CN104138028B - A kind of extracting method of tobacco flavor composition and application thereof - Google Patents
A kind of extracting method of tobacco flavor composition and application thereof Download PDFInfo
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Abstract
The invention provides a kind of tobacco flavor component extracting method, comprise the following steps: pipe tobacco or tobacco leaf are carried out Balance Treatment or dry process, make sample moisture content even; By pipe tobacco or tobacco leaf, after putting into Extraction solvent dipping, cooling; Mixed liquor is put into Ultrasonic Cell Disruptor, utilizes ultrasonic grind pipe tobacco or tobacco leaf; After pulverizing pipe tobacco or tobacco leaf, airtight container, after continuing dipping, centrifugal segregation solid formation, namely obtains tobacco flavor constituents extraction liquid.The present invention still further provides above-mentioned tobacco flavor component extracting method in the analysis of tobacco flavor component content and the application of producing in tobacco extract.Tobacco flavor component extracting method of the present invention, by adopting ultrasonic disruption extractive technique, without the need to making pulverization process in advance to pipe tobacco or tobacco leaf, effective minimizing flavor component scatters and disappears, extraction efficiency is high, simplify extraction process, can carry out quantitatively flavor component in tobacco, and effectively produce tobacco extract.
Description
Technical field
The invention belongs to technical field of tobacco, relate to a kind of tobacco flavor component extracting method and application thereof, be specifically related to a kind of ultrasonic disruption extract tobacco flavor composition method and in the analysis of tobacco flavor component quantifying and the application of producing in tobacco extract.
Background technology
Playing raw material characteristic and the advantage of Tobacco to greatest extent, is the key point improving Chinese-style cigarette core competitiveness.Along with deepening continuously of tobacco processing procedure technical research, the evaluation of tobacco quality progressively changes to the direction focusing on Inner Quality of Tobacco by stressing physical index, and how effectively to extract aroma component in tobacco, and accurate quantitative analysis is carried out to special component, be optimizing tobacco processing technology and the prerequisite improving Chinese-style cigarette quality of item.
At present, tobacco flavor component extracting method many employings steam distillation, but the original flavor component of long-time high-temperature boiling heavy damage tobacco is formed, and generate new chemical composition.More seriously, steam distillation repeatability is poor, and relative standard deviation scope is 10-30%, and test error may cover the change that technique causes, and causes the conclusion difference of different experiments room even contrary.Also be the comparatively normal extracting mode adopted by Solvent Extract methods, but in order to improve extraction efficiency, usually need in advance tobacco to be dried and grind into powder, and after tobacco clays into power, surface area significantly increases, and the loss of volatile fragrance component is very remarkable; And before abrasive dust, need to carry out drying and processing to tobacco, in the process of heated-air drying, scattering and disappearing with moisture, fragrance component is also in continuous loss.
Compare steam distillation and organic solvent extraction, the method more preferably extracting flavor component is under case without heating, carries out tobacco pulverizing and extraction simultaneously, can reach this effect by ultrasonic cell-break technology.Be different from conventional ultrasonic assistant extractive technique, ultrasonic cell-break method adopts high-frequency ultrasonic, cavitation effect, mechanical effect and fuel factor can be produced when propagating in liquid, there is stronger penetrability in certain distance, clasmatosis can be made, therefore full wafer crushing material can be made in the solution, and without the need to extra machining pulverising step.Ultrasonic disruption auxiliary extraction technology is widely used in the extraction of Chinese herbal medicine effective ingredients and the extraction of bacterial expression albumen, but have not been reported for the research of extracting the flavor component in tobacco (tobacco leaf, waste/hypo-tobacco leaf or pipe tobacco).
Summary of the invention
The object of the present invention is to provide a kind of tobacco flavor component extracting method and application thereof, a kind of method of ultrasonic disruption assisted extraction tobacco flavor composition is provided, need dry sample in advance and grind process for solving tobacco flavor constituents extraction in prior art, need sample size large, sample making course at substantial raw tobacco material, dries and attrition process flavor component loses serious; Or need long-time impregnation process, the problem that chemical reaction affects the structures and characteristics of flavor component in tobacco can occur.
