CN103226135B - Detection and determination method for flavor type of flue-cured tobacco - Google Patents

Detection and determination method for flavor type of flue-cured tobacco Download PDF

Info

Publication number
CN103226135B
CN103226135B CN201210388375.0A CN201210388375A CN103226135B CN 103226135 B CN103226135 B CN 103226135B CN 201210388375 A CN201210388375 A CN 201210388375A CN 103226135 B CN103226135 B CN 103226135B
Authority
CN
China
Prior art keywords
flue
cured tobacco
extraction
type
tobacco
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201210388375.0A
Other languages
Chinese (zh)
Other versions
CN103226135A (en
Inventor
李晋明
董伟
任继阳
孟昭宇
郭仁
台希
朱慧贤
吴亿勤
张伟
李忠任
许健
秦云华
汤建国
张凤梅
龚文岗
桂永发
冯磊
戚文辉
汤利民
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hongta Tobacco Group Co Ltd
Original Assignee
Hongta Tobacco Group Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hongta Tobacco Group Co Ltd filed Critical Hongta Tobacco Group Co Ltd
Priority to CN201210388375.0A priority Critical patent/CN103226135B/en
Publication of CN103226135A publication Critical patent/CN103226135A/en
Application granted granted Critical
Publication of CN103226135B publication Critical patent/CN103226135B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention relates to a detection and determination method for flavor type of flue-cured tobacco, which belongs to the technical field of gradient qualitative and quantitative discriminating application for flavor type of flue-cured tobacco. The invention belongs to initiation, and is characterized in that through a simultaneous distillation-extraction (SDE ) optimization method on a flue-cured tobacco aroma substance, on the base that the current simultaneous distillation-extraction (SDE ) optimization method can extract more aroma substances than that of a traditional simultaneous distillation-extraction (SDE ), qualitative and quantitative analysis on the flue-cured tobacco aroma substances can be carried out, so that the method provides digitalized flue-cured tobacco aroma substance chemical base data for the application technical field. By optimizing the flue-cured tobacco aroma substance analysis and calculating by contrasting the index Y of flue-cured tobacco flavor type, the flue-cured tobacco flavor type scope can be accurately determined from qualitative to quantitative analysis (digitalization): delicate fragrance type, intermediate fragrance type and strong aroma type. According to the invention, the flavor type determination accuracy is 91.1%. The detection and determination method for flavor type of flue-cured tobacco provides data-orienting determination standard for flavor type gradient classification of flue-cured tobacco, tobacco leaf purchasing, maintenance and research exploitation of a tobacco blend formula of brand style and characteristic, and the formula of the essence and perfume.

