CN108845085A - A method of tobacco leaf odor type is predicted based on tobacco leaf chemical composition - Google Patents
A method of tobacco leaf odor type is predicted based on tobacco leaf chemical composition Download PDFInfo
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- 238000012360 testing method Methods 0.000 claims abstract description 17
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
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- 235000013734 beta-carotene Nutrition 0.000 claims description 3
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- 239000001656 lutein Substances 0.000 claims description 3
- KBPHJBAIARWVSC-RGZFRNHPSA-N lutein Chemical compound C([C@H](O)CC=1C)C(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\[C@H]1C(C)=C[C@H](O)CC1(C)C KBPHJBAIARWVSC-RGZFRNHPSA-N 0.000 claims description 3
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- 229910001414 potassium ion Inorganic materials 0.000 claims description 3
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- OENHQHLEOONYIE-JLTXGRSLSA-N β-Carotene Chemical compound CC=1CCCC(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C OENHQHLEOONYIE-JLTXGRSLSA-N 0.000 claims description 3
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0098—Plants or trees
Abstract
The present invention relates to a kind of method based on tobacco leaf chemical composition prediction tobacco leaf odor type, this method includes:Step(1), sample collection;Step(2), standard sample smokes panel test;Step(3), chemical constituents determination;Step(4), screening odor type key index;Step(5), establish discriminant function go forward side by side hold or participate in a prayer service at a temple type differentiation.The accuracy of tobacco leaf odor type prediction can be improved in the present invention, greatly reduce the workload that artificial sense is smoked panel test, it only needs that quickly accurate qualitative description can be carried out to tobacco leaf odor type on the model that early period establishes, identifies that tobacco leaf odor type style provides foundation for formulator.
Description
Technical field
The present invention relates to a kind of methods for predicting tobacco leaf odor type, especially a kind of to predict tobacco incense based on tobacco leaf chemical composition
The method of type belongs to Tobacco Analysis field.
Background technique
The tobacco leaf odor type of flue-cured tobacco is traditionally divided into delicate fragrance type, flat-flavor and three kinds of Luzhou-flavor.Tobacco leaf odor type is by people
Taste and smell determine, when facing large batch of tobacco sample, larger workload and inevitably there is deviation, and it is time-consuming compared with
It is long.
Based on this, the prior art proposes the discriminant method of the tobacco leaf strong-flavor style highlight degree based on flavor component,
Mainly using Support vector regression model to the quantitative relationship of four kinds of characteristic indexs and tobacco leaf strong-flavor style highlight degree
It is simulated, the discrimination model of the tobacco leaf strong-flavor style highlight degree based on flavor component is established, by model to unknown
Sample strong-flavor style highlight degree is differentiated;In addition, the prior art also establishes one kind based on perfume using similar method
The method of discrimination of the tobacco leaf coke sweet tea sense taste characteristics of taste ingredient.
However, above method is based on detection tobacco leaf aroma component, utilizes Support vector regression Model checking.The differentiation
Method depends on this index of aroma component, although however sensory evaluating smoking's result of tobacco leaf be closely related with aroma component,
But and not exclusive correlation, thus, lack persuasion, it is as a result not accurate enough, and measure aroma component when, often target is unknown
Really, need largely to detect many unrelated substances.
