CN104621707B - A kind of Turkish tobaccos extract and electronic cigarette liquid - Google Patents
A kind of Turkish tobaccos extract and electronic cigarette liquid Download PDFInfo
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- CN104621707B CN104621707B CN201510046224.0A CN201510046224A CN104621707B CN 104621707 B CN104621707 B CN 104621707B CN 201510046224 A CN201510046224 A CN 201510046224A CN 104621707 B CN104621707 B CN 104621707B
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- extraction
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- extract
- turkish tobaccos
- soxhlet
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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
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
-
- 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
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
Abstract
The invention discloses a kind of Turkish tobaccos extract and electronic cigarette liquid. This Turkish tobaccos extract, with the Nicotiana tabacum L. of Turkish tobaccos, tobacco shred, offal and/or flue dust for raw material, apparatus,Soxhlet's adds Extraction solvent raw material is carried out surname extraction, it is improved by the condensing tube of apparatus,Soxhlet's and connects vacuum pump, make the vacuum in described apparatus,Soxhlet's maintain 20��80mmHg; In described condensing tube, the temperature of condensed fluid is less than-5 DEG C; After surname extraction completes, collect extracting solution, extracting solution concentration is obtained Turkish tobaccos extract. The present invention makes whole surname extraction system be in negative pressure state, reduces the boiling point of Extraction solvent, makes Extracting temperature reduce, and in extraction process, solvent circulation is accelerated, and extracts frequency and accelerates, in hgher efficiency. Simultaneously because solvent heating-up temperature is lower, extraction conditions is gentleer, it is to avoid excessive chemical reaction between aroma component in the extract that solvent high-temperature heating causes, extract miscellaneous QI is less.
Description
Technical field
The invention belongs to electronic cigarette technical field, specifically a kind of Turkish tobaccos extract and electronic cigarette liquid.
Background technology
Electronic cigarette is as a kind of novel tobacco goods, and electronic cigarette liquid determines the sense organ style and features of electronic cigarette, and therefore the preparation of electronic cigarette liquid becomes the key of electronic cigarette product. The basic technique principle of electronic cigarette is, when sucking electronic cigarette, electronic smoke atomizer is powered by electronic cigarette battery, and nebulizer is started working, and the tobacco juice atomization being stored in electronic cigarette is produced smog. Tobacco juice in electronic cigarette, also referred to as " ree-oil ", is stored in adsorbing material, is commonly called as " adsorption cotton ". Tobacco juice in electronic cigarette, is actually a formula essence, and when sucking electronic cigarette, atomization is for " smog ", and smog includes the materials such as the glycerol, the propylene glycol that evaporate in essence and the fragrance matter evaporated in essence. Tobacco juice for electronic smoke is the source of electronic cigarette fragrance, decides the taste style of electronic cigarette, decides whether product is esthetically acceptable to the consumers. Therefore, the tobacco juice formula technique of electronic cigarette, is one of the key technology of electronic cigarette. Electronic cigarette liquid mainly includes two parts, a part is for causing perfumery, a part causes the base solvent of perfumery for dissolving, furthermore it is possible to adding portion adjuvant, meet the needs of different crowd, wherein, the fragrance of electronic cigarette mainly by causing perfumery offer, causes the mixture that perfumery is various spice, the extracts using Nicotiana tabacum L.s more.
The Nicotiana tabacum L. extracting method of current broad sense, including high-temperature retorting or the high temperature extracting method such as 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, while obtaining Nicotiana tabacum L. aroma component, because what high-temperature heating will certainly destroy Nicotiana tabacum L. itself causes perfumery, and high-temperature heating also brings along deep reaction, these all can bring unnecessary miscellaneous QI to extract, affects the organoleptic quality evaluations of extract. Traditional solvent extraction process is used mostly organic solvent and mixes with Nicotiana tabacum L. and be placed in flask and heat, or until boiling, to increase the dissolubility of organic solvent, dissolves the spice in Nicotiana tabacum L., then filter, and filtrate concentration is obtained extract. This traditional method, 1. extraction efficiency is not high, because certain solvent easily reaches saturated, then cannot extract the aroma component of needs from Nicotiana tabacum L.;2. heating until refluxing to improve extraction efficiency, temperature rises to the boiling point of solvent, can give equally and extract product and bring unnecessary miscellaneous QI; 3. need after extracting to filter, the filtration after extracting especially for flue dust, very consuming time.