For achieving the above object, the invention provides a kind of tobacco flavor component extracting method, comprise the following steps:
Preferably, described tobacco is selected from one or more combinations in tobacco leaf, waste/hypo-tobacco leaf or pipe tobacco.
1) pretreatment: pipe tobacco or tobacco leaf are carried out Balance Treatment or dry process, make sample moisture content even;
Preferably, described Balance Treatment is positioned in climatic chamber by pipe tobacco or tobacco leaf, under certain temperature and humidity conditions, balance a period of time.Further, the temperature of described Balance Treatment is 20-30 DEG C, and humidity is 55-65%.Preferably, the temperature of described Balance Treatment is 25 DEG C, and humidity is 60%.
Further, the time of described Balance Treatment is 48h.
Preferably, described drying process is positioned in air dry oven by pipe tobacco or tobacco leaf, dry process a period of time under uniform temperature condition.Further, the temperature of described drying process is 45-55 DEG C.Preferably, the temperature of described drying process is 50 DEG C.
Further, the time of described drying process is 4h.
Described Balance Treatment or dry process main purpose make different sample moisture content consistent, thus be conducive to carrying out quantitative analysis to pipe tobacco or tobacco leaf flavor component.
2) pre-preg process: by step 1) gained pipe tobacco or tobacco leaf, after putting into Extraction solvent dipping, cooling;
Preferably, described tobacco leaf will be cut into small pieces blade.Further, the area of described fritter blade is less than 1.5cm × 1.5cm.Be conducive to putting into container dipping and carrying out ultrasonic disruption.
Preferably, Extraction solvent is selected from one or more combinations in water, methyl alcohol, ethanol, methyl tertiary butyl ether(MTBE).When ether, carrene are as Extraction solvent, crushing effect is poor, should avoid using.
Preferably, described Extraction solvent addition is the 10-25 times amount of pipe tobacco or tobacco leaf.Concrete, described Extraction solvent addition is that the 10-25 times amount of pipe tobacco or tobacco leaf refers to: Extraction solvent adds 10-25 times that quality is described pipe tobacco or quality of tobacco.Because the density of different solvents is different, the quality of Extraction solvent, divided by its density, obtains the volume that Extraction solvent adds.
Described pipe tobacco or tobacco leaf consumption excessive time, crushing effect be deteriorated, still can leave larger-size fragment after fragmentation terminates; And pipe tobacco or tobacco leaf consumption very few time, the concentration extracting flavor component in the solution that obtains is lower, is unfavorable for the enforcement of subsequent analysis step.
Preferably, described dip time is 5-20min.Preferably, described dip time is 5min.The described prolongation along with dip time, pipe tobacco or the time required for broken leaf breaking can shorten, and within the identical ultrasonication time, extraction effect can promote, but the time that whole processing procedure expends also can increase.
Preferably, described cooling is carried out in ice-water bath.The reason of carrying out cooling while pre-preg is: heat transmission is slower in the solution, especially transmit slower in conventional organic solvent and when amount of solution is larger, for ensureing that in ultrasonication processing procedure, solution temperature keeps lower, makes solution temperature be cooled to close to 0 DEG C when pre-preg by ice-water bath.
3) ultrasonic grind: by step 2) gained mixed liquor puts into Ultrasonic Cell Disruptor, utilizes ultrasonic grind pipe tobacco or tobacco leaf;
Preferably, described ultrasonic grind condition is: ultrasonic power: 500 ~ 950W; Ultrasonic amplitude of fluctuation shank diameter: 2-15mm; The ultrasonic circulation time: ultrasonic time 2-5s, intermittent time 5-10s, circulation is carried out and is ultrasonicly always lasted for 10-30min.
Preferably, described ultrasonic grind condition is: ultrasonic power: 665W; Ultrasonic amplitude of fluctuation shank diameter: 6mm; The ultrasonic circulation time: ultrasonic time 3s, intermittent time 9s, circulation is carried out and is ultrasonicly always lasted for 20min.
