CN106307604B - tobacco extract, extracting method and application - Google Patents
tobacco extract, extracting method and application Download PDFInfo
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- CN106307604B CN106307604B CN201611044807.0A CN201611044807A CN106307604B CN 106307604 B CN106307604 B CN 106307604B CN 201611044807 A CN201611044807 A CN 201611044807A CN 106307604 B CN106307604 B CN 106307604B
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
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Abstract
The invention discloses a kind of tobacco extract, extracting method and application, belongs to tobacco additive agent field.Tobacco extract is extracted to obtain by the method comprised the following steps：1) propane diols is added in tobacco material, is toasted after standing；2) crush, extraction is added in powder；3) leaching liquor crosses milipore filter, obtains permeate, and permeate is evaporated under reduced pressure, and obtains concentrate；4) concentrate molecularly distilled secondary separation, light component is collected, is produced.The extract is rich in the aroma component such as Megastigmatrienone, damascone, neophytadiene, phenmethylol, benzyl carbinol, farnesyl acetone and pyranone, Furanones, baking is fragrant when in use and tobacco sheet is aromatic strongly fragrant, hair property is good thoroughly, excitant is small, miscellaneous gas is few, satisfaction is strong, can improve the suction quality of cigarette, while can also provide a certain amount of nicotine to meet the psychological need of consumer.
Description
Technical field
The present invention relates to a kind of tobacco extract, extracting method and application are also related to, belongs to tobacco additive agent field.
Background technology
The main lobe arteries and veins of offal, i.e. tobacco leaf, accounts for the 25%~30% of tobacco leaf weight.China is tobacco leaf production big country, every year
About produce few hundred thousand tonnes of offal.Wherein, part offal is manufactured into expanded cut stem using expansion technique and is added in tobacco leaf formulation, separately
There are part offal and waste tobacco leaf (fragment, offal) to make raw material plus wood pulp etc. together, be manufactured into reconstituted tobacco.In cigarette leaf group
Releasing content of coke tar can be reduced using a certain proportion of expanded cut stem and reconstituted tobacco in formula, increases cigarette Filling power.But
Stem and reconstituted tobacco miscellaneous gas when burning and sucking are heavier, and perfume quantity is few, and strength deficiency, pleasant impression is poor, has a strong impact on the suction taste product of cigarette
Matter, therefore the adding proportion in cigarette composition is relatively low, is often used without stem in high-grade cigarette, one in low and middle-grade cigarette
As additional 5%~15% stem, and ratio of the reconstituted tobacco in Ye Zuzhong is usually no more than 10%.To improve stem and reconstruction
The aesthetic quality of tobacco leaf suction, increases its application percentage in cigarette composition, cigarette enterprise is mainly by applying essence at present
The method lifting stem of spices and the perfume quantity of reconstituted tobacco, cover miscellaneous gas, improve mouthfeel.Wherein tobacco extract is as tobacco
A kind of natural perfume material of origin, tobacco this perfume, increase satisfaction can be lifted, it is more preferable with the harmony of cigarette.
Meanwhile as the propulsion of reducing tar and reducing harm engineering, the research and development of low-coke tar cigarette product become to become more and more important.It is but same with this
When also inevitably there is the phenomenon of cigarette flavor and jealous decline, and perfuming cigarette is a kind of important side for improving flavor and taste
Method.Filter tip perfuming can avoid escaping and being pyrolyzed for spices in cigarette storing process, reduce pipe tobacco and filter tip etc. and spices is cut
Stay, increase transfer efficiency, thus filter tip perfuming has turned into a kind of novel perfuming mode and has been used widely.Publication No.
CN104323423A, CN104256892A and CN104256893A patent of invention are respectively by Pu ' er Tea Polysaccharide, green puerh tea essential
Oil and Pu'er theanine are added in cigarette filter rod, for lifting cigarette flavor, reduce excitant, while filter in main flume
Harmful components.Separately there is patent that Red wine extract is added in cigarette filter, to improve the sour-sweet sense of flue gas.And tobacco carries
Taking thing is extracted from tobacco, contains tobacco origin flavor matter, compared with other natural perfume materials, tobacco extract and volume
The hamony of cigarette is more preferable, can lift cigarette perfume.Tobacco extract, which is added in filter tip, can make small molecule flavor matter prototype
Transfer, perfume loss is reduced, keep the distinctive flavor and taste of tobacco to greatest extent.