Description

A kind of detection decision method of flue-cured tobacco flavor types
Technical field:
The inventive method relates to a kind of flue-cured tobacco flavor types and detects decision method, belong to flue-cured tobacco flavor types gradient qualitative, quantitatively differentiate applied technical field.For the classification of odor type gradient, the tobacco leaf buying of flue-cured tobacco, the ginseng of the maintenance of brand style and features tobacco leaf formulation and research and development, essence and flavoring agent is joined, and the chemistry judgement of datumization is provided.
Background technology
Cigarette is generally divided into four classes by its manufacture craft: mixed type, fire-cured tobacco type, outer odor type, cigar type.Major ingredient is different, and taste is different, and the cigarette of China is generally fire-cured tobacco type, also claims Chinese-style cigarette; External cigarette is generally mixed type.Mixed type is raw material by burley tobaccos, Turkish tobaccos, flue-cured tobacco etc., and tar content is lower than fire-cured tobacco type.Hybrid cigarette is compared maximum advantage with fire-cured tobacco type cigarette be exactly that perfume quantity foot and tar content are low.
China is vast in territory, and each Climate and edaphic condition are different, and the flue-cured tobacco raw material of producing differs greatly in cigarette matter characteristic.The 1950's, the characteristic aroma while sucking according to flue-cured tobacco, is divided into three types, i.e. delicate fragrance type, middle odor type, Luzhou-flavor.
1. delicate fragrance type: fragrance is elegant elegant, has fresh and sweet note, and fragrance sensing speed is fast, and diffusive force is strong, is the key factor that gives good fragrance sensation, and jealous comfortable, smoke concentration is lighter, and the assorted gas of region is lighter, and strength is soft to moderate, represents type Yunnan, the tobacco leaf in Fujian.
2. middle odor type: fragrance is pure stable, and this perfume of tobacco is outstanding, and fragrance sensing speed is medium, be the main aroma of cigarette product, jealous clean, smoke concentration is lighter to denseer, the assorted gas of region has to larger, and strength is soft to larger, represents the tobacco leaf in type Guizhou, Shandong and northeast.
3. Luzhou-flavor: the dense fragrance of fragrance is heavy to overflow, and has burnt fragrant and sweet rhythm, and fragrance sensing speed is slower, long abundant, jealous comfortable, and the assorted gas of region is very light to heavier, and strength is moderate, represents the tobacco leaf in type Henan, Hunan, Anhui.
Because flue-cured tobacco flavor types has gradient, people's correspondence is given certain numerical value, and numerical value is worth from low value to height.According to tobacco leaf odor type, there is the gradient implication from delicate fragrance type to Luzhou-flavor, can adopt the method for assignment, odor type is transformed into numerical value index by qualitative index.By the ascending assignment that gives of delicate fragrance type, middle odor type and Luzhou-flavor.Assignment according to being to take the Typical Representative that Yunnan tobacco, cigarette Yuxi (soft) be delicate fragrance type, statistically according to the chemical composition analyzing and content assignment.
Flue-cured tobacco flavor types has certain gradient: delicate fragrance type--middle odor type--Luzhou-flavor.Convenient for distinguishing odor type, people are by flue-cured tobacco flavor types: delicate fragrance type, middle odor type and Luzhou-flavor are subdivided into again: delicate fragrance type--clearly partially--in partially clear--middle odor type--in partially dense--dense partially in--Luzhou-flavor; Corresponding assignment is: 1.8--2.13--2.46--2.8--3.13--3.46--3.8.
The Li Zhang of Chinese University of Science and Technology sets up in sea flue-cured tobacco flavor types index Y, the middle part blade of different regions flue-cured tobacco of take is material, measure its fragrance component and routine chemical components, and tobacco leaf is carried out to thin material and smoke panel test. adopt the method for successive Regression to set up cured tobacco leaf odor type exponential model.
Wherein to take in sea 36 kinds of fragrance components of 122 cigarette samples and the content of 6 kinds of routine chemical componentses be independent variable to the Li Zhang of Chinese University of Science and Technology, and the tobacco leaf odor type indicial equation that the odor type (assignment) of take is dependent variable is as follows:
Y odor type index=1.61+0.018X isovaleric acid+ 0.027X benzoic acid+ 0.027X solanone+ 0.039X dihydro-β ionol+ 0.265X dihydroactinidiolide+ 0.005X the rare ketone of huge beans three+ 0.019X farnesyl acetone-0.048X damascenone-0.155 methyl hexadecanoate,
Coefficient of multiple correlation R=0.941 of this regression equation, coefficient of determination R 2=0.886, P=0.
Apply above-mentioned flue-cured tobacco flavor types index Y, can help people tentatively to judge odor type, but it is independent variable that this cured tobacco leaf odor type exponential model only adopts the content of 36 kinds of fragrance components and 6 kinds of routine chemical componentses, therefore 87.9%, there is the not high enough shortcoming of reliability in judging nicety rate.
Summary of the invention
The object of the invention is to overcome the shortcoming of above-mentioned prior art.The tobacco of optimizing causes (SDE) extracting process of perfumery, obtain the perfumery chemical fundamentals technical data that cause more, again by the calculating that causes perfumery analysis and contrast flue-cured tobacco flavor types index Y to flue-cured tobacco, can be more exactly from qualitativeization to quantification (digitizing) determine the scope of flue-cured tobacco flavor types: delicate fragrance type, middle odor type, Luzhou-flavor, thereby judgement flue-cured tobacco flavor types style, for manufacturer's cigarette tobacco leaf formulation odor type (being mainly delicate fragrance type) provides the qualitative of odor type material adjustment, quantitative technique parameter, odor type gradient classification for flue-cured tobacco, tobacco leaf buying, maintenance and the research and development of brand style and features tobacco leaf formulation, essence and flavoring agent ginseng is joined quantity, the criterion of datumization is provided.