Further, described ultrasonic amplitude transformer inserts in described maceration extract.
Preferably, need during described ultrasonic grind to continue to cool in ice-water bath.Because Ultrasonic Cell Disruptor power is comparatively large, ultrasonication Process liquor temperature can significantly rise, and causes the conversion of flavor component in the quick volatilization of Extraction solvent and tobacco and scatter and disappear.
The described ultrasonic circulation time is the key factor affecting tobacco flavor constituents extraction efficiency, the ultrasonication processing time is too short pipe tobacco or tobacco leaf just cannot be made completely to pulverize and make pipe tobacco or tobacco leaf cells structure broken, cause flavor component concentration in extract very low; But the ultrasonication processing time is long, Ultrasonic Cell Disruptor can be caused to generate heat obviously, cause volatile component in extract to scatter and disappear serious, must ensure that solution temperature is lower than 50 DEG C, thus the repeatability avoiding subsequent analysis to test be deteriorated.
Described discontinuous time ultrasonic circulation time must not be less than 5s, and reason is: intermittent time too short then solution cooling is insufficient, and thermal accumlation can cause solution temperature to rise, and causes solvent volatilization and flavor component transform and scatter and disappear; Intermittent time is long, and extraction process efficiency can be made to decline.The setting of intermittent time should ensure lower than 50 DEG C as principle to make solution temperature.
Described ultrasonic grind pipe tobacco and tobacco leaf pulverize by making the cell membrane of pipe tobacco and tobacco leaf broken.
4) obtain tobacco flavor composition: after pulverizing pipe tobacco or tobacco leaf, airtight container, after continuing dipping, centrifugal segregation solid formation, namely obtains tobacco flavor constituents extraction liquid.
Preferably, after described ultrasonic grind pipe tobacco or tobacco leaf, pipe tobacco or broken leaf breaking become mixed pulpous state.
Preferably, described continuation dip time is 5-20min.Preferably, described continuation dip time is 5min.
Preferably, described centrifugation time is 5min, and centrifugal speed is 5000rpm.
The invention provides the application of a kind of tobacco flavor component extracting method in tobacco flavor component content is analyzed.
A content analysis method for tobacco flavor composition, comprises the following steps:
A) pretreatment: with a kind of step 1 of tobacco flavor component extracting method) identical;
B) pre-preg process: with a kind of step 2 of tobacco flavor component extracting method) identical;
C) ultrasonic grind: with a kind of step 3 of tobacco flavor component extracting method) identical;
D) tobacco flavor composition is obtained: with a kind of step 4 of tobacco flavor component extracting method) identical;
E) constituent analysis: adopt combined gas chromatography mass spectrometry determination step D) described in the content of tobacco flavor composition.
Preferably; described tobacco flavor composition is butyrolactone, geranyl acetone, benzyl carbinol, neophytadiene, maltol, acetyl pyrrole, Megastigmatrienone A, Megastigmatrienone B, methyl palmitate, 2; 3-dihydro-3; 5-dihydroxy-6-methyl-4-H-pyrans-4-ketone (DDMP), Megastigmatrienone C, Megastigmatrienone D, nicotyrine, dihydroactinidiolide, farnesyl acetone, 2,3-bipyridyls, 3-hydroxyl-damascenone, phytol, 3-oxo-α-ionol.
Preferably, described combined gas chromatography mass spectrometry adopts spectrum data library searching, determines tobacco flavor composition.
Further, described spectrum data storehouse is NIST05 database, and described tobacco flavor composition basis for estimation selects matching degree >=90.
Preferably, described combined gas chromatography mass spectrometry adopts internal standard method to carry out semi-quantitative analysis to tobacco flavor composition.
