CN102559388A - Essential oil of tobaccos as well as preparation method and application thereof to cigarettes - Google Patents
Essential oil of tobaccos as well as preparation method and application thereof to cigarettes Download PDFInfo
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- CN102559388A CN102559388A CN2012100447586A CN201210044758A CN102559388A CN 102559388 A CN102559388 A CN 102559388A CN 2012100447586 A CN2012100447586 A CN 2012100447586A CN 201210044758 A CN201210044758 A CN 201210044758A CN 102559388 A CN102559388 A CN 102559388A
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Abstract
The invention relates to the essential oil of tobaccos as well as a preparation method and application thereof to cigarettes. The essential oil of the tobaccos is prepared by the following method of: taking discarded/defective tobacco wastes, extracting by an organic solvent, taking the crude extract of the essential oil, introducing water vapor, condensing and separating oil and water so as to obtain the essential oil of the tobaccos. By adding the essential oil of the tobaccos, which is disclosed by the invention and is used as a flavoring agent, into the tobacco shreds of cigarettes, the self fragrance of the tobaccos can be increased, the quality of the fragrance of the cigarettes is enhanced, the excitation and the miscellaneous gas of the tobaccos are reduced, and smoke is softened. The essential oil of the tobaccos as well as the preparation method and the application thereof to the cigarettes have the advantages that the advantage of higher extracting yield of a solvent extracting method and the characteristic of refinement of a water-vapor distillation extracting method are combined, the yield of the essential oil of the tobaccos is obviously higher than that of a traditional water-vapor distillation method, and extracting equipment and a solvent are simple and convenient and are easy to obtain; and moreover, no solvent residue exists in a final product of the essential oil of the tobaccos, and the safety of the product is high.
Description
Technical field
The present invention relates to that natural plant essential oils extracts and Application Areas, be specifically related to grow tobacco an essential oil and preparation method thereof and the application in cigarette, particularly utilize the useless time offal of the waste that produces in the production of cigarettes process to prepare the tobacco essential oil.
Background technology
Tobacco is the herb of Solanaceae Nicotiana plant tobacco Nicotiana tabacum L., and gather autumn, dries in the shade.Tobacco all has important status as a kind of important hobby property cash crop in its agricultural in the world.World's cigarette industry has received severe day by day smoking and healthy pressure from public opinion since the 1950's, the security that improves smoking has become the common objective of tobacco industry.Through research for many years, people have concentrated on the emphasis that improves the smoking security and have reduced on the tar in the cigarette.When reducing tar content in cigarette, can also make the fragrance of cigarette still accepted just to become the main attack problem of tobacco industry so by the human consumer.One of method that solves at present just is to use an amount of sweetener, and too much cigarette might destroy the tobacco nature note of cigarette with sweetener.
Research shows that the characteristic perfume material that contains in the tobacco mainly is the micro-volatile organic matter that contains in the tobacco; Its effect substantially exceeds practical in the past various essence spice for cigarette; Therefore from tobacco, extract and have this fragrant aroma substance of tobacco to be used for perfuming cigarette be that an important channel solving a difficult problem that present low-coke tar cigarette faces is (referring to Light Engineering Institutes Of Zhengzhou's journal (natural science edition); 2005 the 20th volume the 2nd phase: 11-13, supercritical extraction technique is in the tobacco component applications in separation).
The useless time offal and the tankage thereof that in production of cigarettes, produce are one type of large sub products, and the tankage in these production processes of rational exploitation and utilization are turned waste into wealth, and can produce huge economic benefit, environmental benefit and social benefit.
Summary of the invention
The object of the invention provides a kind of tobacco essential oil and preparation method thereof and the application in perfuming cigarette.The tobacco essential oil that the present invention is extracted joins in the pipe tobacco in the actual production process, has the effect that improves cigarette pleasant impression, this perfume (or spice) of increase tobacco, raising cigarette flavor quality, the stimulation of minimizing tobacco and the gas of mixing, soft flue gas.
The object of the invention is realized by following scheme:
One grow tobacco essential oil the preparation method, comprise step:
Tobacco → organic solvent extraction → essential oil crude extract → feeding water vapor → condensation → oily water separation → tobacco essential oil.
Described tobacco can select for use the tobacco complete stool also can select tobacco leaf etc. for use, considers to select for use useless time offal from the angle that economizes on resources.
Described organic solvent is selected one or more in sherwood oil, normal hexane, ether, methylene dichloride, ETHYLE ACETATE, the absolute ethyl alcohol for use.
The method of described organic solvent extraction comprises that heating and refluxing extraction, Suo Shi are extracted, a kind of in the ultrasonic-assisted extraction.