The detection decision method of a kind of flue-cured tobacco flavor types of the present invention, is characterized in that step is as follows:
(1) flue-cured tobacco flavor types causes perfumery extraction: by while distillation extraction (SDE) Optimized Extraction method, proceed as follows: in cucurbit, plan is carried out flue-cured tobacco and is caused tobacco sample 20 that perfumery analyzes or 30 grams, add water 350 or 450ml, add internal standard compound matter, in order to distillation; In extraction flask, add 40ml methylene chloride.
1. extraction time: extractant is used methylene chloride, 60 ℃ of constant temperature water baths, conventional extraction mode is carried out 3 hours;
2. extraction temperature: heating jacket vapo(u)rizing temperature is 198 ℃-200 ℃, makes boiling violent, to extract more completely the material of half volatile;
3. separated routinely: in separating funnel, dichloromethane solution to extraction adds excessive sodium sulphate, ratio is 0.5 times of tobacco sample weight, allow sodium sulphate fully absorb the moisture in the dichloromethane solution of extraction, subsequently, successively each once, with 10ml dichloromethane rinse bottle, guarantees that extract all extracts;
4. concentrated routinely: the extractant in step (3) to be concentrated into 0.5-0.4ml, to be back to 1-1.1ml;
5. the refrigeration of routinely sample of extraction in step (4) not being spent the night, the machine of directly going up carries out the makings analysis of GC-MS gas chromatography-mass spectrum.
(2) gaschromatographic mass spectrometry (GC-MS) qualitative and quantitative analysis flue-cured tobacco flavor types causes perfumery.
Described GC-MS gas chromatography-mass spectrum condition:
Chromatographic column: DB-5(30m * 0.25mmi.d. * 0.25 μ m d.f.);
Temperature programme: by the firing rate of 4 ℃/min, be warmed up to for the first time 40 ℃ of insulation 2min, be warmed up to subsequently 250 ℃, insulation 10min;
Injection port: 250 ℃; Carrier gas: He; Column cap is pressed: 100kPa;
Split ratio: 30: 1; Sample size 1.0 μ L;
Transmission line temperature: 250 ℃;
Ion source temperature: 150 ℃;
EI energy: 70eV;
Sweep limit: 35~350u;
Interior mark: n-heptadecane; To the collection of illustrative plates collecting, utilize NIST1.11 upgrade version spectrum storehouse to retrieve; Adopt area normalization standard measure;
The result of analyzing is: theoretical superiors's area of pictural surface reaches more than 0.03% can think a kind of material, because some content reality that causes perfumery is seldom, and the flue-cured tobacco in variety classes, the different places of production; One species, the flue-cured tobacco in the different places of production, what they were out analyzed causes perfumery kind generally in 120-190 kind, has comparative 101, for 89 of statistical study;
(3) analyze and judge: what adopt step (2) acquisition causes perfumery qualitative and quantitative analysis 14 kinds of materials that correlativity is large out to flue-cured tobacco, and substitution can be carried out the following formula of stepwise regression analysis by Matlab software, carry out the detection of flue-cured tobacco flavor types and judge;
Flue-cured tobacco flavor types index Y=1.875-2.702X1, (isoamyl olefine aldehydr)+0.150X2, (2-acetyl furan)+0.061X3, (phenmethylol)-0.416X4, (2-acetyl pyrrole)+0.367X5, (tea ketone)+1.053X6, (n-nonanoic acid)+0.760X7, (indoles)+0.010X8, (different solanone)+0.027X9, (large horse scholar ketone)+0.352X10, (dihydroactinidiolide)-0.029X11, (Megastigmatrienone)-0.31X12, (1 (dihydro) naphtha)+0.051X13, (farnesyl acetone)-0.281X14, (methyl hexadecanoate),
Coefficient of multiple correlation R=0.968041 of this regression equation, coefficient of determination R 2=0.937103, P=6.64 * 10 -14, the F value of odor type index return equation variance analysis reaches the level of signifiance (P≤0. 05); The partial correlation coefficient of 14 significant factor regression coefficients reaches the level of signifiance;
(4) calculate the rear corresponding flue-cured tobacco flavor types index Y numerical value that obtains, as flue-cured tobacco flavor types judgement numerical value, for the ginseng of the maintenance of the odor type gradient classification of flue-cured tobacco, tobacco leaf buying, brand style and features tobacco leaf formulation and research and development, essence and flavoring agent, join, the criterion of datumization is provided.
The statistics equation system of flue-cured tobacco flavor types index Y of the present invention is based on stepwise regression analysis side's ratio juris, method and step.Adopt Matlab software to carry out stepwise regression analysis to the sample data gathering, set up Y(dependent variable) with X(independent variable) " Optimal Regression Equation.The content of 89 kinds of fragrance components of the multiple batches of analysis of 43 flue-cured tobacco samples of take is independent variable, and the odor type (assignment) of take carries out stepwise regression analysis as dependent variable, has set up following equation, i.e. " flue-cured tobacco flavor types index " equation.
Flue-cured tobacco flavor types index Y=1.875-2.702X1, (isoamyl olefine aldehydr)+0.150X2, (2-acetyl furan)+0.061X3, (phenmethylol)-0.416X4, (2-acetyl pyrrole)+0.367X5, (tea ketone)+1.053X6, (n-nonanoic acid)+0.760X7, (indoles)+0.010X8, (different solanone)+0.027X9, (large horse scholar ketone)+0.352X10, (dihydroactinidiolide)-0.029X11, (Megastigmatrienone)-0.31X12, (1 (dihydro) naphtha)+0.051X13, (farnesyl acetone)-0.281X14, (methyl hexadecanoate)
