CN102586019B - 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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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 Smoke Particulate neutral flavor composition.
Background technology
Along with the increasing of domestic tobacco industry reducing tar and reducing harm dynamics, the requirement of centering type cigarette (especially low tar Chinese-style cigarette) compensating aroma technology also promotes day by day.In addition, what cigarette added at present all is food flavor(ing) spices, but the requirement of food flavor(ing) spices being added along with health ministry is standard and strict progressively, 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 has also been proposed a larger difficult problem, the compensating aroma technology has become important research content and the direction of Chinese-style cigarette.
Neutral flavor material in the flue gas is the important chemical composition that affects the cigarette quality.Research to cigarette mainstream flue gas neutral flavor composition, can the most directly understand and organoleptic effect between mutual relationship, thereby for flavoring and casing and the tobacco leaf formulation design of cigarette provides important information, for the inner quality that improves Chinese-style cigarette is laid reliable theoretical basis, for production practice provide more wide application prospect.
Chemical Components in Cigarette Smoke is of a great variety, and the composition of nowadays identifying in the flue gas and kind have reached 7357 kinds, and wherein oxygenatedchemicals just has 3568 kinds, so the Components identification operation irregularity is complicated.In addition, most of material is trace components 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 take the high-quality cigarette smoke separates making the flavor matter that flue gas itself possesses, thereby obtains natural flavouring essence for tobacco as starting point from the sound tobacco Smoke Particulate.Such essence comes from smoke of tobacco self, extracts from natural tobacco leaf Smoke Particulate, 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 a kind of preparation method of neutral aroma components in grain phase of smoke of high-quality tobacco leaves.
Another object of the present invention provides the application of described neutral aroma components in grain phase of smoke of high-quality tobacco leaves.
To achieve these goals, the present invention adopts following technical scheme to realize:
A kind of preparation method of neutral aroma components in grain phase of smoke of high-quality tobacco leaves, described neutral flavor composition is take the sound tobacco Smoke Particulate as raw material, obtain successively the neutral compound of Smoke Particulate through extraction, pickling and alkali cleaning step, the neutral compound of the Smoke Particulate that obtains is separated making again through normal phase silica gel column chromatography.
Better, described 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.
Better, the preparation method of described neutral aroma components in grain phase of smoke of high-quality tobacco leaves specifically comprises the steps:
(1) extracts: on rotary smoking machine, adopt the filter disc Trapping ways, collect the sound tobacco Smoke Particulate with cambridge filter, obtain the cambridge filter ravin; After the cambridge filter ravin employing extraction liquid extraction that obtains, concentrating under reduced pressure obtains the concentrated solution S1 of Vandyke brown crude extract;
Better, described extraction liquid is ether.Further, the concentrated solution S1 of described Vandyke brown crude extract is the diethyl ether solution of Vandyke brown crude extract.
Better, the method for described extraction is for soaking one or more methods in extraction, ultrasonic extraction and the shaking table oscillation extraction; The vacuum tightness of described concentrating under reduced pressure is 500-1000mbar, and the bath temperature that concentrating under reduced pressure adopts is 25-60 ℃.
(2) pickling: the concentrated solution 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;
Better, described sour water is hydrochloric acid soln or sulphuric acid soln.Further, the mass percent concentration of acid is 1-10% in described hydrochloric acid soln or the sulphuric acid soln.Preferably, the mass percent concentration of acid is 5% in described 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 Smoke Particulate;
Better, described alkali lye is sodium hydroxide solution.Further, the mass percent concentration of sodium hydroxide is 1-10% in the described sodium hydroxide solution.Preferably, the mass percent concentration of sodium hydroxide is 5% in the described sodium hydroxide solution.
Better, in the step (3), the vacuum tightness of described concentrating under reduced pressure is 500-1000mbar, the bath temperature that concentrating under reduced pressure adopts 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, collect by equal-volume and to obtain 28 wash-out fraction D1-D28, will D6, D17 among 28 wash-out fraction D1-D28, D18 and D25 obtain described neutral flavor composition after the desolventizing respectively; Wherein gradient elution adopts the gradient elution agent that polarity increases gradually.
Better, in the step (4), the diameter of described 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.
