CN104939305A - Tobacco extract and electronic cigarette liquid - Google Patents
Tobacco extract and electronic cigarette liquid Download PDFInfo
- Publication number
- CN104939305A CN104939305A CN201510258183.1A CN201510258183A CN104939305A CN 104939305 A CN104939305 A CN 104939305A CN 201510258183 A CN201510258183 A CN 201510258183A CN 104939305 A CN104939305 A CN 104939305A
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- Prior art keywords
- extract
- tobacco
- water
- ethanol
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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
- A24B15/26—Use of organic solvents for extraction
Abstract
The invention discloses tobacco extract and electronic cigarette liquid. A preparation method of the tobacco extract comprises the following steps that (1), tobacco powder or/and tobacco shreds serve as raw materials, the raw materials are extracted with ethanol water with the volume fraction more than 75%, an extracting solution is concentrated to obtain ethanol extract, ethanol is used for dissolving the ethanol extract, then the ethanol extract is frozen, dissolved out, precipitated and filtered, and filter liquor is concentrated to obtain extract I; (2), the raw materials extracted with the ethanol are extracted with water, water extract is obtained, the water extract is leached with a solvent A, water phases are collected and then are used for leaching a solvent B, and organic phases are collected and concentrated to obtain extract II, wherein the solvent A is one or more of petroleum ether, normal hexane and cyclohexane, and the solvent B is ethyl acetate or dichloromethane; (3), the extract I and the extract II are mixed to obtain the tobacco extract. The tobacco extract keeps the tobacco aroma, the amount of aroma is full, no black residue exists after atomization, and no scorched flavor exists.
Description
Technical field
The present invention relates to a kind of tobacco extract and electronic cigarette liquid, particularly a kind of have electronic cigarette liquid that is fragrant and sweet and baking fragrant breeze lattice, belongs to electronic cigarette field.
Background technology
In recent years, the novel tobacco such as low temperature cigarette, electronic cigarette goods are just in rapid rising.Electronic cigarette profile is similar to common cigarette, is the device that one can be vaporized into electronic cigarette liquid (also known as electronics tobacco tar, being a kind of fragrance solution) fog, brings the sensation of similar smoking to smoker.
Electronic cigarette decreases the injury of the health to people while the custom meeting people's smoking.Generally, electronic cigarette has following principal characters: one is do not need burning, compares traditional cigarette harmfulness less; Two be PE is had an impact relatively little; Three is the needs that can adapt to and meet consumer to a certain extent.
But compare with traditional cigarette, electronic cigarette exists huge spread on the aesthetic quality sucked, to flavor quality satisfaction not when smoker sucks electronic cigarette, sensation electronic cigarette hay-scented is lightly seasoned thin.
Atomized liquid of electronic smoke disclosed in Chinese patent 200910310536.2, forms with allotment such as leaf tobacco extract 3-5% w/v, tobacco essence 3-5% w/v, nicotine 0-3% w/v pure water 5-10% w/v, propane diols 50-70% w/v etc.Chinese patent 20130195029.5 discloses a kind of fresh and sweet fragrant electrical heating electronic cigarette liquid, obtains the electronic cigarette liquid with fresh and sweet perfume (or spice) after mixing with pipe tobacco water extract, water, propane diols and glycerine.These electronic cigarette liquids are the product allocated of leaf tobacco extract and other essence and flavoring agents mainly, does not specifically describe tobacco extracted method.Tobacco leaf or pipe tobacco ethanol or water mainly extract at low temperature by traditional leaf tobacco extract, in the tobacco extract obtained, some macromolecular substances are after heating atomization, electronic smoke atomizer has black residue, during suction, the heating of these black residue has and is charred taste again, affect the mouthfeel of next time aspirating, therefore tobacco extract must be refined, by separation means such as extractions, remove the macromolecular substances such as carbohydrate and protein, obtain the aroma substance in tobacco with better basic cigarette perfume (or spice).