Tobacco extract is prepared frequently with solvent extraction, subcritical abstraction method and ultrasonic assistant extraction method etc..At present,
Commercially available tobacco extract is prepared using ethanol sequential extractions mostly, and this method has two big shortcomings：1. in extraction process
Part natural scents loss, product fragrance are weaker；2. in product in addition to fragrance component, also pectin, protein, hemicellulose class
Material, these materials can crack during cigarette is burnt and sucked produces some harmful components, while increases the excitant of suction and miscellaneous
Gas, influenceing organoleptic quality, (Song Peng microbial fermentations reduce harmful constituents in cigarette flue gas and improve research [D] of cigarette quality
Xi'an:Northwest University, 2008.；Chi Jingji, wait correlation analysis [J] between tobacco leaf primary chemical indexs and its judging parameter
Yanbian University's agricultural journal, 2006,28 (3):208-210.).Also some researchs are improving satisfaction, increase cigarette perfume, improving
Carry out in terms of mouthfeel, as publication No. CN105754722A patent of invention is isolated and purified using extraction-molecular clock GC-MS
Tobacco material, obtain high satisfaction cigarette perfume thing and be applied in reconstituted tobacco, specifically from enzymolysis or fermenting tobacco leaf, add
Entering 10%~70% ethanol to be heated to reflux once extracting, add water backflow second extraction, extract solution merges concentration, alcohol precipitation twice,
Add propane diols to carry out molecular distillation and collect light component.But second alcohol and water is big polar solvent, it is extract obtained in big pole
Property, based on difficult volatile ingredient, being heated at high temperature extraction in addition easily causes part thermal sensitivity, the loss of volatile fragrance component, even if
Molecular distillation technique separation and concentration light component subsequently is used, but the medium and small polarity flavor component of preceding wall losses is irretrievable.
Publication No. CN101570717A patent of invention digests, ultrasonic wave extraction, mistake using offal as raw material through acid condition
Filter, chromatograph post separation, tobacco extract is made in the step that is concentrated under reduced pressure.Compared with traditional extraction process, this method utilizes cellulose
Enzyme degraded portion of cellulose, reduces influence of the cellulose to cigarette taste, and using ultrasonic wave extraction, temperature is relatively low, the used time is short,
Pass through chromatographic column separation and concentration flavor component again.But Extraction solvent is done with water, the aroma component of medium and small polarity can not be fully molten
Go out, though the composition unfavorable to cigarette smoking effect such as pectin, protein, polysaccharide is extracted, and it is in acid to digest
Carried out under the conditions of property, extract the loss that can cause partially acidic and neutral aroma constituents in acid condition with water afterwards, even if
Column chromatography technology separation and concentration flavor component is used afterwards, but because extraction step early stage has resulted in medium and small polarity flavor component damage
Lose, tobacco extract or Shortcomings prepared by this method, and the complex process of column chromatography for separation, operation are relatively complicated.
In addition, publication No. CN104687241A patent of invention uses successively using stem, low-grade tobacco shred or other natural products as raw material
Basic, normal, high polar solvent extraction, extraction medicinal extract dissolve with ethanol and/or mixed with propylene glycol again, and stem can be improved by, which obtaining, burns and sucks product
The tobacco sauce of matter, wherein low polar solvent such as petroleum ether, hexamethylene or n-hexane, middle polar solvent ether, acetone, dichloromethane
Alkane or ethyl acetate, highly polar solvent methanol or acetic acid, these solvents are mostly volatile, inflammable, toxic solvent, to industrial production
The requirements such as equipment, personnel are higher, and not easy to operate and extraction cost is high.
The content of the invention
It is an object of the invention to provide a kind of tobacco extract, big point of pectin, protein, hemicellulose etc. in the extract
The content of the high boiling substances such as sub- material and long-chain fat hydrocarbon, carbohydrate is extremely low, and being added in stem or reconstituted tobacco to increase
Flue gas concentration, suction satisfaction is improved, pleasant impression and hamony are good, and the property sent out is good thoroughly for fragrance.
