A green extraction, enrichment, separation and purification method of neophytadiene in tobacco raw materials

Abstract

A method for the green extraction, enrichment, separation and purification of neophytadiene in tobacco raw materials, which is to add tobacco leaf powder into pure water, and then use a microwave solvent-free extraction process, and control the conditions of high power and low power and corresponding extraction time to extract To enrich neophytadiene, the neophytadiene-rich tobacco essential oil extracted by microwave solvent-free extraction is further separated by column chromatography, using silica gel as the stationary phase, and using a mixed solution of petroleum ether and ethyl acetate in different proportions As an eluent, neophytadiene with a content of 70% to 95% is eluted from low polarity to high polarity gradient. The method of the invention is environmentally friendly, fast and efficient, has good enrichment effect, and can further separate and purify the essential oil enriched with neophytadiene.

Description

technical field

[0001] The invention relates to the technical field of enrichment, separation and purification of neophytadiene, an important endogenous tobacco aroma substance, and the isolated neophytadiene is used as tobacco essence to enrich the original aroma of tobacco, soften smoke, and improve sweetness , Cover up miscellaneous gas, improve the quality of tobacco products. Background technique

[0002] Under the industry background of tobacco harm reduction and tar reduction, increasing cigarette flavor and maintaining fragrance has become one of the research focuses of cigarette enterprises. Tobacco endogenous aroma substances are the aroma components or precursors of tobacco itself. Adding characteristic tobacco endogenous aroma substances to shredded tobacco can enhance the flavor and concentration, improve the taste, and significantly improve the smoking quality of cigarettes. . Tobacco terpenoids are an important class of tobacco aroma components, and neophyta...

Examples

Embodiment 1

[0018] A method for green extraction, enrichment and separation and purification of neophytadiene in tobacco raw materials, the method steps are as follows:

[0019] (1) Weigh 1 kg of flue-cured tobacco leaf powder, add pure water 3 times the mass of the tobacco leaf powder to make it moist, place it for 3 hours, and then put it into the material tank of the microwave extractor, first adjust the extraction power to 700W, and extract at high power for 7 minutes, then Reduce the extraction power to 300W, extract with low power for 80min, and extract at a temperature of 90-100°C;

[0020] (2) After the extraction was stopped, the tobacco essential oil was separated from the collector of the microwave extractor, added with anhydrous sodium sulfate to dry for 2 hours, and filtered to remove the desiccant to obtain a light yellow transparent tobacco essential oil. According to GC-MS analysis, the relative content of neophytadiene in tobacco essential oil is about 40%;

[0021] (3) ...

Embodiment 2

[0023] A method for green extraction, enrichment and separation and purification of neophytadiene in tobacco raw materials, the method steps are as follows:

[0024] (1) Weigh 1 kg of oriental tobacco leaf powder, add pure water 4 times the mass of the tobacco leaf powder to make it moist, let it stand for 2 hours, and then put it into the material tank of the microwave extractor, first adjust the extraction power to 650W, and extract with high power for 10 minutes , then lower the extraction power to 400W, extract with low power for 60 minutes, and extract at a temperature of 90-105°C;

[0025] (2) After stopping the extraction, separate the tobacco essential oil from the collector of the microwave extraction apparatus, add anhydrous sodium sulfate to dry for 4 hours, and filter to remove the desiccant to obtain a light yellow transparent tobacco essential oil. According to GC-MS analysis, the relative content of neophytadiene in tobacco essential oil is about 28%;

[0026] ...