Summary of the invention
The present invention be directed to tobacco aroma that existing electronic cigarette liquid exists not, taste bad will, easily occur being charred the technical problems such as taste.
Technical scheme of the present invention is, provides a kind of tobacco extract, and the preparation method of this extract comprises the following steps:
(1) with offal or/and pipe tobacco is raw material, extract raw material with the ethanol water that volume fraction is more than 75%, extract is concentrated to obtain ethanol extract; With ethanol, ethanol extract is first dissolved, more freezing precipitation precipitation, filter, filtrate concentrates to obtain extract I;
(2) with water, the raw material crossed through alcohol extract is extracted, obtain water extract; Extracted by water extract solvent orange 2 A, collect aqueous phase, aqueous phase extracts with solvent B again, collects organic phase, and organic phase concentrates to obtain extract II; Described solvent orange 2 A is one or more in benzinum, n-hexane, cyclohexane, and solvent B is that ethyl acetate is or/and carrene;
(3) extract I and extract II are mixed to get described tobacco extract.
Further, the mass ratio of described extract I and extract II mixing is 1 ︰ 1 ~ 1 ︰ 3.
Further, in described step (1), extract at 50 ~ 80 DEG C with ethanol water.
Further, described freezing temperature is 0 ~ 6 DEG C.
Further, the volume fraction of described ethanol water is 95%.
Further, in described step (2), with water, ultrasonic extraction is carried out to the raw material crossed through alcohol extract.
Further, the time of described ultrasonic extraction is 20 ~ 40 minutes.
The present invention further provides a kind of electronic cigarette liquid, comprise base solvent and described tobacco extract.
Further, the volume of described base solvent is 3 ~ 6 times of tobacco extract volume.
Further, described base solvent comprise mass percent be 1 ~ 5% water, 10 ~ 30% glycerine, the propane diols of 3 ~ 15%, the butanediol of 10 ~ 50% and 10 ~ 40% propene carbonate.
Electronic cigarette liquid of the present invention utilizes the solvent of opposed polarity to extract offal or pipe tobacco, and utilize the separation means such as extraction and filtration to refine, obtain that there is the extract I of baking fragrant breeze lattice and the extract II with fragrant and sweet style, mix in certain proportion, obtain tobacco extract; Dilute by the base solvent of electronic cigarette liquid, allotment, obtains the electronic cigarette liquid of better basic cigarette perfume (or spice) again.Through chromatography, the fragrance component of extract I comprises the compounds such as 5 methyl furfural, 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrones, 5 hydroxymethyl furfural, nicotine, hexadecylic acid and stearic acid.Wherein 5 methyl furfural, 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrones, these compounds of 5 hydroxymethyl furfural are all the compounds in tobacco with baking fragrance, therefore give extract I to toast the fragrance of style.The fragrance component of extract II comprises 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrones, phenylacetic acid, nicotine, 3-hydroxyl--damascenone, Megastigmatrienone, 3-oxo-compound such as irisone, stearic acid.Wherein 3-hydroxyl--damascenone, Megastigmatrienone, these compounds of 3-oxo-irisone are all the compounds in tobacco with fragrant and sweet style, therefore give extract II with the fragrance of fragrant and sweet style.
The invention has the beneficial effects as follows, utilize the solvent of opposed polarity to extract respectively offal or pipe tobacco, then through separation means such as extraction and filtrations, then with certain proportion mixing, obtain the electronic cigarette liquid of better basic cigarette perfume (or spice).After atomizer atomization, smoker feels to have fragrant and sweet and baking fragrant breeze lattice tobacco aroma preferably, and flue gas exquisiteness is soft, and pleasant impression is comfortable, there is not black residue matter and is charred taste.
Accompanying drawing explanation
Fig. 1 is the GC-MS figure of fragrance component in the embodiment of the present invention 2 extract obtained 1;
In figure, 1 is 5 methyl furfural; 2 is 2-methylfuroate; 3 is 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrones; 4 is 5 hydroxymethyl furfural; 5 is phenylacetic acid; 6 is nicotine; 7 is Megastigmatrienone; 8 is methyl hexadecanoate; 9 is hexadecylic acid; 10 is stearic acid.