There is a general problem in current electronic cigarette product, electronic cigarette liquid lacks the flavor characteristics of tobacco or the flavor characteristics of tobacco is weak, and some is even closer to food such as chewing gum, in style with suck Medicated cigarette and there is relatively large deviation, on the whole close to style food. Therefore, explore variety classes raw tobacco material extract, necessary in order to improve the basic smoke of electronic cigarette, the sense rich, fine and smooth of cigarette perfume (or spice) and gratification.
Summary of the invention
Present invention solves the technical problem that and be, electronic cigarette liquid lacks the flavor characteristics of tobacco or the flavor characteristics of tobacco is weak.
One of technical scheme is, a kind of Turkish tobaccos extract is provided, with the Nicotiana tabacum L. of Turkish tobaccos, tobacco shred, offal and/or flue dust for raw material, apparatus,Soxhlet's adds Extraction solvent raw material is carried out surname extraction, the condensing tube of apparatus,Soxhlet's connects vacuum pump, makes the vacuum in described apparatus,Soxhlet's maintain 20��80mmHg; In described condensing tube, the temperature of condensed fluid is less than-5 DEG C; After surname extraction completes, collect extracting solution, extracting solution concentration is obtained Turkish tobaccos extract.
Further, described Extraction solvent is ethanol, normal hexane, hexamethylene or petroleum ether.
Further, the condensing tube used in described surname extraction is serpentine condenser.
Further, the extraction time of described surname extraction is 3��8h.
Further, the volume of described Extraction solvent is 14��30 times of raw material volume.
Further, before described surname extraction, raw material is placed in Extraction solvent and soaks 4��8h.
Further, the raw material after described immersion is carried out ultrasonic or microwave extracting 0.5��1h.
Another technical scheme of the present invention is to provide a kind of electronic cigarette liquid, above-mentioned Turkish tobaccos extract is dissolved in base solvent and obtains. Described base solvent is glycerol, propylene glycol, ethanol, the mixture of water or the wherein mixture of three kinds. Wherein being allocated as follows of mass percent: the water of mass percent 0��20%, 60��70% glycerol, 0��20% ethanol, 0��20% propylene glycol.
The another technical scheme of the present invention is, one is provided to grow tobacco extracting method, with Nicotiana tabacum L., tobacco shred, offal and/or flue dust for raw material, apparatus,Soxhlet's adds Extraction solvent raw material is carried out surname extraction, the condensing tube of apparatus,Soxhlet's connects vacuum pump, makes the vacuum in described apparatus,Soxhlet's maintain 20��80mmHg; In described condensing tube, the temperature of condensed fluid is less than-5 DEG C; After surname extraction completes, collect extracting solution, extracting solution concentration is obtained tobacco extract.
Turkish tobaccos have special giving off a strong fragrance, and strength is big, and fragrance protectiveness can be good. Turkish tobaccos are extracted by the present invention, prepare Turkish tobaccos extract as tobacco juice for electronic smoke, increase the flavour of electronic cigarette.
It is desirable to provide a kind of Turkish tobaccos raw extract, taking different producing area, the Turkish tobaccos Nicotiana tabacum L. of different parts according to formulary requirements or be cut into tobacco shred or to be ground into offal be raw material, nontoxic with ethanol, normal hexane, hexamethylene or petroleum ether etc. or micro-poison organic solvent carries out low temperature and repeatedly extracts. Repeatedly extract for realizing low temperature, improved on Soxhlet extraction device, connect vacuum pump in the condensing tube upper end of apparatus,Soxhlet's by a glass three-way valve, make vacuum maintain 20��80mmHg, solvent can be seethed with excitement at a lower temperature, turn avoid the too high generation side reaction of temperature.Serpentine condenser chosen by condensing tube, and the size of condensing tube can be made to lengthen, and condensing tube passes into cold cycle condensed fluid, and condensate temperature is-10��-5 DEG C, to improve condensation effect, it is prevented that solvent is taken away by vacuum pump. After decompression reduces the boiling point of solvent, solvent evaporative cooling circulation rate is accelerated, extraction frequency is accelerated, it is extracted under gentleer temperature conditions to carry out, avoid excessive chemical reaction between aroma component in the extract that solvent high-temperature heating causes, sensory evaluation thinks that the 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 raw tobacco material, polarity size and boiling point based on solvent are different, in the extract finally given, the content of each aroma component is different, the causing perfumery Semi-polarity fragrance component content and can increase of solvent extraction as strong in polarity; Equally, the causing nonpolar fragrance component content in perfumery and can increase of the solvent extraction that polarity is weak. According to the extract that opposed polarity solvent extraction obtains, according to the needs of formula, meet different formulary requirements. Advantage such as ethanol extraction is in that, alcohol solvent will not bring solvent miscellaneous QI, with the obvious advantage in sensory evaluation, additionally belongs to polar solvent, it is easy to extract the polarity aroma component in Nicotiana tabacum L.. And the relative ethanol of normal hexane, polarity is less, and the extraction effect of aroma component nonpolar in Nicotiana tabacum L. is better than ethanol, and therefore normal hexane leaf tobacco extract often strength is big, and gratification is strong, and inferior position is in that extract slightly miscellaneous QI.