Meanwhile the present invention also provides one and grown tobacco extracting method, this method improves cigarette perfume using Maillard reaction, and uses
UF membrane and the dual separation method of molecular distillation, effectively remove the macromolecular substances such as pectin, protein, hemicellulose in extract
And the high boiling substance such as long-chain fat hydrocarbon, carbohydrate.
Finally, the present invention provides a kind of application of tobacco extract again.
In order to realize the above object the technical solution adopted in the present invention is：
Tobacco extract, extract to obtain by the method comprised the following steps：
1) propane diols is added in tobacco material, is stood after 0.5~1.5h of baking at 80~140 DEG C；
2) crush, extraction solvent is added in powder, 4~12h is extracted at temperature -20~40 DEG C；
3) leaching liquor is isolated, crosses milipore filter, permeate is collected and removes solvent, obtain concentrate；
4) concentrate molecularly distilled secondary separation, vapo(u)rizing temperature be room temperature to 40 DEG C, distillation pressure 0.01~
0.1mbar, light component is collected, is produced.
The dosage of propane diols is the 5%~20% of tobacco material quality in step 1).
It is sealing and standing to be stood in step 1), 6~12h of time of repose, so that tobacco leaf fully absorbs propane diols.
Extraction solvent is concentration 95% (V/V, similarly hereinafter) above ethanol in step 2).The mass ratio of powder and extraction solvent is
1:6~10.
50~200nm of aperture microfiltration membranes can be first crossed before leaching liquor crosses milipore filter in step 3).
The aperture of milipore filter is 5~10kD of molecular cut off in step 3).
Solvent is removed in step 3) can use distillation under vacuum.
The extracting method of tobacco extract, comprises the following steps：
1) propane diols is added in tobacco material, is stood after 0.5~1.5h of baking at 80~140 DEG C；
2) crush, extraction solvent is added in powder, 4~12h is extracted at temperature -20~40 DEG C；
3) leaching liquor is isolated, passes sequentially through microfiltration membranes and milipore filter, permeate is collected and removes solvent, concentrated
Thing；
4) concentrate molecularly distilled secondary separation, vapo(u)rizing temperature be room temperature to 40 DEG C, distillation pressure 0.01~
0.1mbar, light component cut is collected, is produced.
The dosage of propane diols is the 5%~20% of tobacco material quality in step 1).
It is sealing and standing to be stood in step 1), 6~12h of time of repose.
Extraction solvent is the ethanol of concentration more than 95% in step 2).The mass ratio of powder and extraction solvent is 1:6~10.
The aperture of microfiltration membranes is 50~200nm in step 3), and the aperture of milipore filter is 5~10kD of molecular cut off.
Solvent is removed in step 3) can use distillation under vacuum.
Application of the tobacco extract in stem, reconstituted tobacco or cigarette filter rod.
Specifically, addition of the tobacco extract in stem or reconstituted tobacco is 0.002wt%~0.01wt%.Tobacco
Application of the extract in filter stick, including：Using the ethanol of concentration more than 95% as solvent, tobacco extract is diluted to mass concentration
1%~5%, it is added to according still further to 5wt%~20wt% ratio in triacetyl glycerine, filter stick is made according to common process；
Or using the ethanol of concentration more than 95% as solvent, tobacco extract is diluted to mass concentration 20%~40%, after dilution
Solution dip-coating filter stick center line, dry, perfuming line filter stick is made according to common process；Or using the ethanol of concentration more than 95% as
Solvent, tobacco extract is diluted to mass concentration 20%~40%, with the solution coating filter stick formation paper after dilution, after drying
Minor diameter filter stick is made according to common process, the concentric circles composite filter of stock size is rolled into centered on the filter stick.
The tobacco extract can be used alone also essence can be deployed into other spices after use.
Beneficial effects of the present invention：
Tobacco extract is rich in Megastigmatrienone, damascone, neophytadiene, phenmethylol, benzyl carbinol, method in the present invention
The aroma component such as Thessaloniki acetone and pyranone, Furanones, and the macromolecular substances such as pectin, protein, hemicellulose and sugar
The content of the higher boiling volatile-resistant substances such as class, long-chain fat hydrocarbon derivative is extremely low, is added to energy in stem or reconstituted tobacco
Enough enrichment flue gases, cover miscellaneous gas, improve strength, increase stem and/or reconstituted tobacco and mix rate in tobacco leaf formulation, reduce volume
Tar content.For cigarette filter rod perfuming, baking is fragrant during suction and tobacco sheet is aromatic strongly fragrant, and hair property is good thoroughly, and excitant is small, miscellaneous gas
Few, satisfaction is strong, can improve the suction quality of cigarette, while can also provide a certain amount of nicotine to meet the physiology need of consumer
Ask.