Fig. 2 is the GC-MS figure of fragrance component in the extract obtained II of the embodiment of the present invention 2;
In figure, 11 is 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrones; 12 is 5 hydroxymethyl furfural; 13 is phenylacetic acid; 14 is nicotine; 15 is 3-hydroxyl--damascenone; 16 is Megastigmatrienone; 17 is 3-oxo-irisone; 18 for planting acetic acid; 19 is stearic acid dienol; 20 is stearic acid.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described.
embodiment 1
The present embodiment provides a kind of tobacco extract and electronic cigarette liquid, its preparation method is as follows: the ethanol lixiviate 1d at normal temperatures adding 500 milliliters of 85vol% in the B3F of 50g Sangzhi, filter, filtrate is concentrated into dry ethanol extract, add 40 milliliters of hot ethanols and dissolve ethanol extract, then the solution after dissolving is placed the freezing precipitation precipitation of 2h at 4 DEG C, filter, be concentrated into 10 milliliters, obtain extract I.The pipe tobacco that alcohol extract is crossed uses 500 ml waters ultrasonic 30 minutes at normal temperatures again, filter to obtain water extract, water extract first uses the n-hexane degreasing of 300 milliliters, and the process of n-hexane degreasing is actual to be extracted aqueous extract with n-hexane exactly, collect aqueous phase (skimming processes, lower same); Aqueous phase uses the dichloromethane extraction of 300 milliliters again, and carrene is evaporated to 10 milliliters at 30 DEG C, obtains extract II.Get 2 milliliters of extract I and 2 milliliters of extract II mixing respectively, dilute 6 times by base solvent, obtain containing described electronic cigarette liquid.
Getting the above-mentioned electronic cigarette liquid of 1mL adds in electronic smoke atomizer, and smoked panel test by the personnel that smoke panel test of specialty, electronic cigarette has tobacco aroma, and perfume quantity is comparatively sufficient, without black residue, without being charred taste.
embodiment 2
The present embodiment provides a kind of tobacco extract and electronic cigarette liquid, its preparation method is as follows: the ethanol lixiviate 1d at normal temperatures adding 2000 milliliters of 95vol% in 180g pipe tobacco Zimbabwe pipe tobacco, filter, add 150 milliliters of hot ethanols after filtrate is concentrated to dissolve, obtain ethanol extract, at 4 DEG C, place the freezing precipitation precipitation of 2h, filter, be concentrated into 30 milliliters, obtain extract I.The pipe tobacco that alcohol extract is crossed uses 2000 ml waters ultrasonic 30 minutes at normal temperatures again, filter to obtain water extract, water extract first uses the petroleum ether degreasing of 1000 milliliters, then uses the extraction into ethyl acetate of 1000 milliliters, ethyl acetate is evaporated to 40 milliliters at 40 DEG C, obtains extract II.
Through chromatography, as shown in Figure 1, the material that in figure, the peak position of each label represents is as follows: 1 is 5 methyl furfural; 2 is 2-methylfuroate; 3 is 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrones; 4 is 5 hydroxymethyl furfural; 5 is phenylacetic acid; 6 is nicotine; 7 is Megastigmatrienone; 8 is methyl hexadecanoate; 9 is hexadecylic acid; 10 is stearic acid.The fragrance component of extract I comprises the compounds such as 5 methyl furfural, 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrones, 5 hydroxymethyl furfural, nicotine, hexadecylic acid and stearic acid.Wherein 5 methyl furfural, 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrones, these compounds of 5 hydroxymethyl furfural are all the compounds in tobacco with baking fragrance, therefore give extract I to toast the fragrance of style.As shown in Figure 2, the material that in figure, the peak position of each label represents is as follows: 11 is 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrones; 12 is 5 hydroxymethyl furfural; 13 is phenylacetic acid; 14 is nicotine; 15 is 3-hydroxyl--damascenone; 16 is Megastigmatrienone; 17 is 3-oxo-irisone; 18 for planting acetic acid; 19 is stearic acid dienol; 20 is stearic acid.The fragrance component of extract II comprises 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyrones, phenylacetic acid, nicotine, 3-hydroxyl--damascenone, Megastigmatrienone, 3-oxo-compound such as irisone, stearic acid.Wherein 3-hydroxyl--damascenone, Megastigmatrienone, these compounds of 3-oxo-irisone are all the compounds in tobacco with fragrant and sweet style, therefore give extract II with the fragrance of fragrant and sweet style.