Further, described internal standard method refers to: choose one grow tobacco in the composition that do not possess as interior mark, be mark working solution in solvent configuration concentration known with methyl alcohol, join through overbalance by marking working solution in certain volume or dry to process and in the tobacco leaf carrying out pre-preg process or tobacco sample, ultrasonic disruption technology is adopted to carry out fragmentation and extraction process to sample again, GC-MS is adopted to detect the sample solution obtained, be reference by detecting the corresponding relation obtaining interior target content and peak area, and will chromatographic peak area corresponding to each flavor component of obtaining be detected and interior mark peak area compares, obtain the semi-quantitative results of various flavor component in tobacco.
Preferably, described combined gas chromatography mass spectrometry adopts external standard method to carry out quantitative analysis to tobacco flavor composition.
Further, described external standard method refers to: the standard sample solution choosing various flavor component in tobacco, pipette a series of different volumes respectively, adopt the analysis of GC-MS sample introduction, obtain the content of various flavor component and the linear relationship of peak area in standard liquid, with its corresponding content corresponding of chromatographic peak area in various flavor component, draw corresponding standard working curve, calculate the regression equation of standard working curve.Adopt GC-MS to detect the sample solution of actual extracting again, by the chromatographic peak area of various flavor component in the sample solution of acquisition, substitute in the regression equation of described standard working curve, the content of flavor component in corresponding tobacco can be obtained.
Preferably, as step e) as described in GC-MS condition be:
GC conditions is: chromatographic column: DB-Wax capillary column (60m × 0.32mm × 0.25 μm); Carrier gas: high-purity helium, purity >=99.999%; Flow velocity: 1.2mL/min (constant current mode); Split ratio: 50:1; Heating schedule: 50 DEG C (3min), 3 DEG C/min rise to 200 DEG C (0min), 20 DEG C/min rises to 220 DEG C (30min), namely initial temperature 50 DEG C keeps 3min, rise to 200 DEG C with the speed of 3 DEG C/min, then rise to 220 DEG C of maintenance 30min with the speed of 20 DEG C/min.
Mass Spectrometry Conditions is: transmission line temperature: 240 DEG C; Ion source temperature: 230 DEG C; Solvent delay: 18min; Ionization mode: EI source; Ionizing energy: 70eV; Scan mode: full scan (Scan).
The present invention also provides a kind of tobacco flavor component extracting method producing the application in tobacco extract.
Produce a method for tobacco extract, comprise the following steps:
I) pre-preg process: with a kind of step 2 of tobacco flavor component extracting method) identical;
II) ultrasonic grind: with a kind of step 3 of tobacco flavor component extracting method) identical;
III) tobacco flavor composition is obtained: with a kind of step 4 of tobacco flavor component extracting method) identical;
IV) prepare tobacco extract: by step III) in containing the supernatant low temperature solvent evaporated of tobacco flavor composition, obtain tobacco extract.
Preferably, described evaporate to dryness temperature is 40 ± 5 DEG C.
As mentioned above, a kind of tobacco flavor component extracting method of the present invention, by adopting ultrasonic disruption extractive technique, the enormous pressure utilizing ultrasonic cavitation to produce makes pipe tobacco or tobacco leaf cells wall break, accelerate flavor component in tobacco and enter solvent, extract while pipe tobacco or broken leaf breaking, without the need to making pulverization process in advance to pipe tobacco or tobacco leaf, by contrast, traditional steam distillation or organic solvent extraction, at sample making course for producing a sample, often need to dry and abrasive dust process the tobacco leaf of about 100g, can accomplish " sampling as required ", significantly reduce the tobacco leaf waste that sample making course causes, effectively reduce flavor component to scatter and disappear simultaneously, extraction efficiency is high, simplify extraction process.And ultrasonic grind is a physical process, occurs without chemical reaction in whole fragmentation and leaching process, do not affect the structures and characteristics of flavor component in tobacco.
In addition, the present invention still further provides the application of above-mentioned tobacco flavor component extracting method in tobacco flavor component content is analyzed, analyze by adopting GC-MS, effectively can obtain the quantitative result of flavor component in tobacco, wherein, adopt internal standard method to carry out semi-quantitative analysis to flavor component in tobacco, have good reappearance, RSD is all less than 10%.And tobacco flavor component extracting method of the present invention can also be used for producing tobacco extract, compares conventional method, not running off of flavor component in tobacco can be kept, preparation method is simple, fast.
