CN104621709B - Flue-cured tobacco extract and electronic cigarette liquid - Google Patents
Flue-cured tobacco extract and electronic cigarette liquid Download PDFInfo
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- CN104621709B CN104621709B CN201510046427.XA CN201510046427A CN104621709B CN 104621709 B CN104621709 B CN 104621709B CN 201510046427 A CN201510046427 A CN 201510046427A CN 104621709 B CN104621709 B CN 104621709B
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- extraction
- flue
- solvent
- extract
- cured tobacco
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
-
- 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
- A24B15/26—Use of organic solvents for extraction
Abstract
The invention discloses flue-cured tobacco extract and electronic cigarette liquid. Tobacco leaves, tobacco shreds, tobacco powder and/or tobacco ash of flue-cured tobacco serve as raw materials for the flue-cured tobacco extract, and extract solvent is added into a Soxhlet extractor so that Soxhlet extraction can be conducted on the raw materials; as an improvement, a vacuum pump is connected to a condensation pipe of the Soxhlet extractor so that the vacuum degree in the Soxhlet extractor can be kept within the range of 20 mmHg to 80 mmHg; the temperature of condensate in the condensation pipe is 5 DEG C below zero or lower; after Soxhlet extraction is completed, the condensate is collected and concentrated into the flue-cured tobacco extract. A whole Soxhlet extraction system is in a negative pressure state, the boiling point of the extract solvent is reduced, the extraction temperature is reduced, the solvent circulation in the extraction process is accelerated, the extraction frequency is increased, and efficiency is higher. Meanwhile, the solvent heating temperature is lower, and therefore the extraction condition is more moderate, the excessive chemical reaction, caused by solvent high-temperature heating, between aroma components in the extract is avoided, and the extract contains less offensive odor.
Description
Technical field
The invention belongs to electronic cigarette technical field, specifically a kind of flue-cured tobacco extract and electronic cigarette liquid.
Background technology
Used as a kind of novel tobacco product, electronic cigarette liquid determines the sense organ style and features of electronic cigarette, therefore electricity to electronic cigarette
The preparation of sub- tobacco juice becomes the key of electronic cigarette product.The basic technique principle of electronic cigarette is, when electronic cigarette is sucked, electronic cigarette
Battery is powered to electronic smoke atomizer, and nebulizer is started working, and the tobacco juice being stored in electronic cigarette atomization is produced smog.Electricity
Tobacco juice in sub- cigarette, also referred to as " ree-oil ", are stored in adsorbing material, are commonly called as " adsorption cotton ".Tobacco juice in electronic cigarette, actually
One formula essence, when electronic cigarette is sucked atomization for " smog ", glycerol that smog is evaporated in including essence, Propylene Glycol etc.
The fragrance matter evaporated in material, and essence.Tobacco juice for electronic smoke is the source of electronic cigarette fragrance, decides electronic cigarette
Taste style, decides whether product is esthetically acceptable to the consumers.Therefore, the tobacco juice formula technique of electronic cigarette, is the key of electronic cigarette
One of technology.Electronic cigarette liquid mainly includes two parts, and a part is cause perfumery, and a part causes the base solvent of perfumery for dissolving,
Furthermore it is possible to add partial supplementary material, the needs of different crowd are met, wherein, the fragrance of electronic cigarette is caused mainly by causing perfumery to provide
Perfumery is the mixture of various spice, more using the extract of Nicotiana tabacum L..
The high temperature extracting method such as the Nicotiana tabacum L. extracting method of broad sense, including high-temperature retorting at present or distillation or steam distillation,
And solvent heating reflux method.In numerous Nicotiana tabacum L. extracting method, the high temperature extracting method such as dry distilling or distillation is obtaining Nicotiana tabacum L.
