CN103468403B - A kind of water extraction and supercritical CO 2extraction process method of flavor matter in directed compound collecting tobacco from tobacco material - Google Patents
A kind of water extraction and supercritical CO 2extraction process method of flavor matter in directed compound collecting tobacco from tobacco material Download PDFInfo
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Abstract
The present invention relates to a kind of water extraction and supercritical CO
2extraction process method of flavor matter in directed compound collecting tobacco from tobacco material, step is as follows: 1) water extraction is directed from tobacco extracts polarity flavor matter; 2) supercritical carbon dioxide fluid extraction is directed from tobacco extracts nonpolar flavor matter; 3) by above-mentioned polarity flavor matter and the mixing of nonpolar flavor matter, formula rate is 1000: 0.1 ~ 5.Tobacco material used herein is offal, cigarette ash or the offal the like waste that the particle that produces in tobacco leaf, pipe tobacco or tobacco processing course is tiny, and " turning waste into wealth " decreases the pollution to environment; The present invention passes through tobacco water extracting liquid and tobacco supercritical CO
2extract carries out suitably than allotment, its composite spices that causes is sprayed in reconstituted tobacco, promotes the quality of reconstituted tobacco, increase perfume quantity, carry raise note, to set off nature cigarette fragrant, reduce flue gas drying sense, strengthen flue gas and to promote the production of body fluid sense, raising cigarette comfort level.
Description
Technical field
The present invention relates to Field of Tobacco, particularly relate to a directed composite extracting method growing tobacco this Studies of The Aromatic Substances of endogenous.
Background technology
Chemical composition in tobacco is numerous.Since 20 century 70s, due to the development of analysis and testing technology, the chemical composition in tobacco is constantly found.Shi Hongzhi etc. 2011 report, in the tobacco leaf through identifying, chemical composition has 4992 kinds, and wherein relevant to tobacco flavor have more than 700 to plant.In tobacco flavor matter molecule in containing the specific Zhi Xiang functional group such as-OH ,-CO ,-NH and-SH, irritate the different fragrance of generation with different can to the sense of smell of people.According to the difference of fragrance matter functional group, tobacco flavor material can be divided into alcohols, acids, ketone, ester class and terpene etc.Mostly tobacco flavor material is secondary metabolite, therefore also can be divided into the classifications such as carotenoid, phenylalanine degradation product, class western cypress alkanes degradation product, mailland reaction product according to Aroma precursor material in secondary metabolism.
Receive and the tankage such as the waster tobacco of about 25% can be produced in production process can not use at the Bian of tobacco, regarded refuse treatment more, while bringing pollution to environment, also cause the significant wastage of natural resources.For the reconstituted tobacco method that utilized recent domestic to rise of the tankage such as waster tobacco.Reconstituted tobacco, also known as making tobacco sheet, it utilizes discarded offal, tobacco leaf fragment, offal etc. to be raw material, through lixiviate, concentrated, separation, making beating, defibrination, manufacture paper with pulp, dry, perfuming process process, make the reconstituted tobacco thin slice of excellent property, as cigarette weighting material, be back to production of cigarettes.
Reconstituted tobacco can lose a part of this Studies of The Aromatic Substances of tobacco in the course of processing, needs to add a certain amount of tobacco endogenous spices to increase reconstituted tobacco fragrance fragrance, improves smoke, reduces xylon gas and pungent sense.Crucial aroma component containing organic acid, alcohols, carbonyl class, phenols, terpenes, carbohydrate, amino acids in the tobaccos such as neophytadiene, nicotine, solanone, trans-Damascenone, geranyl acetone, Megastigmatrienone, alpha, beta-lonone, phenyl aldehyde, phenylcarbinol, dihydroactinidiolide in waster tobacco, illustrate containing a large amount of important aroma components of tobacco in waster tobacco, can as the source of tobacco flavour.
Existing being carried out by waster tobacco water is extracted, concentrates at present, water extracting liquid is added to the fragrance fragrance improving reconstituted tobacco in reconstituted tobacco.Water extraction uses solvent to be water, and leaching process good economy performance, security are high, strong operability, and have good extraction effect to water-soluble flavor matters such as carbohydrate, amino acids, phenols in tobacco leaf, can improve the fragrance of reconstituted tobacco.But there is the crucial aroma component such as a large amount of low polarity, volatile organic acid, terpenes, alcohols in tobacco adopts its extraction effect of water extraction often poor, and volatile aroma component may destroy and lose in extraction, concentration process, still there is the shortcoming of fragrance deficiency in the reconstituted tobacco only adding water extracting liquid.