The present invention is pre-processed using baking process to tobacco material, can promote the reduced sugar of tobacco itself with it is nitrogenous
Maillard reactions occur for compound, produce the materials such as pyranone, furanone, raising baking is fragrant, and reduces content of reducing sugar.
Propane diols is added in tobacco leaf can avoid baking temperature is too high from causing tobacco leaf to be charred to bring bad breath.Simultaneously using UF membrane-
The dual separating technology of molecular distillation can effectively remove macromolecular substances and higher boiling volatile-resistant substance, and in separation and concentration tobacco
Aroma component.Whole extraction operation is carried out at a lower temperature, can effectively avoid low boiling in tobacco, thermal sensitivity feature
The loss of aroma component, keep this perfume of tobacco.
The preparation technology of tobacco extract is simple in the present invention, easy to operate, suitable for industrialized production and application.
Embodiment
Following embodiments are only described in further detail to the present invention, but do not form any limitation of the invention.
Embodiment 1
Tobacco extract is prepared by following steps in the present embodiment：
1) 1kg flue-cured tobacco raw materials are weighed, raw material is placed in SY-III-A type experiment machine of preparing tobacco, uniformly spray plus raw material
The propane diols of quality 5%, 12h is placed in sealing fully absorbs tobacco leaf, is then heated to 80 DEG C of baking 1.5h；
2) raw material after baking is crushed to 200 mesh, and adds the alcohol steep of concentration 95%, feed liquid mass ratio 1:10, leaching
40 DEG C of temperature raising degree, time 4h；After extraction terminates, leaching liquor is filtered out with 400 mesh filter clothes, filter residue solubilizer extracts once again；
3) merge leaching liquor twice, first cross aperture 200nm microfiltration membranes, ultrafiltration of the permeate after molecular cut off 10kD
Film, ultrafiltration permeate is collected, be evaporated under reduced pressure to without low boiling point solvent, obtain concentrate；
4) secondary separation is carried out to above-mentioned concentrate using molecularly distilled, 40 DEG C, pressure 0.05mbar of vapo(u)rizing temperature, received
Collect light component, produce.
Embodiment 2
Tobacco extract is prepared by following steps in the present embodiment：
1) 1kg flue-cured tobacco raw materials are weighed, raw material is placed in SY-III-A type experiment machine of preparing tobacco, uniformly spray plus raw material
The propane diols of quality 15%, 6h is placed in sealing fully absorbs tobacco leaf, is then heated to 120 DEG C of baking 0.5h；
2) raw material after baking is crushed to 20 mesh, and adds absolute ethyl alcohol extraction, feed liquid mass ratio 1:10, extraction temperature
20 DEG C, time 8h；After extraction terminates, leaching liquor is filtered out with 400 mesh filter clothes, filter residue solubilizer extracts once again；
3) merge leaching liquor twice, first cross aperture 50nm microfiltration membranes, ultrafiltration of the permeate after molecular cut off 5kD
Film, ultrafiltration permeate is collected, be evaporated under reduced pressure to without low boiling point solvent, obtain concentrate；
4) secondary separation is carried out to above-mentioned concentrate using molecularly distilled, distilled at room temperature, distillation pressure 0.01mbar,
Light component is collected, is produced.
