Method for separating and purifying neophytadiene in flue-cured tobacco leaves

A technology for separation and purification of neophytadiene, which is applied in the field of tobacco and can solve the problems of complex process and high production cost

Active Publication Date: 2020-06-05
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The above-mentioned methods all have the pr

Method used

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  • Method for separating and purifying neophytadiene in flue-cured tobacco leaves
  • Method for separating and purifying neophytadiene in flue-cured tobacco leaves
  • Method for separating and purifying neophytadiene in flue-cured tobacco leaves

Examples

Experimental program
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Effect test

Embodiment 1

[0043] The fresh-cured tobacco leaves were dried at 45°C for 2 hours, then crushed and sieved in sequence to obtain fresh-cured tobacco leaves with 20-60 meshes. Weigh 60g of fresh-cured tobacco leaves with a particle size of 20-60 meshes and perform supercritical CO 2 Extraction to obtain 1.035g of the initial extract of new phytadiene; of which supercritical CO 2 The extraction pressure is 20MPa, the extraction temperature is 40°C, the carbon dioxide flow rate is 15g / min, the extraction time is 1h, the separation pressure is 5MPa, and the separation temperature is 40°C;

[0044] Weigh 0.1969g of the initial extract of new phytadiene, add 8mL of sodium hydroxide solution with a concentration of 0.05mol / L to obtain an alkaline extract;

[0045] Transfer the alkaline extract to the separatory funnel, and then add 8 mL of petroleum ether, n-hexane and n-pentane in a volume ratio of 2:1:1 to obtain a stripping agent. The obtained mixed solution is heated at 3000r / After shaking at min ...

Embodiment 2

[0047] The flue-cured tobacco leaves were dried at 50°C for 1.8 hours and then pulverized and sieved in order to obtain 20-60 mesh flue-cured tobacco leaves. Weigh 60g of the flue-cured tobacco leaves with a particle size of 20-60 mesh and perform supercritical CO 2 Extraction to obtain 1.274g of the initial extract of new phytadiene; of which supercritical CO 2 The extraction pressure is 25MPa, the extraction temperature is 45°C, the carbon dioxide flow rate is 20g / min, the extraction time is 1.5h, the separation pressure is 5MPa, and the separation temperature is 40°C;

[0048] Weigh 0.1969g of the initial extract of new phytadiene, add 4mL of sodium hydroxide solution with a concentration of 0.1mol / L to obtain an alkaline extract;

[0049] Transfer the alkaline extract to the separatory funnel, and then add 8 mL of the stripping agent obtained by mixing petroleum ether and n-pentane in a volume ratio of 3:1, and the resulting mixed solution is shaken at 3000r / min. After 4 minutes...

Embodiment 3

[0051] The flue-cured tobacco leaves were dried at 55°C for 2.2 hours and then pulverized and sieved to obtain 20-60 mesh flue-cured tobacco leaves. Weigh 60g of the flue-cured tobacco leaves with a particle size of 20-60 mesh and perform supercritical CO 2 Extraction to obtain 1.326g of new phytadiene initial extract; of which supercritical CO 2 The extraction pressure is 25MPa, the extraction temperature is 50°C, the carbon dioxide flow rate is 25g / min, the extraction time is 2h, the separation pressure is 5MPa, and the separation temperature is 40°C;

[0052] Weigh 0.1969g of the initial extract of new phytadiene, add 2mL of 0.2mol / L sodium hydroxide solution to obtain an alkaline extract;

[0053] Transfer the alkaline extract to the separatory funnel, and then add 8 mL of the stripping agent obtained by mixing petroleum ether and n-hexane in a volume ratio of 3:1, and the resulting mixed solution is oscillated at 3000r / min. After 5 minutes, let stand for stratification, take th...

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Abstract

The invention belongs to the technical field of tobaccos, and particularly relates to a method for separating and purifying neophytadiene in flue-cured tobacco leaves. The method comprises the following steps: carrying out supercritical CO2 extraction on flue-cured tobacco leaves to obtain neophytadiene primary extract, mixing the neophytadiene primary extract with an alkaline solution to obtain an alkaline extracting solution, carrying out back extraction on the alkaline extracting solution to obtain an oil phase, and removing a back extraction agent in the oil phase to obtain high-purity neophytadiene, wherein the back extraction agent for back extraction is a mixture of petroleum ether and alkane or petroleum ether. The method provided by the invention is simple and easy to operate, andthe result of the embodiment shows that the yield of the neophytadiene obtained by the method provided by the invention reaches 15.74% and the purity reaches 97.99%.

Description

Technical field [0001] The invention belongs to the technical field of tobacco, and specifically relates to a method for separating and purifying new phytadiene in the flue-cured tobacco leaves. Background technique [0002] New phytadiene (7,11,15-trimethyl-3-methylidenehexadec-1-ene) molecular formula is C 20 H 38 , The relative molecular weight is 278.516, and the boiling point is 344.5°C (760mmHg). Neophytadiene is a clustered isoprene aroma substance with 20 carbon atoms, and is an important aroma substance in tobacco leaves. Studies have shown that neophytadiene is mainly derived from the degradation and transformation of chlorophyll in natural green plants, and its mass fraction in tobacco leaves is about 0.06% to 0.10%. As a carrier for capturing aroma substances in smoke aerosols, neophytadiene has the ability to carry volatile aroma substances and aroma components in tobacco leaves into the smoke. As an important flavoring agent for tobacco leaves, it can increase, enr...

Claims

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Application Information

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IPC IPC(8): C07C7/00C07C7/10C07C11/12
CPCC07C7/00C07C7/005C07C7/10C07C11/12Y02P20/54
Inventor 顾丽莉杜康张尉张花黄智华李江舟张立猛
Owner KUNMING UNIV OF SCI & TECH
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