Supercritical liquid extraction technique has the incomparable high purity of traditional extraction process, All Pure Nature, no solvent residue and the feature such as pollution-free, has been widely used in now and has extracted essential oil in tobacco and spices.Nonpolar mostly or low-pole compound in volatile aromatic composition in tobacco, at supercritical CO
2in solubleness very large, be thus particularly suitable for adopting supercritical CO
2extract.Use supercritical CO
2abstraction technique is extracted tobacco aroma component from tobacco, extract the important aroma component contained in the aroma component that obtains all obtains much bigger than the extraction of traditional solvent extration on composition or percentage contents, this essential oil is used for perfuming cigarette and obviously can changes the fragrance of tobacco and suppress the assorted gas of tobacco.Adopt gas chromatograph and GC-MS to supercritical CO
2extract the product that obtains to analyze, find wherein mainly nonpolar and low-pole compound, and contain many important aroma components having substantial connection with the suction taste of cigarette.
In the tobacco leaf of document and patent report, the main extracting method of aroma component has water extraction, alcohol extracting method, supercritical extraction, molecular distillation method etc.Its document and Patent as follows:
LI XUEMEIs etc. utilize supercritical CO
2from oriental tobacco leaf concrete, extract tobacco cleaned oil, determining best extractant condition is extraction temperature 40 ~ 45 DEG C, and extracting pressure is 25 ~ 30MPa, CO
2flow 2 ~ 4L/min, extraction time 3 ~ 5h, certain the solvent mixture of 4% ~ 8% (volume ratio) is added as entrainment agent while extraction, can obtain the Turkish tobaccos absolute oil being equivalent to the thick cream amount 8% ~ 10% of raw material, experimental result also shows that entrainment agent is a vital factor of extracted tobacco absolute oil.
Zhu Renfa etc. point out, in order to extract required essential oil targetedly, can add the entrainment agents such as ethyl acetate to reduce CO
2solvability, improve its selectivity, and then improve the percentage extraction of essential oil.
Chinese patent (201010131371.5) " a kind of extracting method of neutral aroma compositions in tobacco ".It is characterized in that, the tobacco after pulverizing is loaded in supercritical extraction reactor, then pours supercritical CO
2fluid pressurized circulation, regulate extracting pressure 8 ~ 30MPa, temperature 35 ~ 60 DEG C, extraction time is 1 ~ 3 hour, solution after extracting tobacco is carried out two-stage decompression separation, entrainment agent is ethanol, the filler that flash trapping stage still is filled is zeolite, 4A molecular sieve, the mixture of ion exchange resin, the pressure of flash trapping stage still is 10 ~ 20MPa, temperature is 35 ~ 55 DEG C, the pressure of the second-order separation still is 4 ~ 6MPa, temperature is 35 ~ 45 DEG C, neutral aroma compositions in tobacco is obtained after separation, it is apolar substance that this extracting method obtains this Studies of The Aromatic Substances, composition is comparatively single, the Production requirement of banana aldehyde and reconstituted tobacco cannot be reached, simultaneously single technology cannot the plyability feature of complete embodiment person's character material.
Chinese patent (201110248504.1) " method that tobacco is extracted continuously ".This patent characteristic is that tobacco powder is broken into particle diameter and is no less than 20 object powder, add and be equivalent to tobacco volume 10-30 water medium doubly, adjust ph is to 9-13, and carry out ultrasonic pretreatment, ultrasonic power is no less than 20kHz, the ultrasonic pretreatment time is no less than 20 minutes, obtains ultrasonic pretreatment liquid, further extraction nicotine, hemicellulose, xylogen, Mierocrystalline cellulose.Although the method extracting substance is comparatively thorough, but operation is comparatively complicated, more comparatively assorted this Studies of The Aromatic Substances being not suitable for reconstituted tobacco of extracting substance adds, and the introducing of more material simultaneously can destroy the fragrance of tobacco equally, and abstraction process is single, this Studies of The Aromatic Substances extracts specificity shortcoming.
Chinese patent (201110183851.0) " a kind of preparation method of tobacco extract granules ".It is characterized in that a kind of preparation method of tobacco extract granules, first get tobacco leaf and/or offal and shredded, be solvent extraction with water or ethanol or ether, tobacco extract is obtained through sedimentation and filtration, reconcentration is to relative density 1.00-1.30 and control temperature is 20 ~ 40 DEG C, obtains tobacco and extracts concentrated solution or tobacco extract, then beta-cyclodextrin in mass ratio: flavouring essence for tobacco is 1 ~ 3:1, flavouring essence for tobacco and beta-cyclodextrin are carried out inclusion, the inclusion time is 1/5 ~ 3 hour, obtain spices and Benexate Hydrochloride, again spices and Benexate Hydrochloride and tobacco are extracted the drying of concentrated solution co-spray and obtain tobacco spray-drying powder, be added into subsequently in cigarette to increase tobacco flavor, what this invention was single have employed water, alcohol or ether are as extraction reagent, but the beta-cyclodextrin of the follow-up interpolation parent that only just the dried particles of auxiliary person's character material is shaping, lack the mediation of nonpolar person's character material, thus the mouthfeel aspect of tobacco promotes not obvious.