Get 5 milliliters of extracts 1 and 10 milliliters of extract II mixing respectively, dilute 4 times by base solvent, obtain described electronic cigarette liquid.Getting the above-mentioned electronic cigarette liquid of 1mL adds in electronic smoke atomizer, is smoked panel test by the personnel that smoke panel test of specialty, and electronic cigarette has good tobacco fragrant, and fragrance enriches, and fine and smooth soft, pleasant impression is comfortable, without black residue, without being charred taste.
embodiment 3
The present embodiment provides a kind of tobacco extract and electronic cigarette liquid, its preparation method is as follows: the ethanol lixiviate 1d at normal temperatures adding 800 milliliter 75% in 80g white sand tobacco leaf formulation offal, filter, filtrate is concentrated into dry ethanol extract, add 60 milliliters of hot ethanols and dissolve ethanol extract, the solution after dissolving places the freezing precipitation precipitation of 2h at 4 DEG C, filters, be concentrated into 15 milliliters, obtain extract I.The pipe tobacco that alcohol extract is crossed uses 800 ml waters ultrasonic 30 minutes at normal temperatures again, filter to obtain water extract, water extract first uses the petroleum ether degreasing of 500 milliliters, then uses the dichloromethane extraction of 500 milliliters, carrene is evaporated to 20 milliliters at 40 DEG C, obtains extract II.Get 5 milliliters of extract I and 8 milliliters of extract II mixing respectively, dilute 3 times by base solvent, obtain described electronic cigarette liquid.
Getting the above-mentioned electronic cigarette liquid of 1mL adds in electronic smoke atomizer, is smoked panel test by the personnel that smoke panel test of specialty, and the atomizing effect of electronic cigarette is better, has certain tobacco aroma, without black residue, without being charred taste.
Claims (10)
1. a tobacco extract, is characterized in that, the preparation method of this extract comprises the following steps:
(1) with offal or/and pipe tobacco is raw material, extract raw material with the ethanol water that volume fraction is more than 75%, extract is concentrated to obtain ethanol extract; With ethanol, ethanol extract is first dissolved, more freezing precipitation precipitation, filter, filtrate concentrates to obtain extract I;
(2) with water, the raw material crossed through alcohol extract is extracted, obtain water extract; Extracted by water extract solvent orange 2 A, collect aqueous phase, aqueous phase extracts with solvent B again, collects organic phase, and organic phase concentrates to obtain extract II; Described solvent orange 2 A is one or more in benzinum, n-hexane, cyclohexane, and solvent B is that ethyl acetate is or/and carrene;
(3) extract I and extract II are mixed to get described tobacco extract.
2. tobacco extract as claimed in claim 1, is characterized in that, the mass ratio of described extract I and extract II mixing is 1 ︰ 1 ~ 1 ︰ 3.
3. tobacco extract as claimed in claim 1 or 2, is characterized in that, in described step (1), extract with ethanol water at 50 ~ 80 DEG C.
4. tobacco extract as claimed in claim 1 or 2, it is characterized in that, described freezing temperature is 0 ~ 6 DEG C.
5. tobacco extract as claimed in claim 1 or 2, it is characterized in that, the volume fraction of described ethanol water is 95%.