Coefficient of multiple correlation R=0.968041 of this regression equation, coefficient of determination R 2=0.937103, P=6.64 * 10 -14, the F value of odor type index return equation variance analysis reaches the level of signifiance (P≤0. 05); The partial correlation coefficient of 14 significant factor regression coefficients reaches the level of signifiance.
In a multiple linear regression model, not all X(independent variable) and Y(dependent variable) have a significant linear relationship.For solve the problem that has the part independent variable X of remarkable relation with dependent variable Y of how picking out from independent variable that in a large number may be relevant, adopting the method for stepwise regression analysis is exactly a kind of effective method.
The basic thought of successive Regression is: big or small to Y influence degree by it to whole dependent variables, adopt partially recurrence squaresize judge, one by one introduce successively from big to small regression equation, and at any time to regression equation at that time contained whole variablees test, see that whether it is still remarkable, if not remarkable just by its rejecting, until contained all variablees are all remarkable to the effect of Y in regression equation, just consider to introduce new variable.In remaining not selecting in the factor, select Y effect the maximum again, check its conspicuousness, as significantly, introduce equation, not remarkable, do not introduce.To the variable one by one inspection of having introduced, by inapparent, to pick out, in the variable subset that has so just guaranteed finally to obtain, all variablees are all significant.Through some steps, just obtained optimal subset like this.
Multiple linear regression equations is expressed as:
Y=a+b 1X 1+b 2X 2+…+b nX n
In multiple linear regression analysis, should make estimated value and it is minimum that the residual error between observed reading y reaches on all sample points.We use coefficient of determination, or claim the coefficient of determination, evaluate the fitting degree of multiple linear regression model.
R 2 = SSR SST = ( y ^ i - y ‾ ) 2 ( y i - y ‾ ) 2
At this, SSR is deviation from regression, and SST is total departure, and the decomposition formula of total sum of squares of deviations is: total departure (SST)=deviation from regression (SSR)+residual deviation (SSE).
And for multiple correlation coefficient, it is that (for example independent variable is analyzed data X1, X2, X3, Xn, Xn+1 to a variable of measurement (for example dependent variable odor type index Y) with other a plurality of variablees ...) between the index of linear dependence degree.
Y value of the present invention is to be decided by 14 aroma components and a coefficient, than many 5 compositions in the Li Zhang of Chinese University of Science and Technology sea.9 kinds of compositions that do not have in the Y odor type indicial equation of Li Zhanghai: tea ketone, 2-acetyl furan, isoamyl olefine aldehydr, 2-acetyl pyrrole, (dihydro) naphtha, indoles, different solanone, n-nonanoic acid, large horse scholar ketone; Different 4 kinds of aroma components of the present invention and Li Zhanghai: isovaleric acid, solanone, dihydro-β-ionol, damascenone; Remaining 5 kinds of aroma component is identical: phenmethylol, Megastigmatrienone, farnesyl acetone, dihydroactinidiolide, methyl hexadecanoate.
Coefficient of multiple correlation R of the present invention and coefficient of determination R 2all be greater than coefficient of multiple correlation R and the coefficient of determination R of Li Haizhang etc. 2.P of the present invention value≤0.005 meets the requirements.
By after flue-cured tobacco sample analysis data substitution flue-cured tobacco flavor types index of the present invention Y computing formula, the odor type type of judgement sample substantially just, odor type index return equation reliability is higher.
Flue-cured tobacco flavor types judging nicety rate of the present invention is 91.1%.For maintenance and the ginseng of research and development, essence and flavoring agent of the odor type gradient classification of flue-cured tobacco, tobacco leaf buying, cigarette brand style and features tobacco leaf formulation, join, provide the chemistry of datumization to judge.
Accompanying drawing explanation
Below in conjunction with accompanying drawing illustrated embodiment, be described further, but protection domain of the present invention is not limited to this embodiment.
Fig. 1 tradition SDE extracting process and the present invention optimize SDE extraction detection method comparative result figure.
Fig. 2 is the histogram of flue-cured tobacco flavor types of the present invention and result of calculation.
Fig. 3: be the Tobacco Types that shown in Fig. 2, each sequence number represents.
Embodiment
As can be seen from Figure 1: in vapo(u)rizing temperature, be 198 ℃-200 ℃, extraction time surpassed after 3 hours, and extract does not increase, and the flavor matter that adopts the present invention to optimize the acquisition of SDE extracting process reaches capacity, then it is meaningless to extend extraction time.
(1) adopt distillation extraction (SDE) optimization method simultaneously, the data that cause perfumery in extraction flue-cured tobacco sample (the traditional SDE extracting process of accompanying drawing 1 and optimization SDE extracting process comparative result)
In cucurbit, intend carrying out flue-cured tobacco and cause tobacco sample 20 that perfumery analyzes or 30 grams, add water 350 or 450ml, add internal standard compound matter, in order to distillation; In extraction flask, add 40ml methylene chloride.