Chinese patent (200910027400) " a kind of preparation method of tobacco extract and application thereof ".The preparation method of described tobacco extract take tobacco as raw material, obtains tobacco extract through enzymolysis, ultrasonic extraction, filtration, chromatography column separation, concentrating under reduced pressure step; The dissolve with ethanol of described tobacco extract concentration 80%, adopts atomizing type spray to be added in pipe tobacco.The comparatively loaded down with trivial details very difficult large-scale industrial production of this invention step, and the spices that single mode is extracted becomes single, is not well positioned to meet the mouthfeel demand of reproducing pipe tobacco.
Chinese patent (201210412334.0) " a kind of preparation method of tobacco cleaned oil ".Get the thick extracted extract of 70g Turkish tobaccos and chemical filler mix evenly fills people's extraction kettle afterwards, carry out supercritical extraction, extraction temperature 40-45 DEG C, pressure 25-30MPa squeeze into while squeezing into flow velocity to be about the supercritical CO 2 of 2-5L/min add 4-8% (volume ratio) entrainment agent; After reaching extraction conditions, extraction time 3-5h, to obtain final product.Chemical filler can be the porcelain fillers such as granulated glass sphere, Raschig ring or rectangular saddle ring.
Summary of the invention
In order to solve above-mentioned technical problem, the object of the invention is to provide a kind of water extraction and supercritical CO
2extraction process method of flavor matter in directed compound collecting tobacco from tobacco material.It is simple that the method has technique, cost is low, this Studies of The Aromatic Substances good selective, with the obvious advantage in the fragrance reduction and lifting of reconstituted tobacco, to compare single extraction and add this Studies of The Aromatic Substances technology, the defects such as the present invention can solve that the suction taste of reconstituted tobacco is uncomfortable, harsh feeling and dry sensation, greatly promote the mouthfeel of reconstituted tobacco.。
The present invention for achieving the above object, adopts following technical scheme:
A kind of water extraction and supercritical CO
2extraction process method of flavor matter in directed compound collecting tobacco from tobacco material, the method comprises the following steps:
1) water extraction is directed from tobacco extracts polarity flavor matter
Tobacco material 3 ~ 9 times of water gagings 30 ~ 70 DEG C extract 0.5 ~ 2 hour, extract 1 ~ 3 time; It is 1.1 ~ 1.3mg/mL that extracting solution is concentrated into density;
2) supercritical carbon dioxide fluid extraction is directed from tobacco extracts nonpolar flavor matter
Extraction conditions is extraction kettle pressure is 20 ~ 30MPa, and extraction temperature is 35 ~ 45 DEG C, extraction time 2 ~ 4 hours, and separation condition is separating still pressure is 5 ~ 10MPa, and separation temperature is 35 ~ 50 DEG C;
3) by above-mentioned polarity flavor matter and the mixing of nonpolar flavor matter, formula rate is 1000: 0.1 ~ 5.
As preferably, described polarity flavor matter and the formula rate of nonpolar flavor matter are 1000: 2 ~ 3.
As preferably, described tobacco material is one or more mixing in offal, cigarette ash, tobacco fragment, offal or other tobacco wastes that the particle that produces in tobacco leaf, pipe tobacco or tobacco processing course is tiny.
The present invention be some deficiency is mainly manifested in the modulation of reconstituted tobacco and tobacco extract thereof composition on carry out suitable supplementing, and total and natural baccy has gap for the modulation way of the component of this perfume (or spice) of tobacco.The present invention adopts water extraction and supercritical CO by a kind of
2extraction process is the method for endogenous flavor matter and the application in tobacco product perfuming thereof in directed compound collecting tobacco from tobacco, comprises and adopts water extraction directed extraction polarity flavor matter and supercritical CO from tobacco
2extraction process is the directed composite extracting method extracting nonpolar flavor matter from tobacco, according to a certain percentage polarity flavor matter and nonpolar flavor matter are allocated again, then its composite spices that causes is added in the tobacco products such as reconstituted tobacco, promote the quality of the tobacco products such as reconstituted tobacco, increase perfume quantity, carry raise note, to set off nature cigarette fragrant, reduce flue gas drying sense, enhancing flue gas promotes the production of body fluid sense, improve cigarette comfort level, reaches the object of flavouring humectation.