Described tobacco essential oil can be applicable in the cigarette, need not change the original complete processing of cigarette during application, generally described tobacco essential oil is joined as sweetener to prepare cigarette in the cigarette shreds.Specifically be preferably: earlier the tobacco essential oil being dissolved in absolute ethyl alcohol or ethanol mass percentage concentration is to dilute in 90% the edible ethanol, evenly joins to be sprinkled upon with atomizing type then and adopts existing cigarette preparation method to prepare cigarette on the pipe tobacco.
The consumption of described tobacco essential oil is preferably 0.001%～0.01% of cigarette shreds weight.
Compared with prior art, the present invention has following advantage:
The present invention has combined solvent extraction process to extract productive rate advantage of higher and water vapour distillation method purified characteristics; Tobacco essential oil productive rate is significantly higher than traditional water vapor distillation method; Extraction equipment and solvent be easy, be easy to get; And no solvent residue in the final tobacco essential oil product, Product Safety is high.Can be raw material with the useless time offal that produces in the production of cigarettes process simultaneously, product be with strong points, and Chinese style cigarette and wasted resources and environment protection are significant for developing.
Smoking result shows that tobacco essential oil of the present invention perfuming in cigarette is obvious, can increase this perfume (or spice) of tobacco, raising cigarette flavor quality, the stimulation of minimizing tobacco and the gas of mixing, soft flue gas.
Embodiment
Embodiment 1:
Accurately take by weighing useless time offal sample 50g, put into the 1000mL flask, add petroleum ether solvent 400mL, 40 ℃ of water-bath refluxed are extracted 1h, and extracting solution is used 1mol/L H after filtering
2SO
4Solution washing three times, behind the anhydrous sodium sulfate drying, 40 ℃ of following underpressure distillation remove desolvates; Obtain tobacco essential oil crude extract 1.8g, then tobacco essential oil crude extract is put into the 500mL flask, add 50mL zero(ppm) water; In flask, feed water vapour 1h, oily water separation behind the water vapor condensation obtains tobacco essential oil 0.14g; Detect the products obtained therefrom no solvent residue through headspace gas chromatography.
Get the tobacco essential oil by 0.001% of cigarette shreds weight, be sprayed onto on the cigarette shreds with atomizing type with absolute ethyl alcohol dilution back, constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) is balance 48h down, rolls into Cigarette.Sensory evaluating smoking result is: this tobacco essential oil perfuming in cigarette is obvious, can increase this perfume (or spice) of tobacco, raising cigarette flavor quality, the stimulation of minimizing tobacco and the gas of mixing, soft flue gas.
Embodiment 2:
Accurately take by weighing useless time offal sample 50g, put into the 1000mL flask, add petroleum ether solvent 700mL, 40 ℃ of water-bath refluxed are extracted 3h, and extracting solution is used 1mol/L H after filtering
2SO
4Solution washing three times, behind the anhydrous sodium sulfate drying, 40 ℃ of following underpressure distillation remove desolvates; Obtain tobacco essential oil crude extract 2.1g, then tobacco essential oil crude extract is put into the 500mL flask, add 100mL zero(ppm) water; In flask, feed water vapour 3h, oily water separation behind the water vapor condensation obtains tobacco essential oil 0.15g; Detect the products obtained therefrom no solvent residue through headspace gas chromatography.
Get the tobacco essential oil by 0.01% of cigarette shreds weight; Using the ethanol mass percentage concentration is that 90% edible ethanol dilution back is sprayed onto on the cigarette shreds with atomizing type; Constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) is balance 48h down, rolls into Cigarette.Sensory evaluating smoking result is: this tobacco essential oil perfuming in cigarette is obvious, can increase this perfume (or spice) of tobacco, raising cigarette flavor quality, the stimulation of minimizing tobacco and the gas of mixing, soft flue gas.
Embodiment 3:
Accurately take by weighing offal sample 50g useless time, put into apparatus,Soxhlet's after wrapping with qualitative filter paper, add the 200mL normal hexane in the 500mL flask, connect apparatus,Soxhlet's, 70 ℃ of water-baths be extracted into solvent that condensation gets off colourless till, extracting solution is used 1mol/L H
2SO
4Solution washing three times, behind the anhydrous sodium sulfate drying, 40 ℃ of following underpressure distillation remove desolvates; Obtain tobacco essential oil crude extract 2.5g, then tobacco essential oil crude extract is put into the 500mL flask, add 50mL zero(ppm) water; In flask, feed water vapour 1h, oily water separation behind the water vapor condensation obtains tobacco essential oil 0.18g; Detect the products obtained therefrom no solvent residue through headspace gas chromatography.