Accompanying drawing explanation
Fig. 1 is shown as the total ion current figure of pipe tobacco extract;
Fig. 2 is shown as ultrasonic disruption and extracts and Solvent Extract methods effect contrast figure
Fig. 3 is shown as the repeated design sketch of ultrasonic disruption extraction method
Wherein, 1: butyrolactone; 2: geranyl acetone; 3: benzyl carbinol; 4: neophytadiene; 5: maltol; 6: acetyl pyrrole; 7: Megastigmatrienone A; 8: Megastigmatrienone B; 9: methyl palmitate; 10:2,3-dihydro-3,5-dihydroxy-6-methyl-4-H-pyrans-4-ketone (DDMP); 11: Megastigmatrienone C; 12: Megastigmatrienone D; 13: nicotyrine; 14: dihydroactinidiolide; 15: farnesyl acetone; 16:2,3-bipyridyl; 17:3-hydroxyl-damascenone; 18: phytol; 19:3-oxo-α-ionol.
Detailed description of the invention
Set forth the present invention further below in conjunction with specific embodiment, should be understood that these embodiments are only not used in for illustration of the present invention and limit the scope of the invention.
Below by way of specific instantiation, embodiments of the present invention are described, those skilled in the art the content disclosed by this description can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by detailed description of the invention different in addition, and the every details in this description also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
The reagent that embodiment uses, instrument are as follows:
1, reagent
Tobacco leaf, waste/hypo-tobacco leaf, pipe tobacco (all tobacco samples provide by Shanghai Tobacco Group Co., Ltd.); Standard specimen product (Sigma-Aldrich company) in methyl nicotinate; Water (distilled water); Methyl alcohol, ethanol, methyl tertiary butyl ether(MTBE) (HPLC level, grace section chemistry).
2, instrument
Climacell type climatic chamber (German MMM company); DHG type air dry oven (Shanghai precision instrumentation Co., Ltd); Scientz-IID ultrasonic cell disruptor (NingBo XinZhi Biology Science Co., Ltd); RJ-LDL-50G type centrifuge (Ruijiang Analyzer Co. Ltd., Wuxi City); 6890GC/5975M GC-MS (Anjelen Sci. & Tech. Inc); DB-Wax capillary column (60m × 0.32mm × 0.25 μm) (Anjelen Sci. & Tech. Inc); Electronic balance (sensibility reciprocal 0.0001g, Mettler Toledo Inc.)
Embodiment 1
Sample is the sheet cigarette chopping after the tobacco redrying of producing region, Jilin.Pipe tobacco is positioned in air dry oven, at 50 DEG C, under baking temperature condition, processes 4h.Then accurately take 0.5g pipe tobacco, load in 50mL round bottom band spiral cover plastic tube, add 10mL absolute ethyl alcohol, and be positioned over freezing dipping 5min in ice-water bath; Afterwards solution is positioned in Ultrasonic Cell Disruptor, the ultrasonic amplitude transformer of 6mm diameter is inserted in Extraction solvent, and arranging ultrasonic power is 665W, the continuous ultrasound time is 3s, intermittent time is 9s, and circulation is carried out and is ultrasonicly always lasted for 20min, utilizes ultrasonic grind pipe tobacco.Ultrasonication terminates rear airtight container, continues Soakage extraction 5min.By suction pipe, mixed slurry is moved in 2mL centrifuge tube, setting centrifugal speed is 5000rpm, centrifugal 5min.Getting supernatant 1mL adds in chromatogram bottle, pending gas chromatography combined with mass spectrometry analysis.
