentrated to obtain 8 fractions, of which the volume The part obtained by elution and concentration with chloroform-acetone with a ratio of 7:3 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 35% m...

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Abstract

The invention discloses a benzolactone compound shown in the formula (I) and its preparation method and use, and belongs to the technical field of tobacco chemistry. The preparation method comprises carrying out extraction on tobacco leaf as a raw material by a high concentration methanol aqueous solution, a high concentration ethanol aqueous solution or a high concentration acetone aqueous solution as an extraction solvent, merging the extract, carrying out filtration, carrying out reduced pressure condensation to obtain extract, carrying out silica gel column chromatography on the extract by a silica gel dry-packaged column, carrying out gradient elution by a chloroform-acetone mixed solvent as an eluant, carrying out TLC monitoring, merging the same parts, carrying out condensation, and by high pressure liquid chromatography, further separating and purifying the part subjected to elution based on the chloroform-acetone mixed solvent with a volume ratio of 7: 3, collection and condensation so that the benzolactone compound is obtained. A cigarette addition experiment proves that the benzolactone compound can make cigarette smell soft, improve cigarette smell fineness and improve oral cavity moistening feeling.

Description

technical field [0001] The invention belongs to the technical field of tobacco chemistry, in particular to a benzolide compound extracted from tobacco for the first time. At the same time, the invention also relates to the preparation method of the compound and its application in improving the smoking quality of cigarettes. 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. With the rapid development of my country's economy, cigarette consumers have higher and higher requirements for the inherent quality of products. Although smoking has been widely recognized as harmful to health, tobacco still has a strong appeal to thousands of consumers. In addition to nicotine In addition to the addictive properties of t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/88A24B3/12A24B15/40
CPCA24B3/12A24B15/406C07D307/88
Inventor 刘春波张天栋申钦鹏周博赵英良杨光宇张凤梅何沛司晓喜苏钟璧刘志华朱瑞芝王昆淼缪明明
Owner CHINA TOBACCO YUNNAN IND
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