6. tobacco extract as claimed in claim 1 or 2, is characterized in that, in described step (2), carry out ultrasonic extraction with water to the raw material crossed through alcohol extract.
7. tobacco extract as claimed in claim 6, it is characterized in that, the time of described ultrasonic extraction is 20 ~ 40 minutes.
8. an electronic cigarette liquid, is characterized in that, comprises base solvent and the tobacco extract described in any one of claim 1 ~ 7.
9. electronic cigarette liquid as claimed in claim 8, it is characterized in that, the volume of described base solvent is 3 ~ 6 times of tobacco extract volume.
10. as claimed in claim 8 or 9 electronic cigarette liquid, is characterized in that, described base solvent comprise mass percent be 1 ~ 5% water, 10 ~ 30% glycerine, the propane diols of 3 ~ 15%, the butanediol of 10 ~ 50% and 10 ~ 40% propene carbonate.
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Cited By (7)
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| CN105542963A (en) * | 2015-12-30 | 2016-05-04 | 立场电子科技发展（上海）有限公司 | Method for extracting essence applicable to electronic cigarettes from betel nut |
| CN105686068A (en) * | 2016-03-11 | 2016-06-22 | 湖南中烟工业有限责任公司 | Electronic cigarette juice in style of burley tobaccos |
| CN107660812A (en) * | 2016-07-27 | 2018-02-06 | 湖南中烟工业有限责任公司 | A kind of Flue-cured Tobacco alkali extract and extraction process |
| CN108201166A (en) * | 2016-12-16 | 2018-06-26 | 湖南中烟工业有限责任公司 | A kind of electronic cigarette extract and preparation method thereof |
| CN110628508A (en) * | 2019-10-15 | 2019-12-31 | 深圳波顿香料有限公司 | Preparation method of compound plant extract for promoting production of body fluid and increasing moisture and cold-extraction electronic cigarette oil |
| CN113242696A (en) * | 2018-12-31 | 2021-08-10 | 菲利普莫里斯生产公司 | Liquid nicotine formulation |
| EP3732998A4 (en) * | 2017-12-27 | 2021-11-17 | Japan Tobacco Inc. | Tobacco extract, method for producing tobacco extract, and non-combustion flavor inhaler including tobacco extract |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542963A (en) * | 2015-12-30 | 2016-05-04 | 立场电子科技发展（上海）有限公司 | Method for extracting essence applicable to electronic cigarettes from betel nut |
| CN105686068A (en) * | 2016-03-11 | 2016-06-22 | 湖南中烟工业有限责任公司 | Electronic cigarette juice in style of burley tobaccos |
| CN105686068B (en) * | 2016-03-11 | 2017-05-10 | 湖南中烟工业有限责任公司 | Electronic cigarette juice in style of burley tobaccos |
| CN107660812A (en) * | 2016-07-27 | 2018-02-06 | 湖南中烟工业有限责任公司 | A kind of Flue-cured Tobacco alkali extract and extraction process |
| CN107660812B (en) * | 2016-07-27 | 2021-02-23 | 湖南中烟工业有限责任公司 | Cured tobacco nicotine extract and extraction process |
| CN108201166A (en) * | 2016-12-16 | 2018-06-26 | 湖南中烟工业有限责任公司 | A kind of electronic cigarette extract and preparation method thereof |
| EP3732998A4 (en) * | 2017-12-27 | 2021-11-17 | Japan Tobacco Inc. | Tobacco extract, method for producing tobacco extract, and non-combustion flavor inhaler including tobacco extract |
| CN113242696A (en) * | 2018-12-31 | 2021-08-10 | 菲利普莫里斯生产公司 | Liquid nicotine formulation |
| CN110628508A (en) * | 2019-10-15 | 2019-12-31 | 深圳波顿香料有限公司 | Preparation method of compound plant extract for promoting production of body fluid and increasing moisture and cold-extraction electronic cigarette oil |
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| CN104939305B (en) | 2016-04-20 |
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