The volume of Extraction solvent is 14��30 times of raw material volume, and the spice in Nicotiana tabacum L. can be made to be fully dissolved out, and is unlikely to again waste solvent, and extraction time is 4��8h, it is ensured that being fully dissolved out of spice, it is to avoid long-time heating produces miscellaneous QI. After extraction completes, collect extracting solution, concentrating under reduced pressure, after dissolving with base solvent, can be used as electronic cigarette liquid. The electronic cigarette that this electronic cigarette liquid is made can improve the flue gas mass of electronic cigarette, improve local flavor, increase gratification.
The described experimental provision that extracts is optimized on the basis of Soxhlet extraction device, is improved, important improvement is in that to connect vacuum pump on the top of surname extraction, whole extraction system is made to be in negative pressure state, to reduce the boiling point of Extraction solvent, Extracting temperature is made to reduce, in extraction process, solvent circulation is accelerated, and extracts frequency and accelerates, and under the identical time, extraction efficiency is higher. 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, reaches to extract requirement; And when reducing pressure, when negative pressure reaches-0.090Mpa (vacuum is about 76mmHg), water-bath design temperature 55 DEG C can meet requirement. Under negative pressure state, solvent has the risk taken away by vacuum pump, in order to ensure that solvent can effectively cool down and be repeatedly circulated, the present invention takes two corrective measures: first extracts condensing tube and chooses serpentine condenser and by the extended length 50% of condensing tube, to increase solvent condensation distance, make condensed fluid that the cooling of Extraction solvent is more abundant; Secondly passing into sub-cooled circulation fluid to condensing tube, the temperature of condensed fluid, below-5 DEG C, can substantially meet condensation requirement between-10��-5 DEG C.
It addition, raw material (Nicotiana tabacum L. or tobacco shred or offal or flue dust) is soaked 4��8h with coordinative solvent before extracting, then extract, it is possible to improve extraction effect. Furthermore, the raw material after solvent soaking is first carried out ultrasonic or microwave extracting 0.5��1h, then it is better to carry out extraction effect.
The present invention proposes the Soxhlet extraction method of a kind of improvement, and significant improvement is in that on the condensing tube of surname extraction to connect vacuum pump, make whole extraction be under negative pressure state. Under negative pressure, boiling temperature significantly reduces, and fresh solvent circulation is accelerated, and extracts frequency and accelerates, and extraction efficiency is higher. Simultaneously because solvent heating-up temperature is lower, extraction conditions is gentleer, it is to avoid excessive chemical reaction between aroma component in the extract that solvent high-temperature heating causes, extract miscellaneous QI is less. Relatively-high temperature extracting method and traditional solvent extraction process, the extract that the present invention obtains because obtaining under less Extracting temperature, therefore extract product and more can embody genuineness, avoid in high temperature extraction method, because of the high temperature in extraction process, unnecessary degree of depth chemical reaction occurs, the basic smoke of Nicotiana tabacum L. is provided for electronic cigarette liquid. The advantage of the Nicotiana tabacum L. extracting method of the present invention is in that:
(1) solvent extraction temperature is low, do not destroy the fragrance component that Nicotiana tabacum L. is intrinsic, it is to avoid excessive chemical reaction between aroma component in the extract that solvent high-temperature heating causes, and extracts product and well maintains the genuineness of Nicotiana tabacum L., and extract miscellaneous QI is less;
(2) extraction efficiency is high, and under negative pressure, boiling temperature reduces, and fresh solvent circulation is accelerated, and extracts frequency and accelerates, and extraction efficiency increases, and extracts completely.
