CN102586019A - Preparation method and application of neutral aroma components in grain phase of smoke of high-quality tobacco leaves - Google Patents
Preparation method and application of neutral aroma components in grain phase of smoke of high-quality tobacco leaves Download PDFInfo
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- CN102586019A CN102586019A CN2012100403323A CN201210040332A CN102586019A CN 102586019 A CN102586019 A CN 102586019A CN 2012100403323 A CN2012100403323 A CN 2012100403323A CN 201210040332 A CN201210040332 A CN 201210040332A CN 102586019 A CN102586019 A CN 102586019A
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Abstract
The invention belongs to the field of separation and preparation of tobacco flavors and fragrances, and in particular relates to a preparation method and application of neutral aroma components in a grain phase of smoke of high-quality tobacco leaves. High-quality unblended tobacco leaves are taken as raw materials, a condensation product of the grain phase of the smoke is collected, the condensation product of the grain phase is subjected to extraction, acid washing, alkali washing and the like to form a neutral component, the neutral component is subjected to normal-phase silicagel column chromatographic separation, 28 elution fractions are obtained, and the neutral aroma components D6, D17, D18 and D25 can be obtained. Different aromatic fractions are added into cut tobacco of cigarettes to improve the smoke quality of the cigarettes at different angles. By separating the grain phase of the smoke of the high-quality cigarettes, the aroma characteristics and aroma compensation effects of crucial aroma components are defined, and technical support is provided for reducing tar and enhancing aroma and maintaining moisture of cigarettes of other brands.
Description
Technical field
The invention belongs to separation, the preparation field of essence spice for cigarette, be specifically related to a kind of preparation method and application of sound tobacco flue gas granule phase substance neutral flavor composition.
Background technology
Along with the increasing of domestic tobacco industry reducing tar and reducing harm dynamics, to the also lifting day by day of requirement of Chinese style cigarette (especially low tar Chinese style cigarette) compensating aroma technology.In addition; What cigarette added at present all is food flavor(ing) spices; But along with requirement progressively standard and the strictness of health ministry to the interpolation of food flavor(ing) spices; Grain, fruit, fishery products, milk preparation etc. are all advocated and are not added essence and flavoring agent as far as possible, thus the tobacco flavor compensation technique have also been proposed a bigger difficult problem, and the compensating aroma technology has become the research content and the direction of Chinese style cigarette.
Neutral flavor material in the flue gas is the important chemical composition that influences the cigarette quality.Research to cigarette mainstream flue gas neutral flavor composition; Can the most directly understand and organoleptic effect between mutual relationship; Thereby design provides important information with tobacco leaf formulation for cigarette flavoring is reinforced; For the inner quality that improves the Chinese style cigarette is laid reliable theoretical basis, for production practice provide more wide application prospect.
The cigarette smoke composition is of a great variety, and composition of nowadays identifying in the flue gas and kind have reached 7357 kinds, and wherein oxygenatedchemicals just has 3568 kinds, so composition identifies that operation irregularity is complicated.In addition, most of material is trace components heng in the flue gas, has further increased the difficulty of smoke components separation, preparation.
Summary of the invention
The flavour ingredient that the present invention itself has with the high-quality cigarette smoke is an origin, from sound tobacco flue gas granule phase substance, separates making the flavor matter that flue gas itself possesses, thereby obtains natural flavouring essence for tobacco.Such essence comes from smoke of tobacco self, from natural tobacco leaf flue gas granule phase substance, extracts, and has avoided adding compound essence spices and has added caused variety of issue in the cigarette.
An object of the present invention is to provide the preparation method of neutral flavor composition in a kind of sound tobacco flue gas granule phase substance.
Another object of the present invention provides the application of neutral flavor composition in the said sound tobacco flue gas granule phase substance.
To achieve these goals, the present invention adopts following technical scheme to realize:
The preparation method of neutral flavor composition in a kind of sound tobacco flue gas granule phase substance; Said neutral flavor composition is a raw material with sound tobacco flue gas granule phase substance; Obtain the neutral compound of flue gas granule phase substance successively through extraction, pickling and alkali cleaning step, the neutral compound with the flue gas granule phase substance that obtains makes through the normal phase silica gel column chromatography separation again.
Preferable, said neutral flavor composition is for separating a cut among D6, D17, D18 and the D25 among 28 eluting fraction D1-D28 that make through normal phase silica gel column chromatography.
