CN103478892B - This Studies of The Aromatic Substances in the tobacco of water extraction and ethanol extraction method directed compound collecting from tobacco material - Google Patents
This Studies of The Aromatic Substances in the tobacco of water extraction and ethanol extraction method directed compound collecting from tobacco material Download PDFInfo
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Abstract
The present invention relates to this Studies of The Aromatic Substances in the tobacco of a kind of water extraction and ethanol extraction method directed compound collecting from tobacco material, this material to be mixed with the Semi-polarity of alcohol extract and weak level flavor matter by the polarity flavor matter of water extraction and forms, and described polarity flavor matter and Semi-polarity and weak level flavor matter fill a prescription 100: 0.1 ~ 5 according to mass ratio.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 is by carrying out proper proportion allotment to tobacco water extracting liquid and alcohol extract concentrate, its composite spices that causes is added in the tobacco products such as reconstituted tobacco, promote organoleptic quality, increase perfume quantity, carry raise note, to set off nature cigarette fragrant, reduce flue gas drying sense, strengthen flue gas promote the production of body fluid sense, improve and aspirate comfort level.
Description
Technical field
The present invention relates to Field of Tobacco, particularly relate to one grow tobacco middle Studies of The Aromatic Substances directed compound collecting tobacco in this Studies of The Aromatic Substances.
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 leftover bits and pieces such as the waster tobacco of about 25 % can be produced in production process can not use at the Bian of tobacco, regarded garbage disposal 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 leftover bits and pieces such as waster tobacco.Reconstituted tobacco, also known as making reconstituted tobacoo, 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 natural tobacco thin slice of function admirable, as cigarette filler, be back to production of cigarettes.
Reconstituted tobacco can lose a part of this Studies of The Aromatic Substances of tobacco in process, 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, damascenone, geranyl acetone, Megastigmatrienone, alpha, beta-lonone, benzaldehyde, phenmethylol, dihydroactinidiolide in waster tobacco, illustrate containing a large amount of important aroma components of tobacco in waster tobacco, can as the source of tobacco essence.
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 the organic acid of a large amount of Semi-polarity and low pole, terpenes, alcohols in tobacco adopts its extraction effect of water extraction often poor, and the reconstituted tobacco only adding water extracting liquid still exists the shortcoming of fragrance deficiency.
Ethanol is conventional organic solvent, nontoxic, very extensive in field application such as chemical industry, medicine, biologies.Ethanol has good dissolubility for the material of Semi-polarity and low pole.Be Semi-polarity or low pole compound mostly in fragrance ingredient in tobacco, solubility is in ethanol very large, is thus particularly suitable for adopting alcohol extract.With ethanol extraction method extracted tobacco flavor matter from tobacco, extract the important aroma component contained in the essential oil that obtains all obtains much bigger than the extraction of traditional water extraction 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 carry out analysiss discovery wherein mainly Semi-polarity and low pole compound to the product that alcohol extract obtains, 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, molecularly distilled etc.Its document and Patent as follows:
The pertinent literature of the extraction of current tobacco mainly concentrates on essential oil of tobaccos, alkaloid and Salanesol etc.Gao Hongjian etc. (2011) are studied the technique that steam distillation extracts essential oil of tobaccos.Experiment for index with essential oil of tobaccos yield, is investigated distillation time, solid-liquid ratio, NaCl concentration, soak time four factor extract essential oil of tobaccos yield impact on steam distillation, is optimized by experiment of single factor and orthogonal experiment to extraction process.Yang Jun etc. (2012) study the technique that ultrasonic-assistant solvent method extracts essential oil of tobaccos crude extract. with essential oil of tobaccos crude extract yield for index, investigate ultrasonic time, ultrasonic power, solid-liquid ratio, soak time 4 factors and reciprocation thereof extract essential oil of tobaccos crude extract yield impact and optimum process condition on ultrasonic-assistant solvent method.Liang Jinfeng etc. take low-class tobacco as a kind of method that rapid extraction nicotine set up by raw material, adopt supercritical ultrasonics technology, the way of distillation and Nicotine Extraction with Microwave, spectrophotometer method is utilized to measure nicotine content, be have studied the impact of different ethanol concentration, different time, different feed liquid comparison tobacco smoke alkaloid extracted amount by single factor experiment respectively, compare the pluses and minuses of three kinds of extraction methods simultaneously.The different test method of Liu Wei etc. (2011) has investigated three kinds of extracting methods respectively, and measures the content of Salanesol with RP-HPLC method for inspection target, optimizes optimum extraction process; Result shows Salanesol optimum extraction process in tobacco extract: potassium hydroxide methanol solution extracts acetone cold-maceration.