Embodiment 2
The solution to be measured containing tobacco flavor composition extracted by ultrasonic disruption in above-described embodiment 1, adopts combined gas chromatography mass spectrometry to measure.Simultaneously, will with same sample in above-described embodiment 1, add interior mark, organic solvent extraction is adopted to extract, extraction time is 24h, also adopts combined gas chromatography mass spectrometry to measure the extract of acquisition, and the combined gas chromatography mass spectrometry condition determination of two kinds of extracting methods is identical, use NIST05 database (matching degree >=90) to carry out qualitative, and adopt internal standard method to carry out semi-quantitative analysis.Concrete testing result is shown in Fig. 1-2, table 1.
As shown in Table 1, Solvent Extract methods liquid compared by the extract adopting ultrasonic disruption extractive technique to obtain, and the chromatographic peak area of its flavor component enlarges markedly, and maximum amplification can reach 88.00%, and average amplification can reach 44.40%.The extraction effect of visible ultrasonic disruption extractive technique is not only better than consuming steam distillation that is large, poor repeatability, even than the better effects if of organic solvent soak extraction 24h.
The tobacco flavor comparison of ingredients (chromatographic peak area) of the GC-MS detection of table 1 two kinds of extracting methods
Embodiment 3
Sample is the sheet cigarette tobacco leaf after the tobacco redrying of producing region, Anhui.Tobacco leaf is positioned in climatic chamber, at 25 DEG C, Balance Treatment 48h under 60% damp condition.Shred with scissors, size Control, within 1.5cm × 1.5cm, then accurately takes 1g smoked sheet, loads in 50mL round bottom band spiral cover plastic tube, adds 30mL methyl alcohol, and be positioned over freezing dipping 5min in ice-water bath; Afterwards solution is positioned in Ultrasonic Cell Disruptor, the ultrasonic amplitude transformer of 6mm diameter is inserted in Extraction solvent, and arranging ultrasonic power is 665W, the continuous ultrasound time is 3s, intermittent time is 9s, and circulation is carried out and is ultrasonicly always lasted for 15min, utilizes ultrasonic grind smoked sheet.Ultrasonication terminates rear airtight container, continues Soakage extraction 5min.By suction pipe, mixed slurry is moved in 2mL centrifuge tube, setting centrifugal speed is 5000rpm, centrifugal 5min.Getting supernatant 1mL adds in chromatogram bottle, gas chromatography combined with mass spectrometry analysis to be entered.
Embodiment 4
Get 7 parts, sample after the sheet cigarette chopping after with the producing region tobacco redrying of a collection of Anhui respectively, every part is 1g, the method specified by above-described embodiment 3 is extracted, combined gas chromatography mass spectrometry sample introduction in the present invention is adopted to analyze, NIST05 database (matching degree >=90) is used to carry out qualitative, and adopt internal standard method to carry out semi-quantitative analysis to tobacco flavor composition, measure the chromatographic peak area of various tobacco flavor composition, repeated concrete outcome is in table 2 and Fig. 3.
Table 2 tobacco flavor composition repeatability investigates result (chromatographic peak area)
Shown by result in table 2, the peak area RSD of various flavor component is all less than 10%, and illustrate that the method repeatability is good, measurement result is accurate, can apply in real work.
Embodiment 5
Sample is producing region, Anhui tobacco leaf fragment.Shredded by smoked sheet scissors, size Control, within 1.5cm × 1.5cm, then takes 10g smoked sheet, loads in 500mL conical flask, adds 300mL ethanol, and be positioned over freezing dipping 10min in ice-water bath; Afterwards solution is positioned in Ultrasonic Cell Disruptor, the ultrasonic amplitude transformer of 6mm diameter is inserted in Extraction solvent, and arranging ultrasonic power is 665W, the continuous ultrasound time is 3s, intermittent time is 9s, and circulation is carried out and is ultrasonicly always lasted for 30min, utilizes ultrasonic grind smoked sheet.Ultrasonication terminates rear airtight container, continues Soakage extraction 5min.By suction pipe, mixed slurry is moved in 50mL centrifuge tube, setting centrifugal speed is 5000rpm, centrifugal 5min.Getting supernatant joins in 500mL round-bottomed flask, is spin-dried for, obtains leaf tobacco extract in 40 DEG C of water-baths.