While aroma component, because high-temperature heating will certainly destroy the cause perfumery of Nicotiana tabacum L. itself, and high-temperature heating also brings along depth
Degree reaction, these can bring unnecessary miscellaneous QI to extract, affect the organoleptic quality evaluations of extract.Traditional solvent is carried
The method of taking be used mostly organic solvent mix with Nicotiana tabacum L. be placed in flask heat, or until boiling, to increase the molten of organic solvent
Xie Du, dissolves the spice in Nicotiana tabacum L., then filters, filtrate is concentrated to give extract.This traditional method, 1. extraction efficiency is not
Height, because certain solvent easily reaches saturation, then the aroma component that needs cannot be extracted from Nicotiana tabacum L.；2. in order to improve
Extraction efficiency can be heated up to backflow, and temperature rises to the boiling point of solvent, equally can bring unnecessary miscellaneous QI to product is extracted；
3. need to filter after extracting, the filtration after extracting especially for flue dust takes very much.
At present, electronics smoke product has one and general problem is that, electronic cigarette liquid lacks the flavor characteristics of tobacco or Nicotiana tabacum L. is fragrant
Taste feature is weak, and some in style and are sucked Medicated cigarette and there is relatively large deviation even closer to food such as chewing gum, are close on the whole
In style food.Therefore, variety classes raw tobacco material extract is explored, is enriched to improve the basic smoke of electronic cigarette, cigarette perfume
Property, fine and smooth sense and gratification it is necessary.
The content of the invention
Present invention solves the technical problem that being, electronic cigarette liquid lacks the flavor characteristics of tobacco or the flavor characteristics of tobacco is weak.
One of technical scheme is to provide a kind of flue-cured tobacco extract, with the Nicotiana tabacum L. of flue-cured tobacco, tobacco shred, offal and/or
Flue dust is raw material, and adding Extraction solvent in apparatus,Soxhlet'ses carries out surname extraction to raw material, in the condensing tube of apparatus,Soxhlet'ses
Upper connection vacuum pump, makes the vacuum in the apparatus,Soxhlet'ses maintain 20～80mmHg；Condensed fluid in the condensing tube
Temperature is less than -5 DEG C；After the completion of surname extraction, extracting solution is collected, extracting solution is concentrated to give into flue-cured tobacco extract.
Further, the Extraction solvent is ethanol, normal hexane, hexamethylene or petroleum ether.
Further, the condensing tube used in the surname extraction is serpentine condenser.
Further, the extraction time of the surname extraction is 3～8h.
Further, 14～30 times for raw material volume of the volume of the Extraction solvent.
Further, before the surname extraction, raw material is placed in into 4～8h of immersion in Extraction solvent.
Further, 0.5～1h of ultrasound or microwave extracting is carried out to the raw material after the immersion.
Another technical scheme of the present invention is to provide a kind of electronic cigarette liquid, above-mentioned flue-cured tobacco extract is dissolved in basis molten
Agent is obtained.The base solvent is the mixture of glycerol, Propylene Glycol, ethanol, the mixture of water or wherein three kinds.Wherein quality hundred
Divide being allocated as follows for ratio：The water of mass percent 0～20%, 60～70% glycerol, 0～20% ethanol, 0～20% the third two
Alcohol.
Flue-cured tobacco has special roasting perfume (or spice), and strength is big, and fragrance protectiveness can be good.The present invention is extracted to flue-cured tobacco, prepares flue-cured tobacco extraction
Thing increases the flavour of electronic cigarette as tobacco juice for electronic smoke.