Preferable, the preparation method of neutral flavor composition specifically comprises the steps: in the said sound tobacco flue gas granule phase substance
(1) extracts: on rotary smoking machine, adopt filter disc to capture mode, collect sound tobacco flue gas granule phase substance, obtain the cambridge filter ravin with cambridge filter; After the cambridge filter ravin employing extraction liquid extraction that obtains, concentrating under reduced pressure obtains the liquid concentrator S1 of Vandyke brown crude extract;
Preferable, said extraction liquid is an ether.Further, the liquid concentrator S1 of said Vandyke brown crude extract is the diethyl ether solution of Vandyke brown crude extract.
Preferable, the method for said extraction is for soaking one or more methods in extraction, ultrasonic extraction and the shaking table oscillation extraction; The vacuum tightness of said concentrating under reduced pressure is 500-1000mbar, and the bath temperature that concentrating under reduced pressure adopted is 25-60 ℃.
(2) pickling: the liquid concentrator S1 of the Vandyke brown crude extract that step (1) is obtained adopts sour water to extract, and extraction repeatedly separates organic phase and water respectively, obtains organic phase extract S2;
Preferable, said sour water is hydrochloric acid soln or sulphuric acid soln.Further, the mass percent concentration of acid is 1-10% in said hydrochloric acid soln or the sulphuric acid soln.Preferably, the mass percent concentration of acid is 5% in said hydrochloric acid soln or the sulphuric acid soln.
(3) alkali cleaning: the organic phase extract S2 that step (2) is obtained adopts alkali lye to extract; Extraction repeatedly respectively; Separate organic phase and water, the organic phase after the alkali cleaning is carried out obtaining organic phase extract S3 behind the concentrating under reduced pressure, be the neutral compound of flue gas granule phase substance;
Preferable, said alkali lye is sodium hydroxide solution.Further, the mass percent concentration of sodium hydroxide is 1-10% in the said sodium hydroxide solution.Preferably, the mass percent concentration of sodium hydroxide is 5% in the said sodium hydroxide solution.
Preferable, in the step (3), the vacuum tightness of said concentrating under reduced pressure is 500-1000mbar, the bath temperature that concentrating under reduced pressure adopted is 25-60 ℃.
Extraction in above-mentioned steps (2) and the step (3) repeatedly, as all being 3 times.
(4) normal phase silica gel column chromatography separates: adopt normal phase silicagel column that the organic phase extract S3 that step (3) obtains is carried out gradient elution; Organic phase extract S3 is when column chromatography for separation; Obtain 28 wash-out fraction D1-D28 by the equal-volume collection, D6, D17, D18 and D25 among 28 wash-out fraction D1-D28 are removed the back of desolvating respectively obtain said neutral flavor composition; Wherein gradient elution adopts the gradient elution agent that polarity increases gradually.
Preferable, in the step (4), the diameter of said normal phase silicagel column is 2.3cm; The weight of the corresponding filling gel of the organic phase extract S3 of every 0.5mL is 20g.
Preferable, in the step (4), when carrying out gradient elution, normal hexane, ether and ethanol are selected in the gradient elution agent that polarity increases gradually for use; When selecting normal hexane, ether and ethanol for use; The employing volume ratio is 100: 0 normal hexane and an ether earlier; Being increased to volume ratio gradually through polarity is 0: 100 normal hexane and ether; Adopting volume ratio again is 100: 0 ether and ethanol, and being increased to volume ratio gradually through polarity is 0: 100 ether and ethanol;
Perhaps, in the step (4), when carrying out gradient elution, Skellysolve A, ether and methyl alcohol are selected in the gradient elution agent that polarity increases gradually for use; When selecting Skellysolve A, ether and methyl alcohol for use; The employing volume ratio is 100: 0 Skellysolve A and an ether earlier; Being increased to volume ratio gradually through polarity is 0: 100 Skellysolve A and ether; Adopting volume ratio again is 100: 0 ether and methyl alcohol, and being increased to volume ratio gradually through polarity is 0: 100 ether and methyl alcohol.