Summary of the invention
In order to solve the above-mentioned technical problem, the present invention proposes a kind of side based on tobacco leaf chemical composition prediction tobacco leaf odor type
Method, the present invention analyze the indexs such as aroma component relevant to tabacum sensory, routine chemical components, organic acid, polyphenol comprehensively,
Main indicator relevant to tobacco leaf odor type is obtained after screening, and establish using the discriminant function based on the above main indicator to
It predicts tobacco leaf different flavor, can more accurately determine the odor type of tobacco leaf.Method of the invention is achieved through the following technical solutions:
A method of tobacco leaf odor type is predicted based on tobacco leaf chemical composition, is included the following steps:
Step (1), sample collection
Several cured tobacco leaf samples of delicate fragrance type, flat-flavor, Luzhou-flavor cigarette district are collected respectively, it is random in above-mentioned sample
It extracts a part and is used as sample to be tested, remaining is as standard modeling sample;
Step (2), standard modeling sample are smoked panel test
Cigarette is made in each standard modeling sample tobacco leaf a part and carries out sensory evaluating smoking, and faint scent is carried out to standard sample
Type, flat-flavor and Luzhou-flavor identify and sort out;Another part is used for chemical constituents determination;
Step (3), chemical constituents determination
Routine chemical components, organic acid, polyphenol, pigment and aroma component measurement are carried out to standard modeling sample tobacco leaf;
Step (4), the key index for screening odor type
Correlation analysis is carried out to standard modeling sample sensory evaluating smoking result and chemical constituents determination result, according to correlation
The key index that size filters out odor type is total reducing sugar, total nitrogen, malic acid and Megastigmatrienone;
Step (5), establish discriminant function go forward side by side hold or participate in a prayer service at a temple type differentiation
Discriminant function is established using mahalanobis distance, is obtained:
Delicate fragrance type:F1(x)=41.844X1+13.235X5-10.386X3+5.195X4-20.329;
Flat-flavor:F2(x)=- 148.737X1+50.983X2+125.189X3+34.867X4-55.28;
Luzhou-flavor:F3(x)=- 65.955X1-31.425X2+65.815X3+24.057X4-21.519;
Wherein X1For total sugar content, X2For total nitrogen content, X3For malic acid content, X4For Megastigmatrienone content, measurement to
Total sugar content, total nitrogen content, malic acid content and the Megastigmatrienone content of sample, the corresponding total reducing sugar of sample to be tested is contained
Amount, total nitrogen content, malic acid content and Megastigmatrienone content substitute into F respectively1(x)、F2(x) and F3(x), the perfume (or spice) of sample to be tested
Type W=max { Fi };
Step (6), discriminant function are examined
For modeling sample, whether there is erroneous judgement by the above-mentioned discriminant function of validation-cross.
Further, routine chemical components include total nitrogen, total reducing sugar, potassium ion, chloride ion, reduced sugar and nicotine;Organic acid
Including citric acid, linoleic acid, isovaleric acid, malic acid and caproic acid;Polyphenol includes chlorogenic acid and scopoletin;Pigment include lutein and
Beta carotene;Aroma component includes bread ketone, furfural, benzyl alcohol, Megastigmatrienone and pungent value diene.
Further, routine chemical components use YC/T159-2002, YC/T161-2002, YC/T217-2007, YC/
T162-2011 and YC/T 468-2013;Organic acid uses YC/T 500-2014;Tobacco leaf polyphenol uses YC/T202-2006;Cigarette
The detection of leaf aroma component uses gas chromatography-mass spectrometry analysis;Tobacco sensory quality is smoked panel test by DB53/T182.3-2006.
Further, the condition of gas chromatography-mass spectrometry analysis is:
Capillary column:HP-5MS, 30m × 0.25mm × 0.25m;Injector temperature:240℃;Carrier gas:He, 1mL/min;
Temperature programming:50 DEG C of initial temperature, 1min is kept, is warming up to 160 DEG C with 8 DEG C/min, keeps 2min, then with 8 DEG C/min heating
To 260 DEG C, 15min is kept;Sample volume:2 μ L, split ratio:25:1;Transmission line temperature:280℃;Ionization mode:EI, ionization energy
Amount:70eV;Ion source temperature:230℃;Level four bars temperature:160℃;Mass range 35-455aum.
Further, before gas chromatography-mass spectrometry analysis, by milled 60 mesh sieve of sample, in temperature 22 in tandem-driving bogie
DEG C, the offal sample 25.0g after accurately weighing balance for 24 hours is balanced under conditions of humidity 60%, is put into SDE method
In, and the internal standard compound of fixed amount is added, dynamic extraction 2h is carried out continuously to pipe tobacco as solvent using methylene chloride.Gained
It is 1.0mL that constant volume, which is concentrated, in extract after drying, and concentrate is analyzed using gas chromatography-mass spectrum.
Compared with the prior art, the advantages of the present invention are as follows:
1, the present invention analyzes aroma component relevant to tabacum sensory, routine chemical components, organic acid, polyphenol comprehensively
Etc. indexs, main indicator relevant to tobacco leaf odor type is obtained after screening, and use discriminant by distance (mahalanobis distance method), with Europe
Unlike family name's distance, in view of the connection between various characteristics, we can effectively analyze tobacco leaf in this way
Connection between inherent component target.