The present invention is intended to provide a kind of flue-cured tobacco raw extract, according to formulary requirements take different producing area, different parts it is roasting
Cigarette Nicotiana tabacum L. is cut into tobacco shred or is ground into offal for raw material, so that ethanol, normal hexane, hexamethylene or petroleum ether etc. be nontoxic or micro- poison
Organic solvent carry out low temperature and extract repeatedly.To realize that low temperature is extracted repeatedly, to being improved on Soxhlet extraction device, in Soxhlet
The condensing tube upper end of extractor connects vacuum pump by a glass three-way valve, makes vacuum maintain 20～80mmHg so that solvent
Can seethe with excitement at a lower temperature, turn avoid the too high generation side reaction of temperature.Condensing tube chooses serpentine condenser, and can make cold
The size of solidifying pipe is lengthened, and condensing tube is passed through cold cycle condensed fluid, and condensate temperature is less than -5 DEG C, to improve condensation effect,
Prevent solvent from being taken away by vacuum pump.After decompression reduces the boiling point of solvent, solvent evaporation cooling circulation rate is accelerated, and extraction frequency adds
Hurry up, being extracted under gentleer temperature conditionss is carried out, it is to avoid in the extract that solvent high-temperature heating causes aroma component it
Between excessive chemical reaction, sensory evaluation thinks that extract miscellaneous QI under temperate condition is less, and flue gas mouthfeel is purer.
The Extraction solvent of prioritizing selection of the present invention is ethanol or normal hexane or hexamethylene or petroleum ether, for same Nicotiana tabacum L.
Raw material, the polarity size and boiling point based on solvent are different, and in the extract for finally giving, the content of each aroma component is different, such as
In the cause perfumery of the strong solvent extraction of polarity, polarity fragrance component content can increase；Equally, the cause of the weak solvent extraction of polarity is fragrant
In thing, nonpolar fragrance component content can increase.According to the extract that opposed polarity solvent extraction is obtained, according to the needs of formula,
Meet different formulary requirements.Advantage such as ethanol extraction is that alcohol solvent will not bring solvent miscellaneous QI, in sensory evaluation
It is with the obvious advantage, belong to polar solvent in addition, easily extract the polarity aroma component in Nicotiana tabacum L..And normal hexane is with respect to ethanol, pole
Property it is less, be better than ethanol to the extraction effect of nonpolar aroma component in Nicotiana tabacum L., therefore normal hexane leaf tobacco extract often strength
Greatly, gratification is strong, and inferior position is extract slightly miscellaneous QI.
The volume of Extraction solvent is 14～30 times of raw material volume, is fully dissolved out can the spice in Nicotiana tabacum L., be unlikely to again
Solvent is wasted, extraction time is 4～8h, it is ensured that spice is fully dissolved out, it is to avoid long-time heating produces miscellaneous QI.Extract
Cheng Hou, collects extracting solution, concentrating under reduced pressure, can be used as electronic cigarette liquid after base solvent dissolving.Made by this electronic cigarette liquid
Electronic cigarette can improve the flue gas mass of electronic cigarette, improve local flavor, increases gratification.
Described extraction experimental provision is optimized on the basis of Soxhlet extraction device, is improved, important improvement be
The top of surname extraction connects vacuum pump, makes entirely to extract system and is in negative pressure state, to reduce the boiling point of Extraction solvent, makes extraction
Temperature is reduced, and solvent circulation in extraction process is accelerated, and extraction frequency is accelerated, and under same time, extraction efficiency is higher.Such as with ethanol
For extractant, surname extraction under normal pressure, heating in water bath need to be set in 90 DEG C of solvents and can seethe with excitement circulating cooling, and reaching extraction will
Ask；And when reducing pressure, when negative pressure reaches -0.090Mpa (vacuum about 76mmHg), 55 DEG C of water-bath design temperature can meet will
Ask.Under negative pressure state, solvent has the risk taken away by vacuum pump, in order to ensure that solvent effectively can be cooled down and iterative cycles make
With the present invention takes two corrective measures：Condensing tube is extracted first chooses serpentine condenser the extended length by condensing tube
50%, to increase solvent condensation distance, make cooling of the condensed fluid to Extraction solvent more abundant；Secondly low temperature cold is passed through to condensing tube
But circulation fluid, the temperature of condensed fluid below -5 DEG C, between -10～-5 DEG C can substantially meet condensation and require.