The gradient elution agent that polarity of the present invention increases gradually selects for use in normal hexane, ether and the ethanol " adopting volume ratio earlier is 100: 0 normal hexane and ether; being increased to volume ratio gradually through polarity is 0: 100 normal hexane and ether; adopting volume ratio again is 100: 0 ether and ethanol; being increased to volume ratio gradually through polarity is 0: 100 ether and ethanol " to be meant to adopt earlier 100% normal hexane to carry out wash-out; The amount that in 100% normal hexane, increases ether then gradually increases the polarity of eluent; Be increased to 100% ether, being employed in 100% the ether increases the polarity that the alcoholic acid amount increases eluent gradually again always, till being increased to 100% ethanol.
Further; When carrying out gradient elution, the elutriant of following polarity and volume is adopted in the gradient elution agent successively: volume ratio is 100: 0 normal hexane and ether 100ml, and volume ratio is 99: 1 normal hexane and ether 100ml; Volume ratio is 98: 2 normal hexane and ether 150ml; Volume ratio is 95: 5 normal hexane and ether 250ml, and volume ratio is 90: 10 normal hexane and ether 100ml, and volume ratio is 80: 20 normal hexane and ether 200ml; Volume ratio is 50: 50 normal hexane and ether 200ml; Volume ratio is 0: 100 normal hexane and ether 100ml, and volume ratio is 100: 0 ether and ethanol 100ml, and volume ratio is 0: 100 ether and ethanol 100ml;
Perhaps, when carrying out gradient elution, the elutriant of following polarity and volume is adopted in the gradient elution agent successively: volume ratio is 100: 0 Skellysolve A and ether 100ml; Volume ratio is 99: 1 Skellysolve A and ether 100ml, and volume ratio is 98: 2 Skellysolve A and ether 150ml, and volume ratio is 95: 5 Skellysolve A and ether 250ml; Volume ratio is 90: 10 Skellysolve A and ether 100ml; Volume ratio is 80: 20 Skellysolve A and ether 200ml, and volume ratio is 50: 50 Skellysolve A and ether 200ml, and volume ratio is 0: 100 Skellysolve A and ether 100ml; Volume ratio is 100: 0 ether and methyl alcohol 100ml, and volume ratio is 0: 100 ether and methyl alcohol 100ml.
In the above-mentioned steps (4); When carrying out gradient elution, the gradient elution agent that polarity increases gradually can also replace with Skellysolve A with normal hexane when selecting normal hexane, ether and ethanol for use, promptly selects Skellysolve A, ether and ethanol for use; Also can ethanol be replaced with methyl alcohol, promptly select normal hexane, ether and methyl alcohol for use.
Preferable, the said collection by equal-volume obtains among 28 wash-out fraction D1-D28, and every equal-volume is 50ml.
Preferable, in the step (4), the said collection by equal-volume obtains when the gradient elution agent begins to flow out, beginning to collect among 28 wash-out fraction D1-D28.
In the step of the present invention (4), collecting 28 wash-out fraction D1-D28 is to collect first cut D1, second cut D2, the 3rd cut D3 successively ..., the 27th cut D27, the 28 cut D28.
Neutral flavor composition of the present invention adopts ethanol to dissolve, and the ethanolic soln of the neutral flavor composition after the dissolving is smoked panel test, and can know that through smokeing panel test different neutral flavor cuts can promote the flue gas quality of cigarette from different perspectives.
The neutral flavor composition is to obtain through above-mentioned preparation method in the sound tobacco flue gas granule phase substance of the present invention.
Neutral flavor composition and preparation method thereof can be widely used in preparing in cigarette shreds or the mouth rod perfuming field in the sound tobacco flue gas granule phase substance of the present invention.
Outstanding advantage of the present invention is:
The present invention is that feedstock production obtains different neutral flavor cuts with sound tobacco flue gas granule phase substance, also can be described as different neutral flavor compositions, the lifting that various neutral flavor cuts have different angles and degree to the suction flavor and the quality of cigarette.The crucial neutral cut with high-quality cigarette smoke style and features of the prepared acquisition of the present invention; Add the style and features that various neutral flavor compositions can bring the pairing high-quality cigarette of each neutral flavor composition through smokeing panel test; For the compensation technique of essence spice for cigarette provides technical support and guarantee; Promoted the development of low-coke tar cigarette, promoted the obvious lifting of cigarette product interior quality simultaneously, on brand cigarette, be more widely used.Present device is simple, and is easy to operate, is convenient to promote.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment only are used to the present invention is described and are not used in restriction protection scope of the present invention.