Embodiment 3

[0028] A method for green extraction, enrichment and separation and purification of neophytadiene in tobacco raw materials, the method steps are as follows:

[0029] (1) Weigh 1 kg of Burley tobacco leaf powder, add pure water 5 times the mass of the tobacco leaf powder to make it moist, let it stand for 1 hour, and then put it into the material tank of the microwave extractor, first adjust the extraction power to 800W, high-power extraction 5min, then reduce the extraction power to 450W, extract with low power for 30min, and extract at a temperature of 100-110°C;

[0030] (2) After stopping the extraction, separate the tobacco essential oil from the collector of the microwave extraction apparatus, add anhydrous sodium sulfate to dry for 12 hours, and filter to remove the desiccant to obtain a light yellow transparent tobacco essential oil. According to GC-MS analysis, the relative content of neophytadiene in tobacco essential oil is about 25%;

[0031] (3) Use silica gel as ...

technical field

[0001] The invention relates to the technical field of enrichment, separation and purification of neophytadiene, an important endogenous tobacco aroma substance, and the isolated neophytadiene is used as tobacco essence to enrich the original aroma of tobacco, soften smoke, and improve sweetness , Cover up miscellaneous gas, improve the quality of tobacco products. Background technique

[0002] Under the industry background of tobacco harm reduction and tar reduction, increasing cigarette flavor and maintaining fragrance has become one of the research focuses of cigarette enterprises. Tobacco endogenous aroma substances are the aroma components or precursors of tobacco itself. Adding characteristic tobacco endogenous aroma substances to shredded tobacco can enhance the flavor and concentration, improve the taste, and significantly improve the smoking quality of cigarettes. . Tobacco terpenoids are an important class of tobacco aroma components, and neophyta...

Examples

Embodiment 1

[0018] A method for green extraction, enrichment and separation and purification of neophytadiene in tobacco raw materials, the method steps are as follows:

[0019] (1) Weigh 1 kg of flue-cured tobacco leaf powder, add pure water 3 times the mass of the tobacco leaf powder to make it moist, place it for 3 hours, and then put it into the material tank of the microwave extractor, first adjust the extraction power to 700W, and extract at high power for 7 minutes, then Reduce the extraction power to 300W, extract with low power for 80min, and extract at a temperature of 90-100°C;

[0020] (2) After the extraction was stopped, the tobacco essential oil was separated from the collector of the microwave extractor, added with anhydrous sodium sulfate to dry for 2 hours, and filtered to remove the desiccant to obtain a light yellow transparent tobacco essential oil. According to GC-MS analysis, the relative content of neophytadiene in tobacco essential oil is about 40%;

[0021] (3) ...

Embodiment 2

[0023] A method for green extraction, enrichment and separation and purification of neophytadiene in tobacco raw materials, the method steps are as follows:

[0024] (1) Weigh 1 kg of oriental tobacco leaf powder, add pure water 4 times the mass of the tobacco leaf powder to make it moist, let it stand for 2 hours, and then put it into the material tank of the microwave extractor, first adjust the extraction power to 650W, and extract with high power for 10 minutes , then lower the extraction power to 400W, extract with low power for 60 minutes, and extract at a temperature of 90-105°C;

[0025] (2) After stopping the extraction, separate the tobacco essential oil from the collector of the microwave extraction apparatus, add anhydrous sodium sulfate to dry for 4 hours, and filter to remove the desiccant to obtain a light yellow transparent tobacco essential oil. According to GC-MS analysis, the relative content of neophytadiene in tobacco essential oil is about 28%;

[0026] ...

Embodiment 3

[0028] A method for green extraction, enrichment and separation and purification of neophytadiene in tobacco raw materials, the method steps are as follows:

[0029] (1) Weigh 1 kg of Burley tobacco leaf powder, add pure water 5 times the mass of the tobacco leaf powder to make it moist, let it stand for 1 hour, and then put it into the material tank of the microwave extractor, first adjust the extraction power to 800W, high-power extraction 5min, then reduce the extraction power to 450W, extract with low power for 30min, and extract at a temperature of 100-110°C;

[0030] (2) After stopping the extraction, separate the tobacco essential oil from the collector of the microwave extraction apparatus, add anhydrous sodium sulfate to dry for 12 hours, and filter to remove the desiccant to obtain a light yellow transparent tobacco essential oil. According to GC-MS analysis, the relative content of neophytadiene in tobacco essential oil is about 25%;

[0031] (3) Use silica gel as ...