In addition, raw material (Nicotiana tabacum L. or tobacco shred or offal or flue dust) is soaked 4～8h with coordinative solvent before extraction, then enter
Row is extracted, and can improve extraction effect.Furthermore, the raw material after solvent soaking is first carried out 0.5～1h of ultrasound or microwave extracting, then
Carry out extraction effect more preferable.
The present invention proposes a kind of improved Soxhlet extraction method, and significant improvement is to connect on the condensing tube of surname extraction
Vacuum pump, makes whole extraction be under negative pressure state.Under negative pressure, boiling temperature is significantly reduced, and fresh solvent circulation is accelerated,
Extraction frequency is accelerated, and extraction efficiency is higher.Simultaneously because solvent heating-up temperature is lower, extraction conditions are gentleer, it is to avoid molten
Excessive chemical reaction between aroma component in the extract that agent high-temperature heating causes, extract miscellaneous QI are less.Relatively-high temperature is extracted
Method and traditional solvent extraction process, the extract that the present invention is obtained is because obtaining under lower Extracting temperature, therefore carries
Take product and can more embody genuineness, it is to avoid it is unnecessary to occur because of the high temperature in extraction process in high temperature extraction method
Depth chemical reaction, provides the basic smoke of Nicotiana tabacum L. for electronic cigarette liquid.The advantage of Nicotiana tabacum L. extracting method of the present invention is：
(1) solvent extraction temperature is low, do not destroy the intrinsic fragrance component of Nicotiana tabacum L., it is to avoid what solvent high-temperature heating caused carries
Excessive chemical reaction between aroma component in thing is taken, the genuineness that product maintains Nicotiana tabacum L. well, extract miscellaneous QI is extracted
Less；
(2) extraction efficiency is high, and under negative pressure, boiling temperature is reduced, and fresh solvent circulation is accelerated, and extraction frequency is accelerated, extraction
Efficiency increase is taken, extracts complete.
Relative to other Nicotiana tabacum L. extractive techniques, with following technique effect, the present invention inherits surname extraction side to the present invention
The advantage of method, the fresh solvent for circulating first repeatedly constantly extract the aroma component in raw tobacco material, and extraction efficiency is high, this
Invention connects vacuum pump by the top in surname extraction, makes entirely to extract system and is in negative pressure state, reduces the boiling of Extraction solvent
Point, reduces Extracting temperature, and solvent circulation in extraction process is accelerated, and extraction frequency is accelerated, and under same time, extraction efficiency is higher.
Simultaneously because solvent heating-up temperature is lower, extraction conditions are gentleer, it is to avoid cause in the extract that solvent high-temperature heating causes
Excessive chemical reaction between fragrant composition, sensory evaluation think that the extract miscellaneous QI under temperate condition is less.
Description of the drawings
Fig. 1 is surname extraction experimental provision schematic diagram used in the present invention.
Fig. 2 is schemed for the GC-MS of 1 extract obtained composition of the embodiment of the present invention.
GC-MS comparison diagrams of the Fig. 3 for the extract obtained composition of Example 1 and Example 2 of the present invention.
Specific embodiment
With reference to specific embodiment, the invention will be further described.Following examples are intended to illustrate rather than
Limitation of the invention further.
Soxhlet extraction device used in embodiment such as Fig. 1, mainly in conventional Soxhlet extraction device top connection one
Individual vacuum pump makes surname extraction be extracted under certain negative pressure, while selecting the apparatus,Soxhlet'ses with long condensing tube to use
In extraction.
Comparative example
By 10g Zimbabwe L10F with 200mL soaked in absolute ethyl alcohol 4h, heating in water bath carries out conventional surname extraction
4h, bath temperature are set as 90 DEG C, and extracting solution is evaporated to solvent and does, and concentrate is with (5mL water+5mL dehydrated alcohol+20mL
Glycerol) dissolving.Used as the tobacco juice perfuming of electronic cigarette, evaluation result of smokeing panel test is：There is Zimbabwe's cigarette perfume feature, cigarette perfume is plentiful, alcohol
With.