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 aqueous medium doubly, regulate pH value to 9-13, and carry out ultrasonic pretreatment, ultrasonic power is no less than 20kHz, ultrasonic pretreatment time is no less than 20 minutes, obtains ultrasonic pretreatment fluid, further extraction nicotine, hemicellulose, lignin, cellulose.Although the method extraction of 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 extraction of 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, be concentrated into relative density 1.00-1.30 again and control temperature is 20 ~ 40 DEG C, obtain tobacco and extract concentrate or tobacco extract, then β-cyclodextrin in mass ratio: flavouring essence for tobacco is 1 ~ 3:1, flavouring essence for tobacco and β-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 concentrate co-spray and obtain tobacco spray dried 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-schardinger dextrin-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 wave extraction, filtration, chromatographic column separation, reduced pressure concentration step; The ethanol of described tobacco extract concentration 80% dissolves, and 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 extracted becomes single, is not well positioned to meet the mouthfeel demand of reproducing pipe tobacco.
Summary of the invention
In order to solve above-mentioned technical problem, the present invention seeks to this Studies of The Aromatic Substances in the tobacco of a kind of water extraction and ethanol extraction method directed compound collecting from tobacco material.This Studies of The Aromatic Substances of the present invention 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.
In order to realize above-mentioned object, present invention employs following technical scheme:
This Studies of The Aromatic Substances in the tobacco of a kind of water extraction and ethanol extraction method directed compound collecting from tobacco material, this material to be mixed with the Semi-polarity of alcohol extract and weak level flavor matter by the polarity flavor matter of water extraction and forms, and described polarity flavor matter and Semi-polarity and weak level flavor matter fill a prescription 100: 0.1 ~ 5 according to mass ratio.
As preferably, described polarity flavor matter and Semi-polarity and weak level flavor matter fill a prescription 100: 2 ~ 3 according to mass ratio.
As preferably, the preparation method of the polarity flavor matter of described water extraction is as follows: water extraction, and tobacco material 3 ~ 9 times of water gagings 30 ~ 70 DEG C extract 0.5 ~ 2 hour, and extract 1 ~ 3 time, it is 1.1 ~ 1.3g/mL that extract is concentrated into density.
As preferably, the Semi-polarity of described alcohol extract and the preparation method of weak level flavor matter as follows: in ethanol extraction method, concentration of alcohol is 60% ~ 90%, ethanol consumption is 4 ~ 8 times amount, Extracting temperature is 40 ~ 70 DEG C, extraction time is 1 ~ 2 hour, extract 1 ~ 2 time, it is 1.1 ~ 1.3 mg/mL that extract is concentrated into density.
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.