Embodiment 6
Sample is producing region, Anhui tobacco leaf fragment.Shredded by smoked sheet scissors, size Control, within 1.5cm × 1.5cm, then takes 10g smoked sheet, loads in 500mL conical flask, adds 100mL methyl tertiary butyl ether(MTBE), and be positioned over freezing dipping 20min in ice-water bath; Afterwards solution is positioned in Ultrasonic Cell Disruptor, the ultrasonic amplitude transformer of 6mm diameter is inserted in Extraction solvent, and arranging ultrasonic power is 500W, the continuous ultrasound time is 2s, intermittent time is 5s, and circulation is carried out and is ultrasonicly always lasted for 30min, utilizes ultrasonic grind smoked sheet.Ultrasonication terminates rear airtight container, continues Soakage extraction 5min.By suction pipe, mixed slurry is moved in 50mL centrifuge tube, setting centrifugal speed is 5000rpm, centrifugal 5min.Getting supernatant joins in 500mL round-bottomed flask, is spin-dried for, obtains leaf tobacco extract in 40 DEG C of water-baths.
Embodiment 7
Sample is producing region, Anhui tobacco leaf fragment.Shredded by smoked sheet scissors, size Control, within 1.5cm × 1.5cm, then takes 5g smoked sheet, loads in 500mL conical flask, adds 125mL methyl tertiary butyl ether(MTBE), and be positioned over freezing dipping 15min in ice-water bath; Afterwards solution is positioned in Ultrasonic Cell Disruptor, the ultrasonic amplitude transformer of 6mm diameter is inserted in Extraction solvent, and arranging ultrasonic power is 950W, the continuous ultrasound time is 5s, intermittent time is 10s, and circulation is carried out and is ultrasonicly always lasted for 10min, utilizes ultrasonic grind smoked sheet.Ultrasonication terminates rear airtight container, continues Soakage extraction 20min.By suction pipe, mixed slurry is moved in 50mL centrifuge tube, setting centrifugal speed is 5000rpm, centrifugal 5min.Getting supernatant joins in 500mL round-bottomed flask, is spin-dried for, obtains leaf tobacco extract in 40 DEG C of water-baths.
Embodiment 8
Sample is producing region, Anhui tobacco redrying rear blade.Getting 50 blades from redrying tail stacks neatly, and sampled from the direction perpendicular to blade face by diameter 1.5cm stainless steel probe tube, obtain 50 wafer samples, blade face remainder can drop into machining production line again.Wafer sample is positioned in climatic chamber, at 25 DEG C, Balance Treatment 48h under 60% damp condition.Then precise example weight, loads in 50mL round bottom band spiral cover plastic tube, adds 20mL absolute ethyl alcohol, and be positioned over freezing dipping 5min in ice-water bath; Afterwards solution is positioned in Ultrasonic Cell Disruptor, the ultrasonic amplitude transformer of 6mm diameter is inserted in Extraction solvent, and arranging ultrasonic power is 665W, and the continuous ultrasound time is 3s, and the intermittent time is 9s, and circulation is carried out and is ultrasonicly always lasted for 20min.Ultrasonication terminates rear airtight container, continues Soakage extraction 5min.By suction pipe, mixed slurry is moved in 2mL centrifuge tube, setting centrifugal speed is 5000rpm, centrifugal 5min.Getting supernatant 1mL adds in chromatogram bottle, pending gas chromatography combined with mass spectrometry analysis.
From above treatment step, adopt the extractive technique in the present invention, without the need to making pulverization process in advance to tobacco leaf, by contrast, traditional steam distillation or organic solvent extraction, at sample making course for producing a sample, often need to dry and abrasive dust process the tobacco leaf of about 100g, can accomplish " sampling as required ", unwanted tobacco portion is dropped into machining production line again, significantly can reduce the tobacco leaf waste that sample making course causes.