Embodiment 1
The preparation of neutral flavor composition in the sound tobacco flue gas granule phase substance:
(1) extracts: on rotary smoking machine, adopt filter disc to capture mode, collect sound tobacco flue gas granule phase substance, obtain the cambridge filter ravin with cambridge filter (diameter is 92mm, and every cambridge filter is collected 20 cigarette smoke granule phase substances); 30 cambridge filter ravin that capture high-quality cigarette smoke granule phase substance are used earlier the ether soaking and extracting, and behind the supersound extraction 5min, 30min is extracted in the shaking table vibration again, places and repeats to extract one time after one day again, obtains extracting solution then.With the liquid concentrator S1 that obtains the Vandyke brown crude extract behind the extracting solution concentrating under reduced pressure that obtains; Wherein, the vacuum tightness of concentrating under reduced pressure is 870mbar, and bath temperature is 36 ℃.
(2) pickling: the liquid concentrator S1 of Vandyke brown crude extract is transferred to separating funnel, and the use mass percent concentration is 5% H
2SO
4Aqueous solution extraction three times, each volume is 250mL.Separate organic phase and water, obtain organic phase extract S2;
(3) alkali cleaning: S2 is transferred to separating funnel with the organic phase extract, and using mass percent concentration is 5% NaOH aqueous solution extraction 3 times, and each volume is 250mL.Separate organic phase and water, the organic phase concentrating under reduced pressure after the alkali cleaning is obtained organic phase extract S3.This organic phase extract S3 is the neutral compound of flue gas granule phase substance; Wherein, the vacuum tightness of concentrating under reduced pressure is 870mbar, and bath temperature is 36 ℃.
(4) normal phase silica gel column chromatography separates: get 1/10 the about 0.5mL of organic phase extract S3; Fill normal phase silicagel column (diameter is 2.3cm) with 20g silica gel and carry out the wash-out separation; The volume ratio that the eluent gradient adopts normal hexane and ether earlier was from 100: 0 to 50: 50; By 0: 100, using ether and ethanol then instead was the gradient elution agent again, and ether and alcoholic acid volume ratio were from 100: 0 to 0: 100.When carrying out gradient elution, the elutriant of following polarity and volume is adopted in concrete gradient elution agent successively: volume ratio is 100: 0 normal hexane and ether 100ml, and volume ratio is 99: 1 normal hexane and ether 100ml; Volume ratio is 98: 2 normal hexane and ether 150ml; Volume ratio is 95: 5 normal hexane and ether 250ml, and volume ratio is 90: 10 normal hexane and ether 100ml, and volume ratio is 80: 20 normal hexane and ether 200ml; Volume ratio is 50: 50 normal hexane and ether 200ml; Volume ratio is 0: 100 normal hexane and ether 100ml, and volume ratio is 100: 0 ether and ethanol 100ml, and volume ratio is 0: 100 ether and ethanol 100ml.
Organic phase extract S3 is when column chromatography for separation;, the gradient elution agent begins to collect when beginning to flow out; Obtain 28 wash-out fraction D1-D28 by equal-volume (50mL) collection, D6, D17, D18 and D25 among 28 wash-out fraction D1-D28 are removed the back of desolvating respectively obtain neutral flavor components D 6, D17, D18 and D25.
Neutral flavor components D 6, D17, D18 and D25 dissolve with ethanol respectively once more, are made into concentration and are 2.4/milliliter solution and are used to smoke panel test.Wherein 2.4/milliliter are meant the neutral flavor composition that contains 2.4 cigarette in every milliliter of ethanol.
(5) smoke panel test: getting the cut D6 that 5 μ L collect and make an addition in the cigarette, is that the group of smokeing panel test that main body is formed goes to carry out the fragrance comparison of smokeing panel test by the expert that smokes panel test in the industry.Think through smokeing panel test and to compare with blank cigarette (not adding the cigarette of cut D6); Add this cut D6 and make cigarette smoke fine and smooth, have fruital, have the style and features of high-quality tobacco; Cut D6 has improved the quality of cigarette product, is that a key of high-quality cigarette smoke granule phase substance causes fragrant cut.
Embodiment 2
The neutral flavor components D 17 for preparing (being cut D17) the 5 μ L of embodiment 1 are made an addition to be used for cigarette in the cigarette and smoke panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D17); The cigarette cigarette that adds this cut D17 is obviously fragrant; Graceful degree improves, and passes through clearly the fragrant quality-improving of cigarette.