Establish and use the discriminant function based on the above main indicator, to predict tobacco leaf different flavor, can it is more acurrate really
Determine the odor type of tobacco leaf.
2, only analysis tobacco leaf intrinsic chemical ingredient can differentiate the odor type style and features of tobacco leaf to the present invention.It is more in sample size
In the case where, only by total sugar content, total nitrogen content, malic acid content and Megastigmatrienone content, can be conducive to quickly
Accurate qualitative description is carried out to tobacco leaf odor type, artificial sense can be reduced and smoked panel test workload, without measuring other unrelated changes
It studies point, economizes on resources and the time, quickly and accurately identify that tobacco style provides foundation for formulator.
Specific embodiment
It is clearly and completely described below in conjunction with the technical solution in embodiment, it is clear that described embodiment is only
It is only rather than whole example to a part of example of the present invention.Based on the embodiments of the present invention, ordinary skill people
Member's every other embodiment obtained under that premise of not paying creative labor, shall fall within the protection scope of the present invention.
Embodiment 1
The method based on tobacco leaf chemical composition prediction tobacco leaf odor type of the present embodiment, includes the following steps:
Step (1), sample collection
Collect respectively by Hongta Group provide delicate fragrance type, flat-flavor, Luzhou-flavor cigarette district junior tobacco leaf sample 508
Part, wherein 437 parts of sample, 71 parts of verification sample for modeling.
Step (2), standard sample are smoked panel test
Assert that the tobacco sensory quality evaluation personnel of qualification forms 20-25 people appraisal group by country, treats modeling sample
Tobacco leaf odor type carry out identification of smokeing panel test;Sample only provides number, does not provide any information (such as place, grade in addition to number
Deng), prevent human factor from influencing qualification result;The qualification result of flue-cured tobacco flavor types is divided into delicate fragrance type, flat-flavor, Luzhou-flavor three
Kind.
By each modeling sample tobacco leaf a part be made cigarette carry out sensory evaluating smoking, and to standard sample carry out delicate fragrance type,
Flat-flavor and Luzhou-flavor identify and sort out;Another part is used for chemical constituents determination;It is consistent with test sample to keep smokeing panel test
Property, tobacco leaf tears off and is divided into two to symmetry after master pulse, and a copy of it preparation is smoked panel test cigarette, another preparation test sample.
Step (3), chemical constituents determination
Routine chemical components, organic acid, polyphenol, pigment and aroma component measurement are carried out to modeling tobacco sample;Wherein, often
Advising chemical component includes total nitrogen, total reducing sugar, potassium ion, chloride ion, reduced sugar and nicotine etc.;Organic acid include citric acid, linoleic acid,
Isovaleric acid, malic acid and caproic acid etc.;Polyphenol includes chlorogenic acid and scopoletin etc.;Pigment includes lutein, beta carotene etc.;It causes
Fragrant ingredient includes bread ketone, furfural, benzyl alcohol, Megastigmatrienone and pungent value diene etc..
Routine chemical components using YC/T159-2002, YC/T161-2002, YC/T217-2007, YC/T162-2011 and
YC/T 468-2013;Organic acid uses YC/T 500-2014;Tobacco leaf polyphenol uses YC/T202-2006;The inspection of tobacco leaf aroma component
It surveys and uses gas chromatography-mass spectrometry analysis;Tobacco sensory quality is smoked panel test by DB53/T182.3-2006.
The instrument used in gas chromatography-mass spectrometry analysis is as follows:
Existing distilling and extracting device;R114 Rotary Evaporators (B ü CHI company of Switzerland);6890N/5975N gas-chromatography/
Mass spectrometer uses HP-5MS capillary chromatographic column (Agilent company of the U.S.).
Analysis method is as follows:
By milled 60 mesh sieve of sample, balanced for 24 hours under conditions of 22 DEG C of temperature, humidity 60% in tandem-driving bogie, it is quasi-
Offal sample 25.0g after really weighing balance, is put into SDE method, and the internal standard compound of fixed amount is added,
Dynamic extraction 2h is carried out continuously to pipe tobacco as solvent using methylene chloride.It is extract obtained after drying concentration constant volume be
1.0mL.Concentrate is analyzed using Gc-mss instrument, and gained map composes library (NIST98, Wiley275) through computer
It retrieves, and calculates the relative amount at each peak with Internal standard correction methods normalization method.