Embodiment 1
By 110g Zimbabwe L10F tobacco shreds with 200mL soaked in absolute ethyl alcohol 4h, filled with improved surname extraction of the invention
Putting carries out extraction 3h, and vacuum is 40mmHg, and water bath heating temperature is 50 DEG C, and extracting solution is evaporated to solvent and does, concentrate
Dissolved with (5mL water+5mL dehydrated alcohol+20mL glycerol), as the tobacco juice perfuming of electronic cigarette, be made as test sample.With comparative example
The electronic cigarette of making carries out sensory evaluating smoking's evaluation as control, and evaluation result of smokeing panel test is：There is obvious Zimbabwe's cigarette perfume feature,
Cigarette perfume is more plentiful, alcohol and.With compare, test sample flue gas is purer.Gained flue-cured tobacco extract GC-MS figure as shown in Fig. 2
As the peak value of nicotine is too big, to clearly show other components, too high peak is not drawn completely.It is fragrant in gained electronic cigarette liquid
In the GC-MS figures of gas composition：1 is furfural；2 is 1- (3- pyridines)-ethyl ketone；3 is DDMP；4 is 5 hydroxymethyl furfural；5 is nicotine；
6 is 2,3'- bipyridyls；7 is three ketenes of huge pillar；8 is N- methoxyl groups-Methanamide；9 is pinane.As can be seen from Figure 2, the extraction of flue-cured tobacco
Thing Furanones compound and terpene compound are more, and this is the odor characteristic of flue-cured tobacco.
Embodiment 2
10g Zimbabwe L10F is soaked into 4h with 200mL normal hexane, is carried with improved Soxhlet extraction device of the invention
Take 3h, vacuum is 80mmHg, and water bath heating temperature is 45 DEG C, and extracting solution is evaporated to solvent and does, concentrate with (5mL water+
5mL dehydrated alcohol+20mL glycerol) dissolving, as the tobacco juice perfuming of electronic cigarette, tested.With the ree-oil that embodiment 1 makes it is
Compare, sensory evaluating smoking's evaluation result is：Compared with the control, test sample strength is bigger, and gratification is higher, slightly miscellaneous QI.
Fig. 3 is the GC-MS figures of fragrance component in 2 gained electronic cigarette liquid of embodiment and being superimposed for Fig. 2.From figure 3, it can be seen that second
Alcohol is polar solvent, and normal hexane is used as non-polar solven, the aroma component dense distribution that non-polar solven normal hexane extraction goes out
In the left end (remarks of the short region of retention time, i.e. GC-MS figures：GC-MS pillars are polar column).Citing, the cigarette in extract
Alkali belongs to polar substancess, and normal hexane is obviously weaker than polar solvent ethanol many to its extraction effect as can be seen from Figure 3.Fig. 3
Illustrate that aroma component that the solvent extraction of opposed polarity is obtained is differentiated, therefore the present invention proposes to select different solvents,
The electronics ree-oil that style is given priority to is obtained, to meet electronic cigarette formulary requirements.
Embodiment 3
Sangzhi B3F Zimbabwe L10F is soaked into 4h with 200mL normal hexane, is entered with improved Soxhlet extraction device of the invention
Row extracts 3h, and vacuum is 80mmHg, and water bath heating temperature is 45 DEG C, and extracting solution is evaporated to solvent and does, concentrate with
(5mL water+5mL dehydrated alcohol+20mL glycerol) dissolves, used as the tobacco juice perfuming of electronic cigarette.Make two samples, an addition city
The electronic cigarette liquid 0.5ml for selling, as control sample；Another is used as experiment sample, addition and the commercially available electronics of control sample identical
Tobacco juice 0.5ml, separately adds 0.25ml flue-cured tobaccos manufactured in the present embodiment again and extracts tobacco juice, and contrasting evaluation result of smokeing panel test is：Relative to
Control sample, tests the Nicotiana tabacum L. perfume feature of sample substantially, and strength is big, and gratification is strong.
