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Method for preparing sotolon on basis of column chromatography separation and application to cigarettes

A technology of fenugreek lactone and column chromatography, applied in directions such as application, tobacco, and tobacco treatment, can solve problems such as complicated operation, and achieve the effects of simple operation, less time-consuming and low equipment requirements

Active Publication Date: 2018-04-24
CHINA TOBACCO GUANGXI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example Chen Yongkuan (2002) established a kind of easy synthetic method of trigonelactone with diethyl malonate as raw material, but this method is loaded down with trivial details

Method used

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  • Method for preparing sotolon on basis of column chromatography separation and application to cigarettes
  • Method for preparing sotolon on basis of column chromatography separation and application to cigarettes

Examples

Experimental program
Comparison scheme
Effect test

preparation Embodiment 1

[0028] In this example, fenugreek extract is used as the raw material, and the GC purity of the sample trigonelactone after extraction is 30.51%. Silica gel with a particle size of 200-300 mesh is used as the adsorbent, and petroleum ether: ethyl acetate = 1:0, 10: 1. 6:1, 1:1 (volume ratio) petroleum ether-ethyl acetate solution is the eluent system.

[0029] (1) Sample pretreatment, weigh 13.41g of fenugreek extract into a 500.00mL Erlenmeyer flask, add 130.00mL of deionized water, then add 130.00mL of dichloromethane as the extraction agent, shake well, take an appropriate amount in a centrifuge tube and vortex Rotate and oscillate, after centrifugation, the solution is separated into layers, the lower layer of methylene chloride is taken out and placed in an eggplant-shaped bottle, and the sample dissolved in deionized water is extracted three times to ensure complete extraction. The lower dichloromethane phases were combined, and the solvent was removed using a rotary eva...

preparation Embodiment 2

[0036] The fenugreek extract or tincture obtained in this example is a sample with a GC purity of 5.96%, using 200-300 mesh particle size silica gel as the adsorbent, and using petroleum ether: ethyl acetate = 1:0, 10:1, 6:1, 1:1 (volume ratio) petroleum ether-ethyl acetate solution is the eluent system.

[0037] (1) Sample pretreatment, weigh 14.23g of fenugreek extract into a 500.00mL conical flask, add 142.00mL of deionized water, then add 142.00mL of petroleum ether as the extraction agent, shake well, take an appropriate amount in a centrifuge tube and vortex After shaking and centrifuging, the solution was separated into layers, and the upper petroleum ether phase was taken into an eggplant-shaped bottle, and the sample dissolved in deionized water was extracted three times to ensure complete extraction. The upper petroleum ether phases were combined, and the solvent was removed by a rotary evaporator.

[0038] (2) Column packing, conventional wet column packing, the ad...

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PUM

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Abstract

The invention provides a separation preparation method of sotolon and an application to cigarettes. Fenugreek seeds taken as the raw material are subjected to baking, extraction and concentration, a fenugreek tincture or extract is obtained, an organic solvent is taken as an eluent system, and the sotolon is obtained through silica-gel column chromatography separation. GC-MS detection indicates that GC purity of the sotolon is higher than 99%. The method is simple to operate, low in equipment requirement and shorter in consumed time.

Description

technical field [0001] This patent relates to a method for separating and preparing monomeric flavors from natural flavors, in particular to a method for separating and preparing trigonelactone based on column chromatography technology and its application in cigarettes. Background technique [0002] Trigonelactone, also known as sugar lactone and 3-hydroxy-4,5-dimethyl-2(5H)furanone, mainly exists in fenugreek extract naturally, and is the key aroma component of fenugreek extract. It is also an important aroma component in sugarcane sugar residues. It has a very strong and long-lasting sugarcane molasses-like aroma with a slightly burnt fruity taste. It can be used as meat products, soups, seasonings, etc. It is a good food Flavor enhancer can also be used as cigarette flavor and fragrance. Used in cigarette flavoring, it can increase the burnt-sweet aroma of tobacco, add smoke aroma, cover up miscellaneous gas, reduce the irritation of cigarettes, and improve the taste of ...

Claims

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Application Information

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IPC IPC(8): C07D307/46A24B15/40
CPCA24B15/406C07D307/46
Inventor 刘鸿李小兰黄世杰黄善松董振山张峻松周芸潘玉灵兰柳妮周奕
Owner CHINA TOBACCO GUANGXI IND
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