1. the prolongation of extraction time: extractant is used methylene chloride, 60 ℃ of constant temperature water baths, extraction time carries out 3 hours; Than traditional prolongation 1 hour.The prolongation of extraction time, has more time extracting substance, is convenient to more completely, extracting substance up hill and dale.Extraction time surpasses 3 hours, is similar in kind, without much meanings with the extraction time extracting substances of 3 hours.
The raising of vapo(u)rizing temperature while 2. extracting: heating jacket vapo(u)rizing temperature is 198 ℃-200 ℃, makes boiling violent, to extract more completely the material of half volatile; Although water has seethed with excitement in the time of 100 ℃, water temperature no longer raises,, under the condition of 198 ℃-200 ℃ of airtight environment and heating jackets, in cucurbit, water temperature increases to some extent, is convenient to extract high boiling substance, has increased the kind of extracting substance.1. 2. two accompanying drawing 1 signals for feature.
3. separated moisture routinely: in separating funnel, dichloromethane solution to extraction adds excessive sodium sulphate, ratio is 0.5 times of tobacco sample weight, allow sodium sulphate fully absorb the moisture in the dichloromethane solution of extraction, subsequently, successively each once, with 10ml dichloromethane rinse bottle, guarantees that extract all extracts.
4. concentrated routinely: the extractant in step (3) to be concentrated into 0.5ml left and right, to be back to 1ml left and right.
5. the refrigeration of routinely sample of producing in step (4) not being spent the night, the machine of directly going up carries out GC-MS(gas chromatography-mass spectrum) makings analysis;
Originally, many researchers caused in the extraction of perfumery tobacco, and extraction time has 2 hours, 2.5 hours, 3 hours; 100 ℃ of vapo(u)rizing temperatures, not completely, thoroughly, large to the amount of collected of low-boiling compound, a little less than the trapping relatively of higher-boiling compound, the flue-cured tobacco material generally extracting, between 42-80 kind for the material extracting.
Adopt tobacco of the present invention to cause perfumery simultaneously after distillation extraction (SDE) optimization method, the amount of collected of higher-boiling compound is increased, about the material 120-190 extracting, can be used for 89 of condition analysis.The reason that extracting substance kind is many is above-mentioned 1. 2. two extraction features.
(2) analysis condition and the analysis result thereof of gaschromatographic mass spectrometry (GC-MS).
Gaschromatographic mass spectrometry GC-MS condition: chromatographic column: DB-5(30m * 0.25mmi.d. * 0.25 μ m d.f.)
Temperature programme: injection port: 250 ℃; Carrier gas: He;
Column cap is pressed: 100kPa; Split ratio: 30: 1; Sample size 1.0 μ L; Transmission line temperature: 250 ℃; Ion source temperature: 150 ℃; EI energy: 70eV; Sweep limit: 35~350u; Interior mark: n-heptadecane; To the collection of illustrative plates collecting, utilize NIST1.11 upgrade version spectrum storehouse to retrieve; Adopt area normalization standard measure.
Result: 1. adopt polarity on the weak side DB-5 chromatographic column (nearly 96% filling material be neutral substance, remaining be polarity on the weak side) neutrality and the low pole material of the separated overwhelming majority, this point be different from domestic literature report with DB-5 chromatographic column Separation of Neutral material.
2. (theoretical superiors's area of pictural surface reaches and more than 0.03% can think a kind of material at 120~190 kinds to analyze tobacco leaf aroma component out, because some content reality that causes perfumery seldom), there are comparative 101, amount to 89 fragrance component indexs of flue-cured tobacco and can be used for analyzing.In Table 1:
Table 1: hyle out of flue-cured tobacco sample analysis (originally have 120-190 material, have comparative 101, in have 89 can be used for statistical study)
(3) use the statistics equation of the flue-cured tobacco flavor types index Y of the present invention's foundation, i.e. " odor type index " formula, the data that the analysis of (SDE) optimization method is obtained, adopt Matlab software to carry out stepwise regression analysis to data, it is independent variable that the present embodiment be take the content of 89 kinds of fragrance components of the multiple batches of analysis of 43 flue-cured tobacco samples, and the odor type (assignment) of take carries out stepwise regression analysis as dependent variable, has set up following equation.
Flue-cured tobacco flavor types index Y=1.875-2.702X1, (isoamyl olefine aldehydr)+0.150X2, (2-acetyl furan)+0.061X3, (phenmethylol)-0.416X4, (2-acetyl pyrrole)+0.367X5, (tea ketone)+1.053X6, (n-nonanoic acid)+0.760X7, (indoles)+0.010X8, (different solanone)+0.027X9, (large horse scholar ketone)+0.352X10, (dihydroactinidiolide)-0.029X11, (Megastigmatrienone)-0.31X12, (1 (dihydro) naphtha)+0.051X13, (farnesyl acetone)-0.281X14, (methyl hexadecanoate).
Coefficient of multiple correlation R=0.968041 of this regression equation, coefficient of determination R 2=0.937103, P=6.64 * 10 -14, the F value of odor type index return equation variance analysis reaches the level of signifiance (P≤0. 05); The partial correlation coefficient of 14 significant factor regression coefficients reaches the level of signifiance, and odor type index return equation reliability is higher.Accompanying drawing 2 provides histogram and describes.
Table 2: flue-cured tobacco flavor types index result of calculation contrast form (40 kinds of flue-cured tobaccos, 43 kinds of flue-cured tobacco samples have 3 kinds and are merged into a kind)
(4) calculate the rear corresponding flue-cured tobacco flavor types index Y numerical value that obtains, as flue-cured tobacco flavor types judgement numerical value, for the ginseng of the maintenance of the odor type gradient classification of cured tobacco production, tobacco leaf buying, cigarette brand style and features tobacco leaf formulation and research and development, essence and flavoring agent, join, the criterion of datumization is provided.