Better, 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; When selecting normal hexane, ether and ethanol, adopting first volume ratio is 100: 0 normal hexane and ether, being increased to gradually volume ratio through polarity is 0: 100 normal hexane and ether, adopting volume ratio is 100: 0 ether and ethanol again, and being increased to gradually volume ratio 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; When selecting Skellysolve A, ether and methyl alcohol, adopting first volume ratio is 100: 0 Skellysolve A and ether, being increased to gradually volume ratio through polarity is 0: 100 Skellysolve A and ether, adopting volume ratio is 100: 0 ether and methyl alcohol again, and being increased to gradually volume ratio through polarity is 0: 100 ether and methyl alcohol.
Normal hexane is selected in the gradient elution agent that polarity of the present invention increases gradually, " adopting first volume ratio is 100: 0 normal hexane and ether; being increased to gradually volume ratio through polarity is 0: 100 normal hexane and ether; adopting volume ratio is 100: 0 ether and ethanol again; being increased to gradually volume ratio through polarity is 0: 100 ether and ethanol " refers to adopt first 100% normal hexane to carry out wash-out in ether and the ethanol, then the amount that increases gradually ether in 100% normal hexane increases the polarity of eluent, be increased to 100% ether always, adopt again the amount that in 100% ether, increases gradually ethanol to increase the polarity of eluent, 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, 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, volume ratio is 90: 10 normal hexane and ether 100ml, 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, 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, volume ratio is 98: 2 Skellysolve A and ether 150ml, 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, 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 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, namely select Skellysolve A, ether and ethanol, also ethanol methyl alcohol be can be replaced with, normal hexane, ether and methyl alcohol namely selected.
Better, the described collection by equal-volume obtains among 28 wash-out fraction D1-D28, and every equal-volume is 50ml.
Better, in the step (4), the described collection by equal-volume obtains beginning to collect among 28 wash-out fraction D1-D28 when the gradient elution agent begins to flow out.
In the step of the present invention (4), collecting 28 wash-out fraction D1-D28 is to collect successively first cut D1, second cut D2, the 3rd cut D3 ..., 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 promote from different perspectives the flue gas quality of cigarette through the different as can be known neutral flavor cut of smokeing panel test.
Neutral aroma components in grain phase of smoke of high-quality tobacco leaves of the present invention is to obtain through above-mentioned preparation method.
Neutral aroma components in grain phase of smoke of high-quality tobacco leaves of the present invention and preparation method thereof can be widely used in preparing in cigarette shreds or the mouth rod perfuming field.
Outstanding advantages of the present invention is:
The present invention also can be described as different neutral flavor compositions take the sound tobacco Smoke Particulate neutral flavor cut different as raw material prepares, the lifting that various neutral flavor cuts have different angles and degree to 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 corresponding 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 simultaneously the obvious lifting of cigarette product interior quality, be more widely used at brand cigarette.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 for explanation the present invention and are not used in restriction protection scope of the present invention.
Embodiment 1
The preparation of neutral aroma components in grain phase of smoke of high-quality tobacco leaves:
(1) extracts: on rotary smoking machine, adopt the filter disc Trapping ways, collect the sound tobacco Smoke Particulate with cambridge filter (diameter is 92mm, and every cambridge filter is collected 20 cigarette smoke granule phase substances), obtain the cambridge filter ravin; 30 cambridge filter ravin that capture high-quality cigarette smoke granule phase substance are soaked extraction with ether first, and then behind the supersound extraction 5min, shaking table mechanical shaking extraction 30min places and repeats to extract one time after one day again again, obtains extracting solution.The concentrated solution S1 of Vandyke brown crude extract will be obtained behind the extracting solution concentrating under reduced pressure that obtain; Wherein, the vacuum tightness of concentrating under reduced pressure is 870mbar, and bath temperature is 36 ℃.
(2) pickling: the concentrated solution S1 of Vandyke brown crude extract is transferred to separating funnel, is 5% H with mass percent concentration
2SO
4Aqueous solution extraction three times, each volume is 250mL.Separate organic phase and water, obtain organic phase extract S2;
(3) alkali cleaning: organic phase extract S2 is transferred to separating funnel, is 5% NaOH aqueous solution extraction 3 times with mass percent concentration, 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 Smoke Particulate; 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 eluent gradient adopts first the volume ratio of normal hexane and ether from 100: 0 to 50: 50, again by 0: 100, then using ether and ethanol instead is the gradient elution agent, and the volume ratio of ether and ethanol was 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, 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, volume ratio is 90: 10 normal hexane and ether 100ml, 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, 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, when beginning to flow out, the gradient elution agent begins to collect, collect by equal-volume (50mL) and to obtain 28 wash-out fraction D1-D28, will D6, D17 among 28 wash-out fraction D1-D28, D18 and D25 obtain neutral flavor components D 6, D17, D18 and D25 after the desolventizing respectively.