Embodiment 3
The neutral flavor components D 18 for preparing (being cut D18) the 5 μ L of embodiment 1 are made an addition to be used for cigarette in the cigarette and smoke panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D18); The cigarette that adds this cut D18 can set off flue-cured tobacco perfume (or spice), combines with cigarette itself to coordinate, and makes this perfume (or spice) of tobacco appear; Cigarette is fragrant to be improved, and does not feel and add thing and add.
Embodiment 4
The neutral flavor components D 25 for preparing (being cut D25) the 5 μ L of embodiment 1 are made an addition to be used for cigarette in the cigarette and smoke panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D25); Adding this cut D25 makes flue gas fragrance obvious; Have blue or green perfume, the fine and smooth convergence of flue gas, and have the effect of pressing assorted gas.
Embodiment 5
The preparation of neutral flavor composition in the sound tobacco flue gas granule phase substance:
The vacuum tightness of removing the concentrating under reduced pressure among the liquid concentrator S1 that obtains the Vandyke brown crude extract behind the extracting solution concentrating under reduced pressure that obtains is 500mbar; Bath temperature is outside 60 ℃; And the vacuum tightness of the concentrating under reduced pressure after the alkali cleaning is 500mbar; Bath temperature is outside 60 ℃, and other preparing methods are identical with embodiment 1, finally obtains neutral flavor components D 6, D17, D18 and D25.Neutral flavor components D 6, D17, D18 and D25 are dissolved with ethanol respectively once more, be made into concentration and be 2.4/milliliter solution and be used to smoke panel test.
Neutral flavor components D 6, D17, D18 and D25 that present embodiment is obtained smoke panel test:
Getting the cut D6 that 5 μ L present embodiments obtain and make an addition in the cigarette, is that the group of smokeing panel test that main body is formed goes to carry out the fragrance comparison of smokeing panel test by the expert that smokes panel test.Think through smokeing panel test and to compare with blank cigarette (not adding the cigarette of cut D6); Cut D6 makes cigarette smoke fine and smooth, has fruital, has the style and features of high-quality tobacco; Cut D6 has improved the quality of cigarette product, is that a key of high-quality cigarette smoke granule phase substance causes fragrant cut.
The neutral flavor components D 17 (being cut D17) that present embodiment is prepared is used for cigarette and smokes panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D17), the cigarette cigarette that adds this cut D17 is obviously fragrant, and graceful degree improves; Pass through clearly the fragrant quality-improving of cigarette.
The neutral flavor components D 18 (being cut D18) that present embodiment is prepared is used for cigarette and smokes panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D18); The cigarette that adds this cut D18 can set off flue-cured tobacco perfume (or spice), combines with cigarette itself to coordinate, and makes this perfume (or spice) of tobacco appear; Cigarette is fragrant to be improved, and does not feel and add thing and add.
The neutral flavor components D 25 (being cut D25) that present embodiment is prepared is used for cigarette and smokes panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D25); Adding this cut D25 makes flue gas fragrance obvious; Have blue or green perfume, the fine and smooth convergence of flue gas, and have the effect of pressing assorted gas.
Embodiment 6
The preparation of neutral flavor composition in the sound tobacco flue gas granule phase substance:
The vacuum tightness of removing the concentrating under reduced pressure among the liquid concentrator S1 that obtains the Vandyke brown crude extract behind the extracting solution concentrating under reduced pressure that obtains is 1000mbar; Bath temperature is outside 25 ℃; And the vacuum tightness of the concentrating under reduced pressure after the alkali cleaning is 1000mbar; Bath temperature is outside 25 ℃, and other preparing methods are identical with embodiment 1, finally obtains neutral flavor components D 6, D17, D18 and D25.Neutral flavor components D 6, D17, D18 and D25 are dissolved with ethanol respectively once more, be made into concentration and be 2.4/milliliter solution and be used to smoke panel test.
Neutral flavor components D 6, D17, D18 and D25 that present embodiment is obtained smoke panel test:
Getting the cut D6 that 5 μ L present embodiments obtain and make an addition in the cigarette, is that the group of smokeing panel test that main body is formed goes to carry out the fragrance comparison of smokeing panel test by the expert that smokes panel test.Think through smokeing panel test and to compare with blank cigarette (not adding the cigarette of cut D6); Add this cut D6 and make cigarette smoke fine and smooth, have fruital, have the style and features of high-quality tobacco; Cut D6 has improved the quality of cigarette product, is that a key of high-quality cigarette smoke granule phase substance causes fragrant cut.