Get the tobacco essential oil by 0.005% of cigarette shreds weight, be sprayed onto on the cigarette shreds with atomizing type with absolute ethyl alcohol dilution back, constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) is balance 48h down, rolls into Cigarette.Sensory evaluating smoking result is: this tobacco essential oil perfuming in cigarette is obvious, can increase this perfume (or spice) of tobacco, raising cigarette flavor quality, the stimulation of minimizing tobacco and the gas of mixing, soft flue gas.
Embodiment 4:
Accurately take by weighing offal sample 50g useless time, put into apparatus,Soxhlet's after wrapping with qualitative filter paper, add the 200mL methylene dichloride in the 500mL flask, connect apparatus,Soxhlet's, 70 ℃ of water-baths be extracted into solvent that condensation gets off colourless till, extracting solution is used 1mol/L H
2SO
4Solution washing three times, behind the anhydrous sodium sulfate drying, 40 ℃ of following underpressure distillation remove desolvates; Obtain tobacco essential oil crude extract 2.8g, then tobacco essential oil crude extract is put into the 500mL flask, add 80mL zero(ppm) water; In flask, feed water vapour 2h, oily water separation behind the water vapor condensation obtains tobacco essential oil 0.19g; Detect the products obtained therefrom no solvent residue through headspace gas chromatography.
Get the tobacco essential oil by 0.008% of cigarette shreds weight, be sprayed onto on the cigarette shreds with atomizing type with absolute ethyl alcohol dilution back, constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) is balance 48h down, rolls into Cigarette.Sensory evaluating smoking result is: this tobacco essential oil perfuming in cigarette is obvious, can increase this perfume (or spice) of tobacco, raising cigarette flavor quality, the stimulation of minimizing tobacco and the gas of mixing, soft flue gas.
Embodiment 5:
Accurately take by weighing useless time offal sample 200g, put into the 5000mL flask, add absolute ethyl alcohol 1600mL; Ultrasonic extraction 30min under 40 ℃ of water-baths, extracting solution spends the night in 4 ℃ of refrigerators behind 0.45 μ m membrane filtration; Filter back underpressure distillation under 40 ℃ of conditions and obtain tobacco essential oil crude extract 79g, then tobacco essential oil crude extract is put into the 1000mL flask except that desolvating; Add 200mL zero(ppm) water, in flask, feed water vapour 1h, oily water separation behind the water vapor condensation; Obtain tobacco essential oil 4.55g, detect the products obtained therefrom no solvent residue through headspace gas chromatography.
Get the tobacco essential oil by 0.01% of cigarette shreds weight; Using the ethanol mass percentage concentration is that 90% edible ethanol dilution back is sprayed onto on the cigarette shreds with atomizing type; Constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) is balance 48h down, rolls into Cigarette.Sensory evaluating smoking result is: this tobacco essential oil perfuming in cigarette is obvious, can increase this perfume (or spice) of tobacco, raising cigarette flavor quality, the stimulation of minimizing tobacco and the gas of mixing, soft flue gas.
Embodiment 6:
Accurately take by weighing useless time offal sample 200g, put into the 5000mL flask, add absolute ethyl alcohol 2800mL; Ultrasonic extraction 60min under 40 ℃ of water-baths, extracting solution spends the night in 4 ℃ of refrigerators behind 0.45 μ m membrane filtration; Filter back underpressure distillation under 40 ℃ of conditions and obtain tobacco essential oil crude extract 82g, then tobacco essential oil crude extract is put into the 1000mL flask except that desolvating; Add 300mL zero(ppm) water, in flask, feed water vapour 3h, oily water separation behind the water vapor condensation; Obtain tobacco essential oil 5.32g, detect the products obtained therefrom no solvent residue through headspace gas chromatography.
Get the tobacco essential oil by 0.001% of cigarette shreds weight; Using the ethanol mass percentage concentration is that 90% edible ethanol dilution back is sprayed onto on the cigarette shreds with atomizing type; Constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) is balance 48h down, rolls into Cigarette.Sensory evaluating smoking result is:
This tobacco essential oil perfuming in cigarette is obvious, can increase this perfume (or spice) of tobacco, raising cigarette flavor quality, the stimulation of minimizing tobacco and the gas of mixing, soft flue gas.
Embodiment 7:
Accurately take by weighing useless time offal sample 200g, put into the 5000mL flask, add ETHYLE ACETATE 1600mL; Ultrasonic extraction 30min under 40 ℃ of water-baths, extracting solution spends the night in 4 ℃ of refrigerators behind 0.45 μ m membrane filtration; Filter back underpressure distillation under 40 ℃ of conditions and obtain tobacco essential oil crude extract 65g, then tobacco essential oil crude extract is put into the 1000mL flask except that desolvating; Add 200mL zero(ppm) water, in flask, feed water vapour 1.5h, oily water separation behind the water vapor condensation; Obtain tobacco essential oil 4.48g, detect the products obtained therefrom no solvent residue through headspace gas chromatography.