Neutral flavor components D 6, D17, D18 and D25 dissolve again with ethanol respectively, are made into the solution that concentration is 2.4/milliliter and are used for smokeing panel test.2.4/milliliter neutral flavor compositions that refer to contain in every milliliter of ethanol 2.4 cigarette wherein.
(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 forms 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 so that cigarette smoke is fine and smooth, with 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, thoroughly clear, 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), coordinate with cigarette combination itself, make 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, with blue or green fragrant, the fine and smooth convergence of flue gas, and have the effect of pressing assorted gas.
Embodiment 5
The preparation of neutral aroma components in grain phase of smoke of high-quality tobacco leaves:
Except the vacuum tightness of the concentrating under reduced pressure among the concentrated solution S1 that obtains the Vandyke brown crude extract behind the extracting solution concentrating under reduced pressure that will obtain 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 ℃, other preparation 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 again with ethanol respectively, be made into the solution that concentration is 2.4/milliliter and be used for smokeing 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 forms 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 with fruital, has the style and features of high-quality tobacco so that cigarette smoke is fine and smooth, 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 prepares is smoked panel test for cigarette, 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, thoroughly clear, the fragrant quality-improving of cigarette.
The neutral flavor components D 18 (being cut D18) that present embodiment prepares is smoked panel test for cigarette, 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), coordinate with cigarette combination itself, make 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 prepares is smoked panel test for cigarette, 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, with blue or green fragrant, the fine and smooth convergence of flue gas, and have the effect of pressing assorted gas.
Embodiment 6
The preparation of neutral aroma components in grain phase of smoke of high-quality tobacco leaves:
Except the vacuum tightness of the concentrating under reduced pressure among the concentrated solution S1 that obtains the Vandyke brown crude extract behind the extracting solution concentrating under reduced pressure that will obtain 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 ℃, other preparation 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 again with ethanol respectively, be made into the solution that concentration is 2.4/milliliter and be used for smokeing 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 forms 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 so that cigarette smoke is fine and smooth, with 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 prepares is smoked panel test for cigarette, 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, thoroughly clear, the fragrant quality-improving of cigarette.
The neutral flavor components D 18 (being cut D18) that present embodiment prepares is smoked panel test for cigarette, 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), coordinate with cigarette combination itself, make 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 prepares is smoked panel test for cigarette, 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, with blue or green fragrant, the fine and smooth convergence of flue gas, and have the effect of pressing assorted gas.
Embodiment 7
The preparation of neutral aroma components in grain phase of smoke of high-quality tobacco leaves:
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, 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, volume ratio is 90: 10 Skellysolve A and ether 100ml, 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, volume ratio is 100: 0 ether and methyl alcohol 100ml, volume ratio is outside 0: 100 the ether and methyl alcohol 100ml, other preparation 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 again with ethanol respectively, be made into the solution that concentration is 2.4/milliliter and be used for smokeing 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 forms 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 so that cigarette smoke is fine and smooth, with 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 prepares is smoked panel test for cigarette, 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, thoroughly clear, the fragrant quality-improving of cigarette.
The neutral flavor components D 18 (being cut D18) that present embodiment prepares is smoked panel test for cigarette, 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), coordinate with cigarette combination itself, make 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 prepares is smoked panel test for cigarette, 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, with blue or green fragrant, the fine and smooth convergence of flue gas, and have the effect of pressing assorted gas.