Embodiment 3
Tobacco extract is prepared by following steps in the present embodiment：
1) 1kg flue-cured tobacco raw materials are weighed, raw material is placed in SY-III-A type experiment machine of preparing tobacco, uniformly spray plus raw material
The propane diols of quality 7%, 10h is placed in sealing fully absorbs tobacco leaf, is then heated to 100 DEG C of baking 1h；
2) raw material after baking is crushed to 40 mesh, and adds the alcohol steep of concentration 95%, feed liquid mass ratio 1:8, extraction
10 DEG C of temperature, time 10h；After extraction terminates, leaching liquor is filtered out with 400 mesh filter clothes, filter residue solubilizer extracts once again；
3) merge leaching liquor twice, first cross aperture 100nm microfiltration membranes, ultrafiltration of the permeate after molecular cut off 8kD
Film, ultrafiltration permeate is collected, be evaporated under reduced pressure to without low boiling point solvent, obtain concentrate；
4) secondary separation is carried out to above-mentioned concentrate using molecularly distilled, 30 DEG C, pressure 0.02mbar of vapo(u)rizing temperature, received
Collect light component, produce.
Embodiment 4
Tobacco extract is prepared by following steps in the present embodiment：
1) 1kg flue-cured tobacco raw materials are weighed, raw material is placed in SY-III-A type experiment machine of preparing tobacco, uniformly spray plus raw material
The propane diols of quality 6%, 11h is placed in sealing fully absorbs tobacco leaf, is then heated to 90 DEG C of baking 1.5h；
2) raw material after baking is crushed to 100 mesh, and adds the alcohol steep of concentration 95%, feed liquid mass ratio 1:9, extraction
- 20 DEG C of temperature, time 12h；After extraction terminates, leaching liquor is filtered out with 400 mesh filter clothes, filter residue solubilizer extracts once again, merges
Leaching liquor twice；
3) leaching liquor is separated with 5kD milipore filters, is collected permeate and is evaporated under reduced pressure untill without low boiling point solvent, obtains
To concentrate；
4) secondary separation is carried out to above-mentioned concentrate using molecularly distilled, 40 DEG C, pressure 0.1mbar of vapo(u)rizing temperature, received
Collect light component, produce.
Embodiment 5
Tobacco extract is prepared by following steps in the present embodiment：
1) flue-cured tobacco raw material is weighed, uniformly the propane diols of spray plus material quality 18%, sealing placement 9h make on flue-cured tobacco raw material
Tobacco leaf fully absorbs, and is then heated to 130 DEG C of baking 0.5h；
2) raw material after baking is crushed to 80 mesh, and adds absolute ethyl alcohol extraction, feed liquid mass ratio 1:6, extraction temperature 0
DEG C, time 10h；After extraction terminates, leaching liquor is filtered out with 400 mesh filter clothes, filter residue solubilizer extracts once again, and merging extracts twice
Liquid；
3) leaching liquor is separated with 10kD milipore filters, is collected permeate and is evaporated under reduced pressure untill without low boiling point solvent,
Obtain concentrate；
4) secondary separation is carried out to above-mentioned concentrate using molecularly distilled, distilled at room temperature, distillation pressure 0.01mbar,
Light component is collected, is produced.
Embodiment 6
Tobacco extract is prepared by following steps in the present embodiment：
1) 1kg flue-cured tobacco raw materials are weighed, raw material is placed in SY-III-A type experiment machine of preparing tobacco, uniformly spray plus raw material
The propane diols of quality 20%, 7h is placed in sealing fully absorbs tobacco leaf, is then heated to 140 DEG C of baking 0.5h；
2) raw material after baking is crushed to 80 mesh, and adds absolute ethyl alcohol extraction, feed liquid mass ratio 1:8, extraction temperature
30 DEG C, time 6h；After extraction terminates, leaching liquor is filtered out with 400 mesh filter clothes, filter residue solubilizer is extracted once again, and merging is soaked twice
Extract；
3) leaching liquor is separated with 8kD milipore filters, is collected permeate and is evaporated under reduced pressure untill without low boiling point solvent, obtains
To concentrate；
4) secondary separation is carried out to above-mentioned concentrate using molecularly distilled, 30 DEG C, pressure 0.05mbar of vapo(u)rizing temperature, received
Collect light component, produce.