The advantage that the present invention inherits Soxhlet extraction method, first circulate fresh solvent repeatedly and constantly extract the aroma component in raw tobacco material, extraction efficiency is high, the present invention connects vacuum pump by the top at surname extraction, makes whole extraction system be in negative pressure state, reduces the boiling point of Extraction solvent, Extracting temperature is made to reduce, in extraction process, solvent circulation is accelerated, and extracts frequency and accelerates, and under the identical time, extraction efficiency is higher. Simultaneously because solvent heating-up temperature is lower, extraction conditions is gentleer, it is to avoid excessive chemical reaction between aroma component in the extract that solvent high-temperature heating causes, sensory evaluation thinks that the extract miscellaneous QI under temperate condition is less.
Accompanying drawing explanation
Fig. 1 is surname extraction experimental provision schematic diagram used in the present invention.
Fig. 2 is the GC-MS figure of the extract obtained composition of the embodiment of the present invention 1.
Fig. 3 is the GC-MS comparison diagram of the extract obtained composition of the embodiment of the present invention 1 and embodiment 2.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described. Following example are intended to illustrate the present invention rather than limitation of the invention further.
The Soxhlet extraction device such as Fig. 1 used in embodiment, mainly connects a vacuum pump on conventional Soxhlet extraction device top and makes surname extraction extract under certain negative pressure, selects the apparatus,Soxhlet's with long condensing tube for extracting simultaneously.
Comparative example
By 10g Turkey Turkish tobaccos IzmirA (2013) offal with 200mL soaked in absolute ethyl alcohol 4h, heating in water bath carries out conventional surname extraction 4h, bath temperature is set as 90 DEG C, extracting solution is evaporated to solvent and does, and concentrate dissolves with (5mL water+5mL dehydrated alcohol+20mL glycerol). As the tobacco juice perfuming of electronic cigarette, evaluation result of smokeing panel test is: have Turkish tobaccos feature, the rich increase of flue gas.
Embodiment 1
By 10g Turkey Turkish tobaccos IzmirA (2013) offal with 200mL soaked in absolute ethyl alcohol 4h, the Soxhlet extraction device improved with the present invention carries out extracting 3h, vacuum is 40mmHg, water bath heating temperature is 50 DEG C, extracting solution is evaporated to solvent and does, and concentrate dissolves with (5mL water+5mL dehydrated alcohol+20mL glycerol).As the tobacco juice perfuming of electronic cigarette, evaluation result of smokeing panel test is: have obvious Turkish tobaccos feature, and flue gas is rich to be dramatically increased. Relative to comparative example, cigarette perfume (or spice) is purer. Fig. 2 is the GC-MS figure of fragrance component in the embodiment of the present invention 1 gained electronic cigarette liquid, owing to the peak value of nicotine is too big, for clearly showing other components, does not draw too high peak completely. In Fig. 2: 1 is isopropylformic acid.; 2 is bran aldehyde; 3 is 3-methvl-pentanoic acid; 4 is 2,4-dihydroxy-2,5-dimethyl-3 (2H)-furan-3-ketone; 5 is 2-oxo-1,3-propanedicarboxylic acid; 6 is 3-hydroxy-butyric acid; 7 is 1-(3-pyridine)-ethyl ketone; 8 is DDMP; 9 is 5 hydroxymethyl furfural; 10 is nicotine; 11 is pinane. As shown in Figure 2, in Turkish tobaccos extract, the content of lower fatty acid is substantially more, determines the style and features of Turkish tobaccos.
Embodiment 2
10g Turkey Turkish tobaccos IZMIR-NEWAG Turkish tobaccos (2008) offal is soaked 4h with 200mL normal hexane, the Soxhlet extraction device improved with the present invention carries out extracting 3h, vacuum is 80mmHg, water bath heating temperature is 45 DEG C, extracting solution is evaporated to solvent and does, concentrate dissolves with (5mL water+5mL dehydrated alcohol+20mL glycerol), as sample sample. The ree-oil made using embodiment 1 is as control sample, and as the tobacco juice perfuming of electronic cigarette, sensory evaluating smoking's evaluation result is: compared with the control, and sample flue gas is rich dramatically increases in test, slightly miscellaneous QI.