Claims (5)
1. a kind of flue-cured tobacco extract, it is characterised in that with the Nicotiana tabacum L. of flue-cured tobacco, tobacco shred, offal and/or flue dust as raw material, in Soxhlet
Adding Extraction solvent in extractor carries out surname extraction to raw material, connects vacuum pump, make institute on the condensing tube of apparatus,Soxhlet'ses
State the vacuum in apparatus,Soxhlet'ses and maintain 20～80 mmHg, water bath heating temperature is 45-50 DEG C；It is cold in the condensing tube
The temperature of lime set is less than -5 DEG C；After the completion of surname extraction, extracting solution is collected, extracting solution is concentrated to give into flue-cured tobacco extract；Institute
Condensing tube is stated for serpentine condenser；The extraction time of the surname extraction is 3～8 h；The volume of the Extraction solvent is raw material
14～30 times of volume.
2. flue-cured tobacco extract as claimed in claim 1, it is characterised in that the Extraction solvent is ethanol, normal hexane, hexamethylene
Or petroleum ether.
3. flue-cured tobacco extract as claimed in claim 1, it is characterised in that before the surname extraction, raw material is placed in and is carried
4～8 h are soaked in taking solvent.
4. flue-cured tobacco extract as claimed in claim 3, it is characterised in that the raw material after the immersion is carried out ultrasonic or micro-
Ripple extracts 0.5～1 h.
5. a kind of electronic cigarette liquid, it is characterised in that the flue-cured tobacco extract described in one of Claims 1 to 4 is dissolved in into base solvent
Obtain.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510046427.XA CN104621709B (en) | 2015-01-29 | 2015-01-29 | Flue-cured tobacco extract and electronic cigarette liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510046427.XA CN104621709B (en) | 2015-01-29 | 2015-01-29 | Flue-cured tobacco extract and electronic cigarette liquid |
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| CN104621709A CN104621709A (en) | 2015-05-20 |
| CN104621709B true CN104621709B (en) | 2017-05-03 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105038983A (en) * | 2015-06-17 | 2015-11-11 | 云南中烟工业有限责任公司 | Glycerol triacetate extract of Zimbabwe tobacco and application thereof to cigarettes |
| CN110810581B (en) * | 2018-08-09 | 2023-10-13 | 湖南中烟工业有限责任公司 | Preparation process of tea extract |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3706594A1 (en) * | 1987-02-28 | 1988-09-08 | Messer Griesheim Gmbh | METHOD FOR THE EXTRACTION OF ORGANIC COMPONENTS FROM SOLIDS |
| US5074319A (en) * | 1990-04-19 | 1991-12-24 | R. J. Reynolds Tobacco Company | Tobacco extraction process |
| CN100415126C (en) * | 2006-07-24 | 2008-09-03 | 宋光泉 | Method for extracting tobacco essence perfume |
| CN102488318A (en) * | 2011-11-18 | 2012-06-13 | 安徽中烟工业有限责任公司 | Preparation method for aired tobacco extracts and essential oil |
| CN102559388A (en) * | 2012-02-27 | 2012-07-11 | 浙江中烟工业有限责任公司 | Essential oil of tobaccos as well as preparation method and application thereof to cigarettes |
| CN102813278B (en) * | 2012-08-09 | 2017-03-15 | 深圳瀚星翔科技有限公司 | A kind of mixed type electronic cigarette tobacco liquid |
| CN102952638B (en) * | 2012-11-13 | 2014-07-02 | 广东中烟工业有限责任公司 | Preparation method and application of tobacco endogenous spice of Boshan aromatic tobacco |
| CN202961958U (en) * | 2012-11-13 | 2013-06-05 | 东华理工大学 | Decompressed soxhlet extractor |
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