Embodiment 7
Tobacco extract is prepared by following steps in the present embodiment：
1) flue-cured tobacco raw material is weighed, uniformly the propane diols of spray plus material quality 12%, sealing placement 8h make on flue-cured tobacco raw material
Tobacco leaf fully absorbs, and is then heated to 110 DEG C of baking 1h；
2) raw material after baking is crushed to 40 mesh, and adds the alcohol steep of concentration 95%, feed liquid mass ratio 1:8, room temperature
Lower extraction 12h；After extraction terminates, leaching liquor is filtered out with 400 mesh filter clothes, filter residue solubilizer extracts once again, and merging extracts twice
Liquid；
3) leaching liquor is separated with 8kD milipore filters, is collected permeate and is evaporated under reduced pressure untill without low boiling point solvent, obtains
To concentrate；
4) secondary separation is carried out to above-mentioned concentrate using molecularly distilled, 30 DEG C, pressure 0.03mbar of vapo(u)rizing temperature, received
Collect light component, produce.
Comparative example (conventional heating extraction)
Tobacco extract is prepared by following steps in this comparative example：
1) 1kg flue-cured tobacco raw material is weighed, is extracted using solvent extraction method, solvent is the ethanol of concentration 95%, feed liquid matter
Measure ratio 1:10, heating and refluxing extraction 2h, after extraction terminates, leaching liquor is filtered out with 400 mesh filter clothes, filter residue solubilizer extracts one again
It is secondary；
2) merge leaching liquor twice, be evaporated under reduced pressure to solvent-free, obtain tobacco extract；
3) 10 times of quality, the ethanol of concentration 95% are added in tobacco extract, is fully placed in solution after dissolving quiet at -5 DEG C
20h is put, treats that insoluble matter fully separates out, takes advantage of cold suction filtration, filtrate decompression is distilled untill solvent-free, obtains pure tobacco oil.
Propane diols used, ethanol are food-grade in above-described embodiment and comparative example.
Test example
1st, perfuming effect contrasts
Test group 1：By tobacco extract prepared by embodiment 1 propane diols-alcohol mixed solvent (mass ratio 1:1) dilute
It is 1% to mass concentration, is added on reconstituted tobacco, seals, at room temperature according to the ratio uniform spray of reconstituted tobacco quality 0.8%
Place 6h；In being cut filler after reconstituted tobacco chopping by 10wt% ratio uniform incorporation Virginian-type cigarette.Control group 1：Adopt
The pure tobacco oil (see comparative example) prepared with reconstituted tobacco of the same race, addition equivalent conventional heating methods, equal proportion, which is mixed, is assigned to of the same race match somebody with somebody
In square pipe tobacco.Cigarette is made using conventional method in test group and control group.
Test group 2：The tobacco extract of the preparation of 0.05g embodiments 2 is weighed, with propane diols-alcohol mixed solvent (mass ratio
2:1) 5g is diluted to, dilution is uniformly sprayed and is added in 1kg expanded cut stems, seals, places 6h at room temperature, then by 15wt%'s
Ratio uniform is incorporated into during Virginian-type cigarette cuts filler.Control group 2：Add the swollen of 15wt% unused tobacco extracts of the same race
The Virginian-type cigarette of the same race of swollen stem cuts filler.Cigarette is made using conventional method in test group and control group.
Test group 3：1) according to tobacco extract in the ratio Example 3 of reconstituted tobacco quality 0.01%, with propane diols-
Alcohol mixed solvent (mass ratio 1:2) uniformly spray is added on reconstituted tobacco after diluting, and is sealed, and places more than 6h at room temperature；In life
In producing line, by original technique, the reconstituted tobacco after perfuming is mixed in 6wt% ratio with formula blade, moisture regain, chopping；2)
In tobacco extract in the ratio Example 3 of expanded cut stem quality 0.002%, with propane diols-alcohol mixed solvent (mass ratio
1:4) uniformly spray is added on expanded cut stem after diluting, and is sealed, and places more than 6h at room temperature；By original technique by the expansion after perfuming
During stem cuts filler by 10wt% ratio uniform incorporation by what is 1) produced.Control group 3：Add equal amount unused cigarette of the same race
The reconstituted tobacco of careless extract and the cigarette composition pipe tobacco of the same race of stem.Volume is made using conventional method in test group and control group
Cigarette.
Test group 4：The perfuming by the way of the perfuming line in filter stick；Using the ethanol of concentration 95% as solvent, embodiment 4 is made
Standby tobacco extract is configured to the solution of mass concentration 20%, the cored wire in dip-coating filter stick axle center, filter-stick forming device is used after drying
The function filter stick containing center line is made.Control group 4：The common filter stick without center line is made of identical tow, forming paper.By two
Kind of filter stick using identical tipping paper be mounted connected to respectively identical tobacco leaf formulation, identical cigarette paper roll low-coke tar cigarette on.