Claims (1)

1. a detection decision method for flue-cured tobacco flavor types, is characterized in that step is as follows:
(1) flue-cured tobacco flavor types causes perfumery extraction: by while distillation extraction (SDE) Optimized Extraction method, proceed as follows: in cucurbit, plan is carried out flue-cured tobacco and is caused tobacco sample 20 that perfumery analyzes or 30 grams, add water 350 or 450ml, add internal standard compound matter, in order to distillation; In extraction flask, add 40ml methylene chloride;
1. extraction time: extractant is used methylene chloride, 60 ℃ of constant temperature water baths, conventional extraction mode is carried out 3 hours;
2. extraction temperature: heating jacket vapo(u)rizing temperature is 198 ℃-200 ℃, makes boiling violent, to extract more completely the material of half volatile;
3. separated routinely: in separating funnel, dichloromethane solution to extraction adds excessive sodium sulphate, ratio is 0.5 times of tobacco sample weight, allow sodium sulphate fully absorb the moisture in the dichloromethane solution of extraction, subsequently, successively each once, with 10ml dichloromethane rinse bottle, guarantees that extract all extracts;
4. concentrated routinely: the extractant by step in is 3. concentrated into 0.5-0.4ml, is back to 1-1.1ml;
5. routinely by step 4. in the sample refrigeration of not spending the night of extraction, the machine of directly going up carries out the makings analysis of GC-MS gas chromatography-mass spectrum;
(2) gaschromatographic mass spectrometry (GC-MS) qualitative and quantitative analysis flue-cured tobacco flavor types causes perfumery;
Described GC-MS gas chromatography-mass spectrum condition:
Chromatographic column: DB-5,30m * 0.25mmi.d. * 0.25 μ m d.f.;
Temperature programme: by the firing rate of 4 ℃/min, be warmed up to for the first time 40 ℃ of insulation 2min, be warmed up to subsequently 250 ℃, insulation 10min;
Injection port: 250 ℃; Carrier gas: He; Column cap is pressed: 100kPa;
Split ratio: 30: 1; Sample size 1.0 μ L;
Transmission line temperature: 250 ℃;
Ion source temperature: 150 ℃;
EI energy: 70eV;
Sweep limit: 35~350u;
Interior mark: n-heptadecane; To the collection of illustrative plates collecting, utilize NIST1.11 upgrade version spectrum storehouse to retrieve; Adopt area normalization standard measure;
The result of analyzing is: theoretical superiors's area of pictural surface reaches more than 0.03% can think a kind of material, because some content reality that causes perfumery is seldom, and the flue-cured tobacco in variety classes, the different places of production; One species, the flue-cured tobacco in the different places of production, what they were out analyzed causes perfumery kind generally in 120-190 kind, has comparative 101, for 89 of statistical study;
(3) analyze and judge: what adopt step (2) acquisition causes perfumery qualitative and quantitative analysis 14 kinds of materials that correlativity is large out to flue-cured tobacco, and substitution can be carried out the following formula of stepwise regression analysis by Matlab software, carry out the detection of flue-cured tobacco flavor types and judge;
Flue-cured tobacco flavor types index Y=1.875-2.702X1, (isoamyl olefine aldehydr)+0.150X2, (2-acetyl furan)+0.061X3, (phenmethylol)-0.416X4, (2-acetyl pyrrole)+0.367X5, (tea ketone)+1.053X6, (n-nonanoic acid)+0.760X7, (indoles)+0.010X8, (different solanone)+0.027X9, (large horse scholar ketone)+0.352X10, (dihydroactinidiolide)-0.029X11, (Megastigmatrienone)-0.31X12, (1 (dihydro) naphtha)+0.051X13, (farnesyl acetone)-0.281X14, (methyl hexadecanoate),
Coefficient of multiple correlation R=0.968041 of this regression equation, coefficient of determination R 2=0.937103, P=6.64 * 10 -14, the F value of odor type index return equation variance analysis reaches level of signifiance P≤0. 05; The partial correlation coefficient of 14 significant factor regression coefficients reaches the level of signifiance;
(4) calculate the rear corresponding flue-cured tobacco flavor types index Y numerical value that obtains, as flue-cured tobacco flavor types judgement numerical value, for the ginseng of the maintenance of the odor type gradient classification of flue-cured tobacco, tobacco leaf buying, brand style and features tobacco leaf formulation and research and development, essence and flavoring agent, join, the criterion of datumization is provided.
CN201210388375.0A 2012-10-15 2012-10-15 Detection and determination method for flavor type of flue-cured tobacco Active CN103226135B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210388375.0A CN103226135B (en) 2012-10-15 2012-10-15 Detection and determination method for flavor type of flue-cured tobacco