The neutral flavor components D 17 (being cut D17) that present embodiment is prepared is used for cigarette and smokes panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D17), the cigarette cigarette that adds this cut D17 is obviously fragrant, and graceful degree improves; Pass through clearly the fragrant quality-improving of cigarette.
The neutral flavor components D 18 (being cut D18) that present embodiment is prepared is used for cigarette and smokes panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D18); The cigarette that adds this cut D18 can set off flue-cured tobacco perfume (or spice), combines with cigarette itself to coordinate, and makes this perfume (or spice) of tobacco appear; Cigarette is fragrant to be improved, and does not feel and add thing and add.
The neutral flavor components D 25 (being cut D25) that present embodiment is prepared is used for cigarette and smokes panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D25); Adding this cut D25 makes flue gas fragrance obvious; Have blue or green perfume, the fine and smooth convergence of flue gas, and have the effect of pressing assorted gas.
Embodiment 7
The preparation of neutral flavor composition in the sound tobacco flue gas granule phase substance:
Remove when carrying out gradient elution in the separation of step (4) normal phase silica gel column chromatography, the elutriant of following polarity and volume is adopted in concrete gradient elution agent successively: volume ratio is 100: 0 Skellysolve A and ether 100ml, and volume ratio is 99: 1 Skellysolve A and ether 100ml; Volume ratio is 98: 2 Skellysolve A and ether 150ml; Volume ratio is 95: 5 Skellysolve A and ether 250ml, and volume ratio is 90: 10 Skellysolve A and ether 100ml, and volume ratio is 80: 20 Skellysolve A and ether 200ml; Volume ratio is 50: 50 Skellysolve A and ether 200ml; Volume ratio is 0: 100 Skellysolve A and ether 100ml, and volume ratio is 100: 0 ether and methyl alcohol 100ml, and volume ratio is outside 0: 100 the ether and methyl alcohol 100ml; Other preparing methods are identical with embodiment 1, finally obtain neutral flavor components D 6, D17, D18 and D25.Neutral flavor components D 6, D17, D18 and D25 are dissolved with ethanol respectively once more, be made into concentration and be 2.4/milliliter solution and be used to smoke panel test.
Neutral flavor components D 6, D17, D18 and D25 that present embodiment is obtained smoke panel test:
Getting the cut D6 that 5 μ L present embodiments obtain and make an addition in the cigarette, is that the group of smokeing panel test that main body is formed goes to carry out the fragrance comparison of smokeing panel test by the expert that smokes panel test.Think through smokeing panel test and to compare with blank cigarette (not adding the cigarette of cut D6); Add this cut D6 and make cigarette smoke fine and smooth, have fruital, have the style and features of high-quality tobacco; Cut D6 has improved the quality of cigarette product, is that a key of high-quality cigarette smoke granule phase substance causes fragrant cut.
The neutral flavor components D 17 (being cut D17) that present embodiment is prepared is used for cigarette and smokes panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D17), the cigarette cigarette that adds this cut D17 is obviously fragrant, and graceful degree improves; Pass through clearly the fragrant quality-improving of cigarette.
The neutral flavor components D 18 (being cut D18) that present embodiment is prepared is used for cigarette and smokes panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D18); The cigarette that adds this cut D18 can set off flue-cured tobacco perfume (or spice), combines with cigarette itself to coordinate, and makes this perfume (or spice) of tobacco appear; Cigarette is fragrant to be improved, and does not feel and add thing and add.
The neutral flavor components D 25 (being cut D25) that present embodiment is prepared is used for cigarette and smokes panel test; The result who obtains through smokeing panel test shows: compare with blank cigarette (not adding the cigarette of cut D25); Adding this cut D25 makes flue gas fragrance obvious; Have blue or green perfume, the fine and smooth convergence of flue gas, and have the effect of pressing assorted gas.