Instrument condition is as follows:
Capillary column:HP-5MS(30m 0.25mm 0.25m);Injector temperature:240℃;Carrier gas:He, 1mL/min;Journey
Sequence heating:50 DEG C of initial temperature, 1min is kept, 160 DEG C is warming up to 8 DEG C/min, keeps 2min, then be warming up to 8 DEG C/min
260 DEG C, keep 15min;Sample volume:2 μ L, split ratio:25:1;Transmission line temperature:280℃;Ionization mode:EI, ionizing energy:
70eV;Ion source temperature:230℃;Level four bars temperature:160℃;Mass range 35-455aum.
Step (4), the key index for screening odor type
It is related to the progress of chemical constituents determination result to modeling sample sensory evaluating smoking result using SPSS17.0 analysis software
Property analysis, according to correlation size filter out odor type key index be total reducing sugar, total nitrogen, malic acid and Megastigmatrienone;
Step (5), establish discriminant function go forward side by side hold or participate in a prayer service at a temple type differentiation
Discriminant function is established using mahalanobis distance, the results are shown in Table 1.
1 Fischer discriminant function coefficient table of table
According to correlation results, obtain constructing cured tobacco leaf using total reducing sugar, total nitrogen, malic acid, Megastigmatrienone as independent variable
The function of odor type, obtains:
Delicate fragrance type:F1(x)=41.844X1+13.235X5-10.386X3+5.195X4-20.329;
Flat-flavor:F2(x)=- 148.737X1+50.983X2+125.189X3+34.867X4-55.28;
Luzhou-flavor:F3(x)=- 65.955X1-31.425X2+65.815X3+24.057X4-21.519;
Wherein X1For total sugar content, X2For total nitrogen content, X3For malic acid content, X4For Megastigmatrienone content, measurement to
Total sugar content, total nitrogen content, malic acid content and the Megastigmatrienone content of sample, the corresponding total reducing sugar of sample to be tested is contained
Amount, total nitrogen content, malic acid content and Megastigmatrienone content substitute into F respectively1(x)、F2(x) and F3(x), the perfume (or spice) of sample to be tested
Type W=max { Fi }.
Step (6), discriminant function are examined
For discriminant analysis, the discriminant function established be used to discriminate accuracy rate be it is vital, it is general with from
Body proof method and cross verification sentence to raw sample, and can obtain with cross verification higher compared with own verification method
False Rate, it is higher time to sentence result credibility.The results are shown in Table 2 for the validation-cross of the discriminant function of the present embodiment.
The validation-cross result of 2 discriminant function of table
Note:1=delicate fragrance type, 2=flat-flavor, 3=Luzhou-flavor.
In table 2, initial part is the differentiation result using commonsense method to every record in training sample, it can be seen that should
Discriminant function does not misjudge verifying sample, and classification accuracy reaches 100.0%, and validation-cross partial results and commonsense method are complete
It is exactly the same, thus the discriminant function be it is stable, the prediction effect of discriminant function is good, have practical application value.
Step (7), prediction result compare
Cigarette is made in another part of sample to be tested tobacco leaf, is smoked panel test by the method for smokeing panel test of step (2).By step
(5) result is made comparisons with artificial smoking result, and the results are shown in Table 3:
The tobacco sample to be verified of table 3 is manually evaluated and discriminant function prediction result
Note:1=delicate fragrance type, 2=flat-flavor, 3=Luzhou-flavor;UI expression not can determine that.