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210388375.0A CN103226135B (en) 2012-10-15 2012-10-15 Detection and determination method for flavor type of flue-cured tobacco

Publications (2)

Publication Number Publication Date
CN103226135A CN103226135A (en) 2013-07-31
CN103226135B true CN103226135B (en) 2014-12-03

Family

ID=48836658

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210388375.0A Active CN103226135B (en) 2012-10-15 2012-10-15 Detection and determination method for flavor type of flue-cured tobacco

Country Status (1)

Country Link
CN (1) CN103226135B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105241977A (en) * 2015-10-29 2016-01-13 云南中烟工业有限责任公司 Method for characterizing cigarette baking aroma characteristic by using index

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105158385A (en) * 2015-07-10 2015-12-16 云南中烟工业有限责任公司 Method for accurately characterizing and evaluating flue-cured tobacco smoke aroma characteristic in cigarette aroma
CN105004826A (en) * 2015-07-10 2015-10-28 云南中烟工业有限责任公司 Method for accurately characterizing and evaluating green fragrance characteristics of cigarette fragrance
CN104991007A (en) * 2015-07-10 2015-10-21 云南中烟工业有限责任公司 Method for exactly characterizing and evaluating sweet aroma characteristics in cigarette aroma
CN105092789B (en) * 2015-08-10 2016-07-06 江苏中烟工业有限责任公司 Tobacco style changing features trend analysis in a kind of sheet nicotinyl alcohol process
CN105372345A (en) * 2015-10-29 2016-03-02 云南中烟工业有限责任公司 Method for representing clean aroma characteristics of cigarettes with indexes
CN106198809B (en) * 2016-07-27 2019-03-29 河南中烟工业有限责任公司 A kind of flat-flavor flue-cured tobacco identification method based on activity threshold
CN106290611B (en) * 2016-07-27 2019-04-02 河南中烟工业有限责任公司 A kind of Luzhou-flavor flue-cured tobacco identification method based on activity threshold
CN106226475B (en) * 2016-08-03 2018-03-09 云南中烟工业有限责任公司 A kind of quantitative judgement method of odor type among cured tobacco leaf
CN106290638A (en) * 2016-08-11 2017-01-04 云南中烟工业有限责任公司 A kind of quantitative forecasting technique of Medicated cigarette bean odor type
CN106290640A (en) * 2016-08-11 2017-01-04 云南中烟工业有限责任公司 A kind of quantitative forecasting technique of Medicated cigarette floral type
CN106442775A (en) * 2016-09-07 2017-02-22 云南中烟工业有限责任公司 Quantitative prediction method for aroma types of cigarettes and flue cured tobaccos
CN106770831B (en) * 2016-12-30 2019-11-01 中国烟草总公司广东省公司 A method of flue-cured tobacco is detected by Different Extraction Method and causes perfumery Megastigmatrienone content
CN109781870B (en) * 2017-11-13 2022-11-22 贵州中烟工业有限责任公司 Method for identifying flavor type of flue-cured tobacco
CN107941978B (en) * 2017-11-23 2020-07-31 陕西中烟工业有限责任公司 Method for evaluating internal quality stability of bead blasting for cigarettes
CN108845085A (en) * 2018-07-03 2018-11-20 云南中烟工业有限责任公司 A method of tobacco leaf odor type is predicted based on tobacco leaf chemical composition
CN109324016A (en) * 2018-10-17 2019-02-12 浙江中烟工业有限责任公司 A kind of determination method of redried odor type style
CN110554130A (en) * 2019-09-20 2019-12-10 云南中烟工业有限责任公司 Material management and control list construction method based on LSE-GC-MS/MS detection result