Claims (10)
1. the preparation method of neutral flavor composition in the sound tobacco flue gas granule phase substance; It is characterized in that; Said neutral flavor composition is a raw material with sound tobacco flue gas granule phase substance; Obtain the neutral compound of flue gas granule phase substance successively through extraction, pickling and alkali cleaning step, the neutral compound with the flue gas granule phase substance that obtains makes through the normal phase silica gel column chromatography separation again.
2. the preparation method of neutral flavor composition in the sound tobacco flue gas granule phase substance as claimed in claim 1; It is characterized in that said neutral flavor composition is for separating a cut among D6, D17, D18 and the D25 among 28 eluting fraction D1-D28 that make through normal phase silica gel column chromatography.
3. the preparation method of neutral flavor composition in according to claim 1 or claim 2 the sound tobacco flue gas granule phase substance specifically comprises the steps:
(1) extracts: on rotary smoking machine, adopt filter disc to capture mode, collect sound tobacco flue gas granule phase substance, obtain the cambridge filter ravin with cambridge filter; After the cambridge filter ravin employing extraction liquid extraction that obtains, concentrating under reduced pressure obtains the liquid concentrator S1 of Vandyke brown crude extract;
(2) pickling: the liquid concentrator S1 of the Vandyke brown crude extract that step (1) is obtained adopts sour water to extract, and extraction repeatedly separates organic phase and water respectively, obtains organic phase extract S2;
(3) alkali cleaning: the organic phase extract S2 that step (2) is obtained adopts alkali lye to extract; Extraction repeatedly respectively; Separate organic phase and water, the organic phase after the alkali cleaning is carried out obtaining organic phase extract S3 behind the concentrating under reduced pressure, be the neutral compound of flue gas granule phase substance;
(4) normal phase silica gel column chromatography separates: adopt normal phase silicagel column that the organic phase extract S3 that step (3) obtains is carried out gradient elution; Organic phase extract S3 is when column chromatography for separation; Obtain 28 wash-out fraction D1-D28 by the equal-volume collection, D6, D17, D18 and D25 among 28 wash-out fraction D1-D28 are removed the back of desolvating respectively obtain said neutral flavor composition; Wherein gradient elution adopts the gradient elution agent that polarity increases gradually.
4. the preparation method of neutral flavor composition is characterized in that in the sound tobacco flue gas granule phase substance as claimed in claim 3, and in the step (1), said extraction liquid is an ether; The liquid concentrator S1 of said Vandyke brown crude extract is the diethyl ether solution of Vandyke brown crude extract.
5. the preparation method of neutral flavor composition is characterized in that in the sound tobacco flue gas granule phase substance as claimed in claim 3, and in the step (1), the method for said extraction is selected from one or more methods of soaking in extraction, ultrasonic extraction and the shaking table oscillation extraction; The vacuum tightness of said concentrating under reduced pressure is 500-1000mbar, and the bath temperature that concentrating under reduced pressure adopted is 25-60 ℃.
6. the preparation method of neutral flavor composition is characterized in that in the sound tobacco flue gas granule phase substance as claimed in claim 3, and in the step (2), said sour water is hydrochloric acid soln or sulphuric acid soln; In the step (3), said alkali lye is sodium hydroxide solution.
7. the preparation method of neutral flavor composition is characterized in that in the sound tobacco flue gas granule phase substance as claimed in claim 3, and in the step (4), the diameter of said normal phase silicagel column is 2.3cm; The weight of the corresponding filling gel of the organic phase extract S3 of every 0.5mL is 20g.
8. the preparation method of neutral flavor composition is characterized in that in the sound tobacco flue gas granule phase substance as claimed in claim 3, and in the step (4), when carrying out gradient elution, normal hexane, ether and ethanol are selected in the gradient elution agent that polarity increases gradually for use; When selecting normal hexane, ether and ethanol for use; The employing volume ratio is 100: 0 normal hexane and an ether earlier; Being increased to volume ratio gradually through polarity is 0: 100 normal hexane and ether; Adopting volume ratio again is 100: 0 ether and ethanol, and being increased to volume ratio gradually through polarity is 0: 100 ether and ethanol;
Perhaps, in the step (4), when carrying out gradient elution, Skellysolve A, ether and methyl alcohol are selected in the gradient elution agent that polarity increases gradually for use; When selecting Skellysolve A, ether and methyl alcohol for use; The employing volume ratio is 100: 0 Skellysolve A and an ether earlier; Being increased to volume ratio gradually through polarity is 0: 100 Skellysolve A and ether; Adopting volume ratio again is 100: 0 ether and methyl alcohol, and being increased to volume ratio gradually through polarity is 0: 100 ether and methyl alcohol.