Claims (5)
1. the preparation method of a neutral aroma components in grain phase of smoke of high-quality tobacco leaves specifically comprises the steps:
(1) extracts: on rotary smoking machine, adopt the filter disc Trapping ways, collect the sound tobacco Smoke Particulate with cambridge filter, obtain the cambridge filter ravin; After the cambridge filter ravin employing extraction liquid extraction that obtains, concentrating under reduced pressure obtains the concentrated solution S1 of Vandyke brown crude extract, and described extraction liquid is ether; The concentrated solution S1 of described Vandyke brown crude extract is the diethyl ether solution of Vandyke brown crude extract;
(2) pickling: the concentrated solution 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 Smoke Particulate;
(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, collect by equal-volume and to obtain 28 wash-out fraction D1-D28, will D6, D17 among 28 wash-out fraction D1-D28, D18 and D25 obtain described neutral flavor composition after the desolventizing respectively;
When carrying out gradient elution, the elutriant of following polarity and volume is adopted in the gradient elution agent successively: volume ratio is normal hexane and the ether 100ml of 100:0, volume ratio is normal hexane and the ether 100ml of 99:1, volume ratio is normal hexane and the ether 150ml of 98:2, volume ratio is normal hexane and the ether 250ml of 95:5, volume ratio is normal hexane and the ether 100ml of 90:10, volume ratio is normal hexane and the ether 200ml of 80:20, volume ratio is normal hexane and the ether 200ml of 50:50, volume ratio is normal hexane and the ether 100ml of 0:100, volume ratio is ether and the ethanol 100ml of 100:0, and volume ratio is ether and the ethanol 100ml of 0:100;
Perhaps, when carrying out gradient elution, the elutriant of following polarity and volume is adopted in the gradient elution agent successively: volume ratio is Skellysolve A and the ether 100ml of 100:0, volume ratio is Skellysolve A and the ether 100ml of 99:1, volume ratio is Skellysolve A and the ether 150ml of 98:2, volume ratio is Skellysolve A and the ether 250ml of 95:5, volume ratio is Skellysolve A and the ether 100ml of 90:10, volume ratio is Skellysolve A and the ether 200ml of 80:20, volume ratio is Skellysolve A and the ether 200ml of 50:50, volume ratio is Skellysolve A and the ether 100ml of 0:100, and volume ratio is ether and the methyl alcohol 100ml of 100:0, and volume ratio is ether and the methyl alcohol 100ml of 0:100;
The described collection by equal-volume obtains among 28 wash-out fraction D1-D28, and every equal-volume is 50ml; When beginning to flow out, the gradient elution agent begins to collect.
2. the preparation method of neutral aroma components in grain phase of smoke of high-quality tobacco leaves as claimed in claim 1 is characterized in that, in the step (1), the method for described extraction is selected from one or more methods of soaking in extraction, ultrasonic extraction and the shaking table oscillation extraction; The vacuum tightness of described concentrating under reduced pressure is 500 – 1000mbar, and the bath temperature that concentrating under reduced pressure adopts is 25-60 ° of C.
3. the preparation method of neutral aroma components in grain phase of smoke of high-quality tobacco leaves as claimed in claim 1 is characterized in that, in the step (2), described sour water is hydrochloric acid soln or sulphuric acid soln; In the step (3), described alkali lye is sodium hydroxide solution.
4. the preparation method of neutral aroma components in grain phase of smoke of high-quality tobacco leaves as claimed in claim 1 is characterized in that, in the step (4), the diameter of described 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.
5. adopt the application of neutral flavor composition in preparation cigarette shreds or mouth rod perfuming field of preparation method's acquisition of the arbitrary described neutral aroma components in grain phase of smoke of high-quality tobacco leaves of claim 1-4.
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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 |
| 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 |
| CN103919270B (en) * | 2014-03-28 | 2016-08-17 | 广东中烟工业有限责任公司 | A kind of cigarette products |
| CN106093252B (en) * | 2016-05-27 | 2019-01-11 | 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 |
| CN108627600B (en) * | 2017-03-20 | 2021-03-12 | 上海烟草集团有限责任公司 | Method for analyzing aroma components in smoke |
| CN109959649B (en) * | 2017-12-26 | 2022-03-04 | 中国农业科学院烟草研究所 | Cigarette tar extract with chemiluminescence property and chemiluminescence system thereof |
| 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 |
| CN114711455B (en) * | 2022-03-10 | 2022-12-23 | 浙江中烟工业有限责任公司 | Preparation method and application of alkaline flavor components with characteristics of Canadian tobacco smoke |
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| CN1099957A (en) * | 1993-09-11 | 1995-03-15 | 中国烟草总公司郑州烟草研究院 | Adsorbent for cigarette filter-tip |
| CN101194749A (en) * | 2007-12-28 | 2008-06-11 | 广东中烟工业公司 | Thin section for tobacco, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1099957A (en) * | 1993-09-11 | 1995-03-15 | 中国烟草总公司郑州烟草研究院 | Adsorbent for cigarette filter-tip |
| CN101194749A (en) * | 2007-12-28 | 2008-06-11 | 广东中烟工业公司 | Thin section for tobacco, preparation method and application thereof |
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