Test group 5：Using the ethanol of concentration 95% as solvent, tobacco extract prepared by embodiment 5 is configured to mass concentration
40% solution, the cored wire in dip-coating filter stick axle center, the function filter stick containing center line is made of filter-stick forming device after drying.Control group
5：The common filter stick without center line is made of identical tow, forming paper.Two kinds of filter sticks are hinged with respectively using identical tipping paper
Identical tobacco leaf formulation, identical cigarette paper roll cigarette on.
Test group 6：The perfuming in filter stick formation plasticizer, it is specially：Using the ethanol of concentration 95% as solvent, by embodiment 6
The tobacco extract of preparation is configured to the solution of mass concentration 5%, and the solution is added into three triacetins with 5wt% ratio
In ester, and it is sprayed onto in filter stick tow, the cigarette filter rod of perfuming is made according to common process.Control group 6：Using identical tow,
The common filter stick of not perfuming is made in forming paper.Two kinds of filter sticks are mounted connected to identical tobacco leaf formulation, phase respectively using identical tipping paper
On the cigarette rolled with cigarette paper.
Test group 7：The perfuming in the forming paper of the small filter stick in concentric circles composite filter center, it is specially：With the second of concentration 95%
Alcohol is solvent, and tobacco extract prepared by embodiment 7 is configured to the solution of mass concentration 30%, is coated on filter stick formation paper
On, routinely technique rolls into small filter stick after drying, and the filter stick of stock size is rolled into centered on small filter stick.Control group 7：Adopt
The common filter stick without the small filter stick of concentric circles is made with identical tow, common forming paper.Two kinds of filter sticks are used into identical tipping paper
Be mounted connected to respectively identical tobacco leaf formulation, identical cigarette paper roll cigarette on.
Above-mentioned each test group and each self sealss of control group cigarette, respectively at 22 ± 1 DEG C of temperature, the ring of relative humidity 60 ± 2%
48h is balanced in border, group smokes panel test by cigarette sensory evaluation, as a result see the table below 1.
The Sensory Quality of Cigarette of table 1 contrasts smoking result
As shown in Table 1, compared with control group cigarette, the perfume quantity of test group cigarette substantially increases, this perfume of tobacco and baking
Roasting perfume (or spice) is remarkably reinforced, and hamony is good, and miscellaneous gas mitigates, and is stimulated and is reduced, pleasant impression is comfortable, and satisfaction substantially increases, overall sucking quality
It is improved.
2nd, volatility, semi-volatility component analysis and contrast
Constituent analysis is carried out using the GC/MS tobacco extracts prepared to embodiment 4 and comparative example, as a result see the table below 2.
The GC/MS analysis results of table 2
As shown in Table 2, the tobacco extract that low temperature extracts in embodiment 4 causes after the dual separation of UF membrane-molecular distillation
Fragrant component content is apparently higher than the pure tobacco oil of heating extraction, and as nicotine content is higher by 31.9771 μ g/mg, Megastigmatrienone contains
Amount is that 2.8 times of comparative example, phenmethylol, benzyl carbinol, 5,6- dihydro -2H- pyran-2-ones etc. do not detect in comparative example, but real
The content applied in example 4 is higher.In addition, there is the content of the boiling point such as methyl linolenate, ethyl palmitate higher building matter in embodiment 4
Declined.Just because of phenmethylol, Megastigmatrienone, neophytadiene, 5,6- dihydro -2H- pyran-2-ones, 4- hydroxy-betas-dihydro
The presence of the flavor matters such as damascenone, geranyl acetone and its organic assembling, tobacco extract of the present invention is just set to possess high fragrance
The features such as, play a part of flavouring enrichment increase satisfaction.
3rd, content of reducing sugar measure and contrast
Use for reference professional standard YC/T 159-2002《Tobacco and the measure continuous flow method of tobacco product water-soluble sugar》, it is right
Tobacco extract carries out content of reducing sugar measure in embodiment 4~7 and comparative example, as a result see the table below 3.