9. the preparation method of neutral flavor composition is characterized in that in the sound tobacco flue gas granule phase substance as claimed in claim 8,
In the step (4); When carrying out gradient elution, the elutriant of following polarity and volume is adopted in the gradient elution agent successively: volume ratio is 100: 0 normal hexane and ether 100ml, and volume ratio is 99: 1 normal hexane and ether 100ml; Volume ratio is 98: 2 normal hexane and ether 150ml; Volume ratio is 95: 5 normal hexane and ether 250ml, and volume ratio is 90: 10 normal hexane and ether 100ml, and volume ratio is 80: 20 normal hexane and ether 200ml; Volume ratio is 50: 50 normal hexane and ether 200ml; Volume ratio is 0: 100 normal hexane and ether 100ml, and volume ratio is 100: 0 ether and ethanol 100ml, and volume ratio is 0: 100 ether and ethanol 100ml;
Perhaps, when carrying out gradient elution, the elutriant of following polarity and volume is adopted in the gradient elution agent successively: volume ratio is 100: 0 Skellysolve A and ether 100ml; Volume ratio is 99: 1 Skellysolve A and ether 100ml, and volume ratio is 98: 2 Skellysolve A and ether 150ml, and volume ratio is 95: 5 Skellysolve A and ether 250ml; Volume ratio is 90: 10 Skellysolve A and ether 100ml; Volume ratio is 80: 20 Skellysolve A and ether 200ml, and volume ratio is 50: 50 Skellysolve A and ether 200ml, and volume ratio is 0: 100 Skellysolve A and ether 100ml; Volume ratio is 100: 0 ether and methyl alcohol 100ml, and volume ratio is 0: 100 ether and methyl alcohol 100ml;
In the step (4), the said collection by equal-volume obtains among 28 wash-out fraction D1-D28, and every equal-volume is 50ml; , the gradient elution agent begins to collect when beginning to flow out.
10. adopt the neutral flavor composition of preparing method's acquisition of neutral flavor composition in the arbitrary described sound tobacco flue gas granule phase substance of claim 1-9 preparing cigarette shreds or mouth rod perfuming Application for Field.
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| CN102763893A (en) * | 2012-08-14 | 2012-11-07 | 云南烟草科学研究院 | Method for expanding cut tobaccos |
| CN102879250A (en) * | 2012-11-01 | 2013-01-16 | 云南烟草科学研究院 | Smoke extract and method for determining HRMS information content in smoke extract |
| CN103919268A (en) * | 2014-03-28 | 2014-07-16 | 广东中烟工业有限责任公司 | Cigarette without generating secondhand smoke |
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| CN102763893A (en) * | 2012-08-14 | 2012-11-07 | 云南烟草科学研究院 | Method for expanding cut tobaccos |
| CN102879250A (en) * | 2012-11-01 | 2013-01-16 | 云南烟草科学研究院 | Smoke extract and method for determining HRMS information content in smoke extract |
| CN103919268A (en) * | 2014-03-28 | 2014-07-16 | 广东中烟工业有限责任公司 | Cigarette without generating secondhand smoke |
| CN103919270A (en) * | 2014-03-28 | 2014-07-16 | 广东中烟工业有限责任公司 | Tobacco product |
| CN103919268B (en) * | 2014-03-28 | 2016-03-30 | 广东中烟工业有限责任公司 | A kind of cigarette not producing second-hand-cigarette |
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| CN106093252A (en) * | 2016-05-27 | 2016-11-09 | 河南中烟工业有限责任公司 | A kind of separation method of cigarette mainstream flue gas Neutral Aroma Components |
| CN108627600A (en) * | 2017-03-20 | 2018-10-09 | 上海烟草集团有限责任公司 | The analysis method of flavor component in a kind of flue gas |
| CN109959649A (en) * | 2017-12-26 | 2019-07-02 | 中国农业科学院烟草研究所 | A kind of coke tar in cigarette extract and its chemical luminous system with chemiluminescence property |
| CN109846077A (en) * | 2018-12-12 | 2019-06-07 | 云南中烟工业有限责任公司 | A kind of method and application that characteristic component is screened and prepared from tobacco |
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