The present invention has following beneficial effect:
1. tobacco material used herein is offal, cigarette ash or the offal the like waste that the particle that produces in tobacco leaf, pipe tobacco or tobacco processing course is tiny, and " turning waste into wealth " decreases the pollution to environment;
2. the present invention is by water extraction and supercritical CO
2the method of the directed compound collecting flavor matter of extraction process, directed compound ground extracts tobacco endogenous flavor matter from tobacco;
3. the present invention passes through tobacco water extracting liquid and tobacco supercritical CO
2extract carries out suitably than allotment, its composite spices that causes is sprayed in reconstituted tobacco, promotes the quality of reconstituted tobacco, increase perfume quantity, carry raise note, to set off nature cigarette fragrant, reduce flue gas drying sense, strengthen flue gas and to promote the production of body fluid sense, raising cigarette comfort level.
Accompanying drawing explanation
Fig. 1 is supercritical CO
2extract GC-MS analysis chart.
Fig. 2 is water extracting liquid GC-MS analysis chart.
Embodiment
As previously mentioned, according to content disclosed above, one of skill in the art can apply the present invention to greatest extent.It should be pointed out that the present invention aims to provide a directed composite extracting method and uses thereof growing tobacco middle flavor matter.After following embodiment part provides directed composite extracting method being enough to confirm flavor matter in described tobacco and uses thereof, those skilled in the art are according to the routine techniques of perfuming cigarette purposes, can expect the directed composite extracting method of flavor matter in tobacco of the present invention completely can be used in above-mentioned field and can expectation function be realized, therefore the following examples can help the present invention of those skilled in the art's comprehend, but do not limit the present invention in any way.
embodiment 1:
Get useless time 40 DEG C, cigarette ash 40kg 280L water and stir extraction 1 hour, filter, it is 1.2g/mL that extracting solution is concentrated into density, gets water extracting liquid 10000g, is added in 10kg reconstituted tobacco substrate, sample sets in contrast.
embodiment 2:
Get useless time 50 DEG C, cigarette ash 40kg 200L water and stir extraction 1 hour, filter, it is 1.2g/mL that extracting solution is concentrated into density, and water extracting liquid is for subsequent use; Get waster tobacco 3kg supercritical CO
2extract, extraction conditions is extraction kettle pressure is 25MPa, and extraction temperature is 40 DEG C, CO
2flow is 200L/ hour, and extraction time is 4 hours; Separating still pressure is 5MPa, and separation temperature is 45 DEG C, obtains 115g extract after extraction; Get water extracting liquid 10000g and supercritical CO
2extraction 30g, both are added in 10kg reconstituted tobacco substrate after mixing, by sensory evaluating smoking, compared with control sample group fragrance texture, perfume quantity comparatively control sample promote all to some extent, tobacco aroma performance more clear, more naturally.Stimulation, clean level slightly decline, and moisture feeling keeps good.
embodiment 3:
Get useless time 40 DEG C, cigarette ash 40kg 200L water and stir extraction 1 hour, extract 2 times, filter, it is 1.1g/mL that extracting solution is concentrated into density, and water extracting liquid is for subsequent use; Get useless time cigarette ash 6kg supercritical CO
2extract, extraction conditions is extraction kettle pressure is 20MPa, and extraction temperature is 35 DEG C, CO
2flow is 180L/ hour, and extraction time is 3 hours; Separating still pressure is 5.5MPa, and separation temperature is 40 DEG C, obtains 265g extract after extraction; Get water extracting liquid 10000g and supercritical CO
2extraction 20g, both are added into after mixing in 10kg reconstituted tobacco substrate, pass through sensory evaluating smoking, compared with control sample group fragrance texture, perfume quantity comparatively control sample promote all to some extent, cigarette perfume (or spice) is sent out more thoroughly, fuller, sweet sense some manifest, stimulate, clean level slightly decline.
embodiment 4:
Get useless time 70 DEG C, cigarette ash 30kg 210L water and stir extraction 1 hour, extract 2 times, filter, it is 1.2g/mL that extracting solution is concentrated into density, gets 70 DEG C, 10kg offal 45L water and extracts 1 hour, filter, it is 1.22g/mL that extracting solution is concentrated into density, then merges for subsequent use by cigarette ash and offal concentrated solution; Get useless time cigarette ash 7kg supercritical CO
2extract, extraction conditions is extraction kettle pressure is 30MPa, and extraction temperature is 45 DEG C, CO
2flow is 180L/ hour, and extraction time is 3.5 hours; Separating still pressure is 6.5MPa, and separation temperature is 45 DEG C, obtains 315g extract after extraction; Get cigarette ash and offal water extracting liquid 10000g and supercritical CO
2extraction 50g, both are added into after mixing in 10kg reconstituted tobacco substrate, pass through sensory evaluating smoking, compared with control sample group fragrance texture, perfume quantity comparatively control sample promote all to some extent, cigarette perfume (or spice) is sent out more thoroughly, fuller, sweet sense some manifest, stimulate, clean level slightly decline.