Get the tobacco essential oil by 0.01% of cigarette shreds weight; Using the ethanol mass percentage concentration is that 90% edible ethanol dilution back is sprayed onto on the cigarette shreds with atomizing type; Constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) is balance 48h down, rolls into Cigarette.Sensory evaluating smoking result is: this tobacco essential oil perfuming in cigarette is obvious, can increase this perfume (or spice) of tobacco, raising cigarette flavor quality, the stimulation of minimizing tobacco and the gas of mixing, soft flue gas.
Embodiment 8:
Accurately take by weighing useless time offal sample 50g, put into the 1000mL flask, add ether solvent 400mL, 35 ℃ of water-bath refluxed are extracted 1h, and extracting solution is used 1mol/L H after filtering
2SO
4Solution washing three times, behind the anhydrous sodium sulfate drying, 40 ℃ of following underpressure distillation remove desolvates; Obtain tobacco essential oil crude extract 1.6g, then tobacco essential oil crude extract is put into the 500mL flask, add 50mL zero(ppm) water; In flask, feed water vapour 1h, oily water separation behind the water vapor condensation obtains tobacco essential oil 0.12g; Detect the products obtained therefrom no solvent residue through headspace gas chromatography.
Get the tobacco essential oil by 0.001% of cigarette shreds weight, be sprayed onto on the cigarette shreds with atomizing type with absolute ethyl alcohol dilution back, constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2%) is balance 48h down, rolls into Cigarette.Sensory evaluating smoking result is: this tobacco essential oil perfuming in cigarette is obvious, can increase this perfume (or spice) of tobacco, raising cigarette flavor quality, the stimulation of minimizing tobacco and the gas of mixing, soft flue gas.
Comparative Examples 1:
Accurately take by weighing useless time offal sample 50g, put into the 1000mL flask, add 50mL zero(ppm) water, in flask, feed water vapour 1h, oily water separation behind the water vapor condensation obtains tobacco essential oil 0.06g.
Claims (9)
- One grow tobacco essential oil the preparation method, comprise step:Tobacco → organic solvent extraction → essential oil crude extract → feeding water vapor → condensation → oily water separation → tobacco essential oil.
- 2. the preparation method of tobacco essential oil according to claim 1 is characterized in that, described tobacco is useless time offal.
- 3. the preparation method of tobacco essential oil according to claim 1 is characterized in that, described organic solvent is one or more in sherwood oil, normal hexane, ether, methylene dichloride, ETHYLE ACETATE, the absolute ethyl alcohol.
- 4. the preparation method of tobacco essential oil according to claim 1 is characterized in that, the method for described organic solvent extraction comprises that heating and refluxing extraction, Suo Shi are extracted, a kind of in the ultrasonic-assisted extraction.
- 5. according to the tobacco essential oil of the preparation method of each described tobacco essential oil of claim 1-4 preparation.
- 6. the application of tobacco essential oil according to claim 5 in cigarette.
- 7. the application of tobacco essential oil according to claim 6 in cigarette is characterized in that, described tobacco essential oil joined as sweetener prepare cigarette in the cigarette shreds.
- 8. the application of tobacco essential oil according to claim 7 in cigarette; It is characterized in that; Earlier the tobacco essential oil being dissolved in absolute ethyl alcohol or ethanol mass percentage concentration is to dilute in 90% the edible ethanol, evenly joins to be sprinkled upon with atomizing type then to prepare cigarette on the pipe tobacco.
- 9. according to claim 7 or 8 application of described tobacco essential oil in cigarette, it is characterized in that the consumption of described tobacco essential oil is 0.001%～0.01% of a cigarette shreds weight.
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| CN103126062A (en) * | 2013-03-04 | 2013-06-05 | 湖北中烟工业有限责任公司 | Method for extracting tobacco components |
| CN103385537A (en) * | 2013-07-31 | 2013-11-13 | 浙江中烟工业有限责任公司 | Burley tobacco and alcohol normal hexane mixed solution extract and preparation method as well as application thereof |
| CN103525553A (en) * | 2013-10-23 | 2014-01-22 | 红云红河烟草(集团)有限责任公司 | Tobacco and spice plant mixing essence and application thereof |
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| CN104498185A (en) * | 2014-12-02 | 2015-04-08 | 云南中烟工业有限责任公司 | Carambola extract as well as preparation method and application of carambola extract in cigarettes |
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| CN104774693A (en) * | 2015-03-31 | 2015-07-15 | 川渝中烟工业有限责任公司 | Tobacco flower essential oil prepared from tobacco waste and application and preparation method thereof |
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| CN105158383A (en) * | 2015-07-09 | 2015-12-16 | 郑州大学 | Method for extracting tobacco oil component through ultrasonic assisted Soxhlet extraction method |
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