Content of reducing sugar contrasts in the tobacco extract of table 3
As shown in Table 3, the content of reducing sugar (1.15%~3.32%) of tobacco extract is significantly lower than in embodiment 4~7
Comparative example (34.82%), show that content of reducing sugar can be substantially reduced by preparing tobacco extract using the inventive method, make it more
Suitable for cigarette filter rod perfuming.
Claims (5)
1. tobacco extract, it is characterised in that：Extract to obtain by the method comprised the following steps：
1）Propane diols is added in flue-cured tobacco raw material, is stood after 0.5 ~ 1.5h of baking at 80 ~ 140 DEG C；
2）Crush, extraction solvent is added in powder, 4 ~ 12h is extracted at temperature -20 ~ 20 DEG C；
3）Leaching liquor is isolated, crosses milipore filter, permeate is collected and removes solvent, obtain concentrate；
4）Concentrate molecularly distilled secondary separation, vapo(u)rizing temperature be room temperature to 40 DEG C, 0.01 ~ 0.1mbar of distillation pressure, receive
Collect light component, produce；
Step 1）The dosage of middle propane diols is the 5% ~ 20% of tobacco material quality；Step 1）Middle standing is sealing and standing, during standing
Between 6 ~ 12h so that tobacco leaf fully absorbs propane diols；Step 2）Middle extraction solvent is the ethanol of concentration more than 95%；Powder is molten with extracting
The mass ratio of agent is 1:6~10；Step 3）Middle leaching liquor can first cross 50 ~ 200nm of aperture microfiltration membranes before crossing milipore filter；Step
3）The aperture of middle milipore filter is 5 ~ 10kD of molecular cut off；Step 3）Middle removal solvent uses distillation under vacuum.
2. the extracting method of tobacco extract, it is characterised in that：Comprise the following steps：
1）Propane diols is added in tobacco material, is stood after 0.5 ~ 1.5h of baking at 80 ~ 140 DEG C；
2）Crush, extraction solvent is added in powder, 4 ~ 12h is extracted at temperature -20 ~ 20 DEG C；
3）Leaching liquor is isolated, passes sequentially through microfiltration membranes and milipore filter, permeate is collected and removes solvent, obtain concentrate；
4）Concentrate molecularly distilled secondary separation, vapo(u)rizing temperature be room temperature to 40 DEG C, 0.01 ~ 0.1mbar of distillation pressure, receive
Collect light component cut, produce；
Step 1）The dosage of middle propane diols is the 5% ~ 20% of tobacco material quality；Step 1）Middle standing is sealing and standing, during standing
Between 6 ~ 12h so that tobacco leaf fully absorbs propane diols；Step 2）Middle extraction solvent is the ethanol of concentration more than 95%；Powder is molten with extracting
The mass ratio of agent is 1:6~10；Step 3）Middle leaching liquor can first cross 50 ~ 200nm of aperture microfiltration membranes before crossing milipore filter；Step
3）The aperture of middle milipore filter is 5 ~ 10kD of molecular cut off；Step 3）Middle removal solvent uses distillation under vacuum.
3. application of the tobacco extract in stem, reconstituted tobacco or cigarette filter rod as described in the appended claim 1.
4. application according to claim 3, it is characterised in that：Addition of the tobacco extract in stem or reconstituted tobacco
For 0.002wt% ~ 0.01wt%.
5. application according to claim 3, it is characterised in that：Application of the tobacco extract in filter stick, including：With concentration
More than 95% ethanol is solvent, and tobacco extract is diluted into mass concentration 1% ~ 5%, is added according still further to 5wt% ~ 20wt% ratio
Into triacetyl glycerine, filter stick is made；Or using the ethanol of concentration more than 95% as solvent, tobacco extract is diluted to quality
Concentration 20% ~ 40%, with the solution dip-coating filter stick center line after dilution, dry, perfuming line filter stick is made；Or with concentration 95% with
Upper ethanol is solvent, and tobacco extract is diluted into mass concentration 20% ~ 40%, with the solution coating filter stick formation paper after dilution,
Minor diameter filter stick is made after drying, concentric circles composite filter is rolled centered on the filter stick.
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| CN110663993B (en) * | 2019-10-10 | 2022-04-22 | 福建中烟工业有限责任公司 | Tobacco extract and preparation method thereof |
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