In sum, the invention provides a kind of tobacco flavor component extracting method and application thereof, by adopting ultrasonic disruption extractive technique, without the need to making pulverization process in advance to pipe tobacco or tobacco leaf, significantly reduce the tobacco leaf waste that sample making course causes, effective minimizing flavor component scatters and disappears, extraction efficiency is high, simplifies extraction process, does not affect the structures and characteristics of flavor component in tobacco, and effectively can obtain the semi-quantitative results of flavor component in tobacco, can also be used for producing tobacco extract.So the present invention effectively overcomes various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (9)
1. a tobacco flavor component extracting method, comprises the following steps:
1) pretreatment: pipe tobacco or tobacco leaf are carried out Balance Treatment or dry process, make sample moisture content even;
2) pre-preg process: by step 1) gained pipe tobacco or tobacco leaf, after putting into Extraction solvent dipping, cooling;
3) ultrasonic grind: by step 2) gained mixed liquor puts into Ultrasonic Cell Disruptor, utilizes ultrasonic grind pipe tobacco or tobacco leaf;
Described ultrasonic grind condition is: ultrasonic power: 500 ~ 950W; Ultrasonic amplitude of fluctuation shank diameter: 2-15mm; The ultrasonic circulation time: ultrasonic time 2-5s, intermittent time 5-10s, circulation is carried out and is ultrasonicly always lasted for 10-30min; Described ultrasonic grind carries out in ice-water bath;
4) obtain tobacco flavor composition: after pulverizing pipe tobacco or tobacco leaf, airtight container, after continuing dipping, centrifugal segregation solid formation, namely obtains tobacco flavor constituents extraction liquid.
2. a kind of tobacco flavor component extracting method according to claim 1, is characterized in that, as step 1) as described in Balance Treatment be pipe tobacco or tobacco leaf are positioned in climatic chamber balance; The temperature of described Balance Treatment is 20-30 DEG C, and humidity is 55-65%; The time of described Balance Treatment is 48h.
3. a kind of tobacco flavor component extracting method according to claim 1, is characterized in that, as step 1) as described in dry process be pipe tobacco or tobacco leaf are positioned in air dry oven carry out drying; The temperature of described drying process is 45-55 DEG C; The time of described drying process is 4h.
4. a kind of tobacco flavor component extracting method according to claim 1, is characterized in that, as step 2) as described in Extraction solvent to be selected from water, methyl alcohol, ethanol, methyl tertiary butyl ether(MTBE) one or more combinations; Described Extraction solvent addition is the 10-25 times amount of pipe tobacco or tobacco leaf; Described dip time is 5-20min.
5. a kind of tobacco flavor component extracting method according to claim 1, is characterized in that, as step 2) as described in cooling carry out in ice-water bath.
6. a kind of tobacco flavor component extracting method according to claim 1, is characterized in that, as step 4) as described in continuation dip time be 5-20min; Described centrifugation time is 5min, and centrifugal speed is 5000rpm.
7. according to the application of the arbitrary described a kind of tobacco flavor component extracting method of claim 1-6 in tobacco flavor component content is analyzed.
8. a content analysis method for tobacco flavor composition, comprises the following steps:
A) pretreatment: the step 1 adopting tobacco flavor component extracting method described in the arbitrary claim of claim 1-6) process;
B) pre-preg process: the step 2 adopting tobacco flavor component extracting method described in the arbitrary claim of claim 1-6) process;
C) ultrasonic grind: the step 3 adopting tobacco flavor component extracting method described in the arbitrary claim of claim 1-6) process;
D) tobacco flavor composition is obtained: the step 4 adopting tobacco flavor component extracting method described in the arbitrary claim of claim 1-6) process;
E) constituent analysis: adopt combined gas chromatography mass spectrometry determination step D) described in the content of flavor component in tobacco.
9. producing the application in tobacco extract according to the arbitrary described a kind of tobacco flavor component extracting method of claim 1-6.
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| CN106404966B (en) * | 2016-11-09 | 2019-04-26 | 湖北中烟工业有限责任公司 | A kind of pre-treating method of reconstituted tobacco aroma component analysis |
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