It is calculated according to result and differentiates that the accuracy rate of prediction is 91.5% using discriminant function development odor type, illustrated based on tobacco leaf
The technical method of chemical component prediction tobacco leaf odor type is feasible, effective.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of method based on tobacco leaf chemical composition prediction tobacco leaf odor type, it is characterised in that:Include the following steps:
Step(1), sample collection
Several cured tobacco leaf samples for collecting delicate fragrance type, flat-flavor, Luzhou-flavor cigarette district respectively, are randomly selected in above-mentioned sample
A part is used as sample to be tested, remaining is as standard modeling sample;
Step(2), standard modeling sample smokes panel test
By each standard modeling sample tobacco leaf a part be made cigarette carry out sensory evaluating smoking, and to standard sample carry out delicate fragrance type,
Flat-flavor and Luzhou-flavor identify and sort out;Another part is used for chemical constituents determination;
Step(3), chemical constituents determination
Routine chemical components, organic acid, polyphenol, pigment and aroma component measurement are carried out to standard modeling sample tobacco leaf;
Step(4), screening odor type key index
Correlation analysis is carried out to standard modeling sample sensory evaluating smoking result and chemical constituents determination result, according to correlation size
The key index for filtering out odor type is total reducing sugar, total nitrogen, malic acid and Megastigmatrienone;
Step(5), establish discriminant function go forward side by side hold or participate in a prayer service at a temple type differentiation
Discriminant function is established using mahalanobis distance, is obtained:
Delicate fragrance type:F1(x) = 41.844X1 +13.235 X5-10.386X3+5.195X4-20.329;
Flat-flavor:F2(x)=-148.737X1 +50.983X2 +125.189X3+34.867X4-55.28;
Luzhou-flavor:F3(x)=-65.955X1 -31.425X2 +65.815X3+24.057X4-21.519;
Wherein X1For total sugar content, X2For total nitrogen content, X3For malic acid content, X4For Megastigmatrienone content, measure to test sample
Total sugar content, total nitrogen content, malic acid content and the Megastigmatrienone content of product, by the corresponding total sugar content of sample to be tested, always
Nitrogen content, malic acid content and Megastigmatrienone content substitute into F respectively1(x),F2(x)And F3(x), the odor type W=of sample to be tested
max{Fi};
Step(6), discriminant function examine
For modeling sample, whether there is erroneous judgement by the above-mentioned discriminant function of validation-cross.
2. according to the method described in claim 1, it is characterized in that:Routine chemical components include total nitrogen, total reducing sugar, potassium ion, chlorine
Ion, reduced sugar and nicotine;Organic acid includes citric acid, linoleic acid, isovaleric acid, malic acid and caproic acid;Polyphenol includes chlorogenic acid
And scopoletin;Pigment includes lutein and beta carotene;Aroma component includes bread ketone, furfural, benzyl alcohol, Megastigmatrienone
With pungent value diene.
3. according to the method described in claim 1, it is characterized in that:Routine chemical components use YC/T159-2002, YC/
T161-2002, YC/T217-2007, YC/T162-2011 and YC/T 468-2013;Organic acid uses YC/T 500-2014;Cigarette
Leaf polyphenol uses YC/T202-2006;The detection of tobacco leaf aroma component uses gas chromatography-mass spectrometry analysis;Tobacco sensory quality is smoked panel test
By DB53/T182.3-2006.
4. according to the method described in claim 3, it is characterized in that:The condition of gas chromatography-mass spectrometry analysis is:
Capillary column:HP-5MS, 30m × 0.25mm × 0.25m;Injector temperature:240℃;Carrier gas:He, 1mL/min;Program
Heating:50 DEG C of initial temperature, 1min is kept, 160 DEG C is warming up to 8 DEG C/min, keeps 2min, then be warming up to 260 with 8 DEG C/min
DEG C, keep 15min;Sample volume:2 μ L, split ratio:25:1;Transmission line temperature:280℃;Ionization mode:EI, ionizing energy:
70eV;Ion source temperature:230℃;Level four bars temperature:160℃;Mass range 35-455aum.
5. according to the method described in claim 3, it is characterized in that:Before gas chromatography-mass spectrometry analysis, by milled 60 mesh of sample
Sieve balances the offal sample after accurately weighing balance for 24 hours in tandem-driving bogie under conditions of 22 DEG C of temperature, humidity 60%
25.0g is put into SDE method, and the internal standard compound of fixed amount is added, using methylene chloride as solvent pair
Pipe tobacco is carried out continuously dynamic extraction 2h.The extract obtained constant volume of concentration after drying is 1.0mL, and concentrate uses gas-chromatography-
Mass spectrum is analyzed.
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