Fig. 3 is superposing of GC-MS figure and Fig. 2 of fragrance component in embodiment 3 gained electronic cigarette liquid. As can be seen from Figure 3, ethanol is polar solvent, and normal hexane is as non-polar solven, the aroma component dense distribution that non-polar solven normal hexane extraction goes out is at the short region of retention time, the i.e. left end (remarks: GC-MS pillar is polar column) of GC-MS figure. Citing, the nicotine in extract belongs to polar substances, as can be seen from Figure 3 normal hexane to its extraction effect obviously than polar solvent ethanol weak a lot. Fig. 3 illustrates that the aroma component that the solvent extraction of opposed polarity obtains is differentiated, and therefore the present invention proposes to select different solvents, obtains the electronics ree-oil that style is given priority to, to meet electronic cigarette formulary requirements.
Embodiment 3
By 10g Turkey Turkish tobaccos IZMIR-NEWAG Turkish tobaccos (2008) offal with 200mL soaked in absolute ethyl alcohol 4h, the Soxhlet extraction device improved with the present invention carries out extracting 3h, vacuum is 40mmHg, water bath heating temperature is 50 DEG C, extracting solution is evaporated to solvent and does, concentrate dissolves with (5mL water+5mL dehydrated alcohol+20mL glycerol), as the tobacco juice perfuming of electronic cigarette. Making two samples, one is added commercially available electronic cigarette liquid 0.5ml, as control sample; Another is as experiment sample, adding the commercially available electronic cigarette liquid 0.5ml identical with control sample, separately add Turkish tobaccos extraction tobacco juice prepared by 0.25ml the present embodiment again, contrasting evaluation result of smokeing panel test is: relative to control sample, the flue gas of experiment sample is rich to be dramatically increased, and flue gas is softer, fine and smooth.
Claims (5)
1. a Turkish tobaccos extract, it is characterized in that, with the Nicotiana tabacum L. of Turkish tobaccos, tobacco shred, offal and/or flue dust for raw material, apparatus,Soxhlet's adds Extraction solvent raw material is carried out surname extraction, the condensing tube of apparatus,Soxhlet's connects vacuum pump, makes the vacuum in described apparatus,Soxhlet's maintain 20��80mmHg; In described condensing tube, the temperature of condensed fluid is less than-5 DEG C; After surname extraction completes, collect extracting solution, extracting solution concentration is obtained Turkish tobaccos extract;Described condensing tube is serpentine condenser; The extraction time of described surname extraction is 3��8h; The volume of described Extraction solvent is 14��30 times of raw material volume.
2. Turkish tobaccos extract as claimed in claim 1, it is characterised in that described Extraction solvent is ethanol, normal hexane, hexamethylene or petroleum ether.
3. Turkish tobaccos extract as claimed in claim 1, it is characterised in that before described surname extraction, raw material is placed in Extraction solvent and soaks 4��8h.
4. Turkish tobaccos extract as claimed in claim 3, it is characterised in that the raw material after described immersion is carried out ultrasonic or microwave extracting 0.5��1h.
5. an electronic cigarette liquid, it is characterised in that the Turkish tobaccos extract one of Claims 1 to 4 Suo Shu is dissolved in base solvent and obtains.
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| CN201510046224.0A CN104621707B (en) | 2015-01-29 | 2015-01-29 | A kind of Turkish tobaccos extract and electronic cigarette liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107114821B (en) * | 2017-07-07 | 2019-03-19 | 重庆中烟工业有限责任公司 | A kind of device and method of hot trapping preparation smoke fragrance |
| CN107898002B (en) * | 2017-11-29 | 2020-09-25 | 苏州市信睦知识产权服务有限公司 | Device for preparing tobacco flavor spice |
| CN113684097A (en) * | 2021-08-27 | 2021-11-23 | 云南养瑞科技集团有限公司 | Novel continuous heat treatment equipment for tobacco flavor and use method |
| CN114196476A (en) * | 2021-09-08 | 2022-03-18 | 广州东智盟化妆品有限公司 | Extraction method of whitening and freckle-removing perilla frutescens essential oil and extract |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS4813599B1 (en) * | 1969-08-14 | 1973-04-27 | ||
| JPS493676Y2 (en) * | 1971-06-30 | 1974-01-29 | ||
| 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 |
| CN101624555B (en) * | 2009-07-30 | 2012-10-10 | 无锡嘉华香精香料有限公司 | Preparation method of tobacco extract and product thereof |
| 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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