In view of at present, the composition modulation of reconstituted tobacco and tobacco extract thereof being mainly manifested in some deficiency carries out suitable supplementing, and total and natural baccy there is gap for the modulation way of the component of this perfume (or spice) of tobacco.The present invention adopts the method for endogenous flavor matter and the application in tobacco product perfuming thereof in directed compound collecting tobacco from tobacco of water extraction and ethanol extraction method by a kind of, comprise and adopt water extraction directed extraction polarity flavor matter and ethanol extraction method directed extraction Semi-polarity from tobacco from tobacco, the composite extracting method of low pole flavor matter, again according to a certain percentage by polarity flavor matter and Semi-polarity, low pole flavor matter is allocated, then its composite spices that causes is sprayed in reconstituted tobacco, promote the quality of reconstituted tobacco, increase perfume quantity, carry and raise note, set off nature cigarette fragrant, reduce flue gas drying sense, strengthen flue gas to promote the production of body fluid sense, improve cigarette comfort level.
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 the method for the directed compound collecting flavor matter of water extraction and ethanol extraction method, and directed compound ground extracts tobacco endogenous flavor matter from tobacco;
3. the present invention is by carrying out proper proportion allotment to tobacco water extracting liquid and alcohol extract concentrate, its composite spices that causes is added in the tobacco products such as reconstituted tobacco, promote organoleptic quality, increase perfume quantity, carry raise note, to set off nature cigarette fragrant, reduce flue gas drying sense, strengthen flue gas promote the production of body fluid sense, improve and aspirate comfort level.
Accompanying drawing explanation
Fig. 1 is 80% alcohol extract concentrate GC-MS analysis chart.
Fig. 2 is water extracting liquid GC-MS analysis chart.
Detailed description of the invention
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 detailed description of the invention 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 0:
Get useless time 40 DEG C, cigarette ash 40kg 280L water and stir extraction 1 hour, filter, it is 1.2g/mL that extract is concentrated into density, gets water extracting liquid 10000 g, is added in 10 kg reconstituted tobacco substrates, sample sets in contrast.
Embodiment 1:
Get useless time 50 DEG C, cigarette ash 40kg 200L water and stir extraction 1 hour, filter, it is 1.2g/mL that extract is concentrated into density, and water extracting liquid is for subsequent use; Get useless time cigarette ash 10kg 40L80% ethanol 50 DEG C, extraction time is 2 hours, and extract 2 times, it is 1.2 g/mL that extract is concentrated into density; Get water extracting liquid 10000 g and alcohol extract concentrate 300 g, both are added in 10 kg reconstituted tobaccos after mixing, pass through sensory evaluating smoking, compared with control sample group fragrance thoroughly degree of sending out, bright feel slightly good, show slightly some fragrant and sweet senses, flue gas has certain continuous sense, and concentration is medium+, there is superficial puncture in oral cavity, the slightly puckery mouth of pleasant impression.
Embodiment 2:
Get useless time 40 DEG C, cigarette ash 40kg 200L water and stir extraction 1 hour, extract 2 times, filter, it is 1.2g/mL that extract is concentrated into density, and water extracting liquid is for subsequent use; Get useless time cigarette ash 10kg 80L60% ethanol 70 DEG C, extraction time is 1 hour, and extract 1 time, it is 1.2 g/mL that extract is concentrated into density; Get water extracting liquid 10000 g and alcohol extract concentrate 200 g, both are added in 10 kg reconstituted tobaccos after mixing, pass through sensory evaluating smoking, the saturating Fa Dulve of fragrance is good compared with control sample group, flue gas concentration is medium+, still fine and smooth, still agglomerating, there is superficial puncture in oral cavity, show slightly xylon gas, the slightly puckery mouth of pleasant impression.
Embodiment 3:
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 extract is concentrated into density, gets 70 DEG C, 10kg offal 45L water and extracts 1 hour, filter, it is 1.2g/mL that extract is concentrated into density, then merges for subsequent use by cigarette ash and offal concentrate; Get waster tobacco 10kg 60L90% ethanol 70 DEG C, extraction time is 2 hours, and extract 2 times, it is 1.1 g/mL that extract is concentrated into density; Get water extracting liquid 10000 g and alcohol extract concentrate 300 g, both are added into after mixing in 10 kg reconstituted tobaccos, pass through sensory evaluating smoking, fragrance is sent out still thoroughly compared with control sample group, still bright, fragrant and sweetly slightly to manifest, have certain abundant sense, the still soft exquisiteness of flue gas, oral cavity is superficial puncture slightly, and assorted gas shows slightly, the slightly stagnant tongue of pleasant impression, slightly residual, show slightly sweet.