embodiment 5:
Get 60 DEG C, waster tobacco 40kg 320L water and stir extraction 2 hours, extract 2 times, filter, it is 1.2g/mL that extracting solution is concentrated into density, and concentrated solution is for subsequent use; Get waster tobacco 4kg supercritical CO
2extract, extraction conditions is extraction kettle pressure is 25MPa, and extraction temperature is 40 DEG C, CO
2flow is 180L/ hour, and extraction time is 4 hours; Separating still pressure is 5.5MPa, and separation temperature is 35 DEG C, obtains 215g extract after extraction; Get cigarette ash and offal water extracting liquid 10000g and supercritical CO
2extraction 40g, both are added into after mixing in 10kg reconstituted tobacco substrate, pass through sensory evaluating smoking, compared with control sample group fragrance texture, perfume quantity comparatively control sample all obviously promote, cigarette perfume (or spice) is sent out more thoroughly, fuller, sweet sense is more remarkable, stimulates, clean level declines.
embodiment 6:
Supercritical CO
2extract GC-MS analyzes: get 2mL sample and 4mL dichloromethane extraction, and vibration, ultrasonic, stratification, takes off the stillness of night, and 5000rpm is centrifugal, membrane filtration, gets 1ml sample introduction.Instrument: AgilentGC/MS, its gas chromatogram as shown in Figure 1.
In supercritical extraction sample, aroma component content is as following table:
Containing a large amount of tobacco flavor matter in supercritical extract, wherein the component content such as organic acid, ketone, ester class, alcohols is higher.
embodiment 7:
Water extracting liquid GC-MS analyzes: get 2mL sample and 4mL dichloromethane extraction, and vibration, ultrasonic, stratification, takes off the stillness of night, and 5000rpm is centrifugal, membrane filtration, gets 1ml sample introduction.Instrument: AgilentGC/MS, its gas chromatogram is as Fig. 2.From GC-MS collection of illustrative plates, in water extracting liquid, volatile aroma component content is extremely low.
Claims (1)
1. a water extraction and supercritical CO
2extraction process method of flavor matter in directed compound collecting tobacco from tobacco material, it is characterized in that the method comprises the following steps: that getting useless time 40 DEG C, cigarette ash 40kg 200L water stirs extraction 1 hour, extracts 2 times, filters, it is 1.1g/mL that extracting solution is concentrated into density, and water extracting liquid is for subsequent use; Get useless time cigarette ash 6kg supercritical CO
2extract, extraction conditions is extraction kettle pressure is 20MPa, and extraction temperature is 35 DEG C, CO
2flow is 180L/ hour, and extraction time is 3 hours; Separating still pressure is 5.5MPa, and separation temperature is 40 DEG C, obtains 265g extract after extraction; Get water extracting liquid 10000g and supercritical CO
2extraction 20g, both mix.
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| CN104450186B (en) * | 2014-10-29 | 2017-04-19 | 山东中烟工业有限责任公司 | Method for preparing tobacco herbal fragrant substance for cigarette solution of electronic cigarette |
| CN104585863B (en) * | 2015-01-20 | 2016-08-24 | 川渝中烟工业有限责任公司 | A kind of tobacco juice for electronic smoke |
| CN106124679A (en) * | 2016-07-06 | 2016-11-16 | 云南中烟工业有限责任公司 | One assay method growing tobacco middle group compounds of aldehydes and ketones |
| GB201707758D0 (en) | 2017-05-15 | 2017-06-28 | British American Tobacco Investments Ltd | Ground tobacco composition |
| JP7374935B2 (en) | 2018-06-29 | 2023-11-07 | インペリアル タバコ リミテッド | Method of producing reconstituted plant material |
| GB201810729D0 (en) | 2018-06-29 | 2018-08-15 | Nerudia Ltd | A method for manufacturing reconstituted plant material |
| CN113638265B (en) * | 2020-05-11 | 2022-12-27 | 中国烟草总公司郑州烟草研究院 | Cigarette flavor for cigarette paper coating liquid and application thereof, cigarette paper coating liquid and cigarette |
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