Method for separating and purifying two fragrance precursors from tobacco

A technology for separation and purification of tobacco, applied to β-4, separation and purification of α-4, can solve the problems of high preparation cost, limited development, complicated process operation, etc., and achieve high recovery rate, high degree of automation, and simple process operation Effect

Active Publication Date: 2011-10-05
SHANGHAI TOBACCO GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the separation and purification of α-4,8,13-cembratriene-1,3-diol and β-4,8,13-cembratriene-1,3-diol are difficult, involving leaching, extraction, The combination of multiple technologies such as multi-step column chromatography separation and recrystallization, the process operation is complicated, and the preparation cost is high. At present, there is no standard product for sale at home and abroad. Most of the pure products used in relevant scientific research are sponsored by large foreign tobacco companies, and the technology is exclusive strong, which greatly limits the development of related research in China

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  • Method for separating and purifying two fragrance precursors from tobacco
  • Method for separating and purifying two fragrance precursors from tobacco
  • Method for separating and purifying two fragrance precursors from tobacco

Examples

Experimental program
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Effect test

Embodiment 1

[0041] A method for separating and purifying α-4,8,13-cembretriene-1,3-diol and β-4,8,13-cembretriene-1,3-diol in tobacco, the process flow is as follows figure 1shown, including the following steps:

[0042] (1) Extraction: 1000 fresh tobacco leaves were collected from K326 flue-cured tobacco leaves in the tobacco leaf producing area of ​​Yuxi City, Yunnan Province. The leaves were continuously dipped in 10 L of dichloromethane for 3 times, each time for 2 s. After dipping, the solution was filtered with filter paper filled with anhydrous sodium sulfate. The filtrate was concentrated to dryness under reduced pressure (10-13 kPa) at 40° C. to obtain about 80 g of dark brown extract. Detected by GC / MS, as follows figure 2 The chromatogram of the surface secretion extract of fresh tobacco leaves shown, it can be seen from the figure that the target α-4,8,13-cembretriene-1,3-diol and β-4,8,13-cembretriene The total content of -1,3-diol was 67.6%.

[0043] (2) Liquid-liquid e...

Embodiment 2

[0049] A method for separating and purifying α-4,8,13-cembretriene-1,3-diol and β-4,8,13-cembretriene-1,3-diol in tobacco, the process flow is as follows figure 1 shown, including the following steps:

[0050] (1) Extraction: 1000 fresh tobacco leaves were collected from K326 flue-cured tobacco leaves in the tobacco leaf producing area of ​​Yuxi City, Yunnan Province. The leaves were continuously dipped in 10 L of chloroform for 3 times, each time for 2 s. After dipping, the solution was filtered with filter paper filled with anhydrous sodium sulfate. The filtrate was concentrated to dryness under reduced pressure (10-13 kPa) at 40° C. to obtain about 80 g of dark brown extract. By GC / MS detection, the total content of the target α-4,8,13-cembretriene-1,3-diol and β-4,8,13-cembretriene-1,3-diol was 67.6% .

[0051] (2) Liquid-liquid extraction: Weigh 20g of tobacco leaf surface secretion extract and place it in a 250ml conical flask, add 50ml of methanol-water (50:50) mixed...

Embodiment 3

[0056] Except in step (2), the volume ratio of n-hexane, methanol and water in the mixed extraction solvent is 100:90:10, the vacuum degree of the rotary evaporator in step (3) and step (4) is 300mbar and step (5) Except that the vacuum degree of the rotary evaporator is 60mbar, other steps are the same as in Example 1, and the obtained α-4,8,13-cembretriene-1,3-diol and β-4,8,13-cembretriene -1,3-Diol was 2.1g and 680mg, respectively, and the purity was more than 99%; The recoveries of 1,3-diol relative to tobacco leaf surface secretion extract were 10.5% and 3.4%, respectively.

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Abstract

The invention belongs to the technical field of separation and purification and relates to a technique for separating and purifying active ingredients in tobacco, in particular to a method for extracting, separating and purifying alpha-4,8,13-duvatriene-1,3-diol and beta-4,8,13-Duvatriene-1,3-diol from fresh tobacco. The separation and purification method disclosed by the method comprises: (1) leaching; (2) liquid-liquid extraction; (3) separating by normal phase silica gel column chromatography; (4) separating by normal phase cyanogen-based column chromatography; and (5) separating by antiphase C18 column chromatography to obtain two fragrance precursors. The purities of the two fragrance precursors obtained by the separation and purification method are both over 99 percent, so that the two fragrance precursors can be used as standard products in related scientific research; and the product recovery rate of the whole separation and purification process, the process operation is simple and convenient, the automation degree is high, and batch production can be realized easily.

Description

technical field [0001] The invention belongs to the technical field of separation and purification, relates to the separation and purification technology of effective components in tobacco, and in particular relates to a kind of extraction, separation and purification of α-4,8,13-ceperotriene-1,3-diol and β - A method for 4,8,13-ceretatriene-1,3-diol. Background technique [0002] α-4,8,13-Cebertotriene-1,3-diol and β-4,8,13-Cebertotriene-1,3-diol are important aroma precursors in tobacco, mainly derived from Most of the surface secretions of fresh tobacco leaves and fireworks will be degraded after modulation to produce solanone and its derivatives, which are important aroma components, which have a decisive impact on the aroma style and quality of tobacco leaves. one of the substances. On the other hand, α-4,8,13-Cebertotriene-1,3-diol and β-4,8,13-Cebertotriene-1,3-diol have strong antitumor activity, antibacterial activity It also has a certain inhibitory effect on ni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/00C07B57/00
Inventor 孙文梁高伟
Owner SHANGHAI TOBACCO GRP CO LTD
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