Embodiment 4:
Get 60 DEG C, waster tobacco 40kg 320L water and stir extraction 2 hours, extract 2 times, filter, it is 1.2g/mL that extract is concentrated into density, and concentrate is for subsequent use; Get useless time cigarette ash 10kg 70L60% ethanol 70 DEG C, extraction time is 1.5 hours, and extract 2 times, it is 1.2 g/mL that extract is concentrated into density; Get water extracting liquid 10000 g and alcohol extract concentrate 500 g, both are added into after mixing in 10 kg reconstituted tobaccos, pass through sensory evaluating smoking, fragrance is sent out thoroughly compared with control sample group, bright, fragrant and sweetly slightly to manifest, have certain abundant sense, the still soft exquisiteness of flue gas, oral cavity is superficial puncture slightly, and assorted gas shows slightly, the slightly stagnant tongue of pleasant impression, slightly residual, show slightly sweet.
Embodiment 5:
80% alcohol extract concentrate 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: Agilent GC/MS, its gas chromatogram as shown in Figure 1.
In 80% ethanol sample, aroma component content is as following table:
Containing a large amount of tobacco flavor matter in alcohol extract concentrate, wherein the component content such as organic acid, ketone, ester class, alcohols is higher.
Embodiment 6:
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: Agilent GC/MS, its gas chromatogram as shown in Figure 2.From GC-MS collection of illustrative plates, in water extracting liquid, volatile aroma component content is extremely low.
Claims (1)
1. this Studies of The Aromatic Substances in the tobacco of a water extraction and ethanol extraction method directed compound collecting from tobacco material, it is characterized in that the preparation method of this this Studies of The Aromatic Substances is as follows: get 60 DEG C, waster tobacco 40kg 320L water and stir extraction 2 hours, extract 2 times, filter, it is 1.2g/mL that extract is concentrated into density, and concentrate is for subsequent use; Get useless time cigarette ash 10kg 70L60% ethanol 70 DEG C, extraction time is 1.5 hours, and extract 2 times, it is 1.2 g/mL that extract is concentrated into density; Get water extracting liquid 10000 g and alcohol extract concentrate 500 g, both mix.
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| 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 |
| CN109090683A (en) * | 2018-07-19 | 2018-12-28 | 中烟施伟策（云南）再造烟叶有限公司 | A kind of preparation method of high-nicotine type reconstituted tobacco |
| CN111363625A (en) * | 2018-12-25 | 2020-07-03 | 广州华芳烟用香精有限公司 | Preparation method of composite tobacco extract with fragrance styles of pericarpium citri reticulatae and pummelo peel and application of composite tobacco extract in cigarettes |
| CN115399498B (en) * | 2022-08-29 | 2023-06-27 | 河北中烟工业有限责任公司 | Tobacco extract, preparation method thereof and tobacco product |
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| CN103462205B (en) * | 2013-09-18 | 2015-06-03 | 浙江中烟工业有限责任公司 | Reconstructed tobacco leaves containing basic incense substances in tobaccos prepared by water extraction method and ethanol extraction method and cigarettes produced by reconstructed tobacco leaves |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1565286A (en) * | 2003-06-13 | 2005-01-19 | 广东省金叶烟草薄片技术开发有限公司 | Tobacco leaf remaking process using tobacco peduncle and tobacco fragment as material through paper making method |
| CN101708063A (en) * | 2009-12-23 | 2010-05-19 | 湖南中烟工业有限责任公司 | Method for concentrating extraction liquid in production of tobacco sheet by papermaking process |
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