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102435709A (en) * 2011-09-12 2012-05-02 红云红河烟草(集团)有限责任公司 Method for accurately identifying flue-cured tobacco flavor types
CN102608244A (en) * 2012-03-02 2012-07-25 红云红河烟草(集团)有限责任公司 Detection method for simultaneously determining plurality of flavor substances in cigarette cut tobaccos
CN102650630A (en) * 2012-05-08 2012-08-29 红云红河烟草(集团)有限责任公司 Method for building distinguishing model for evaluating odor type of flue-cured tobacco raw material on the basis of note components

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102435709A (en) * 2011-09-12 2012-05-02 红云红河烟草(集团)有限责任公司 Method for accurately identifying flue-cured tobacco flavor types
CN102608244A (en) * 2012-03-02 2012-07-25 红云红河烟草(集团)有限责任公司 Detection method for simultaneously determining plurality of flavor substances in cigarette cut tobaccos
CN102650630A (en) * 2012-05-08 2012-08-29 红云红河烟草(集团)有限责任公司 Method for building distinguishing model for evaluating odor type of flue-cured tobacco raw material on the basis of note components

Non-Patent Citations (10)

* Cited by examiner, † Cited by third party
Title
《Comparative analysis of the volatile components in cut tobacco from different locations with gas chromatography–mass spectrometry (GC–MS) and combined chemometric methods》;Huang FL et al;《Analytica Chimica Acta》;20060831;第575卷(第2期);236-245 *
《Development of a Chromatographic Fingerprint of Tobacco Flavor by Use of GC and GC-MS》;Zhu XL et al;《Chromatographia》;20090430;第69卷(第7-8期);735-742 *
《MATLAB在不同烤烟品种间主要烟气成分差异性分析中的应用》;王浩雅等;《江西农业学报》;20100531;第22卷(第5期);19-21 *
《两个晒烟品种主要致香成分分析》;黄学跃等;《云南农业大学学报》;20060430;第21卷(第2期);192-195 *
《卷烟挥发性成分的聚类分析》;王玉等;《烟草科技》;20071231(第2期);48-52 *
Huang FL et al.《Comparative analysis of the volatile components in cut tobacco from different locations with gas chromatography–mass spectrometry (GC–MS) and combined chemometric methods》.《Analytica Chimica Acta》.2006,第575卷(第2期),236-245. *
Zhu XL et al.《Development of a Chromatographic Fingerprint of Tobacco Flavor by Use of GC and GC-MS》.《Chromatographia》.2009,第69卷(第7-8期),735-742. *
王浩雅等.《MATLAB在不同烤烟品种间主要烟气成分差异性分析中的应用》.《江西农业学报》.2010,第22卷(第5期),19-21. *
王玉等.《卷烟挥发性成分的聚类分析》.《烟草科技》.2007,(第2期),48-52. *
黄学跃等.《两个晒烟品种主要致香成分分析》.《云南农业大学学报》.2006,第21卷(第2期),192-195. *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105241977A (en) * 2015-10-29 2016-01-13 云南中烟工业有限责任公司 Method for characterizing cigarette baking aroma characteristic by using index

Also Published As

Publication number Publication date
CN103226135A (en) 2013-07-31

Similar Documents

Publication Publication Date Title
CN103226135B (en) Detection and determination method for flavor type of flue-cured tobacco
CN103226136B (en) Detection and determination method for flavor type of cigarette
Mercuri et al. The long history of Cannabis and its cultivation by the Romans in central Italy, shown by pollen records from Lago Albano and Lago di Nemi
CN102759588B (en) Method for separating and preparing key acid flavor components in cigarette mainstream smoke and application of key acid volatile components
Schüttler et al. Characterizing aromatic typicality of Riesling wines: merging volatile compositional and sensory aspects
CN102495163A (en) Establishing method and use of flue-cured tobacco GC/MS fingerprint
CN103217408A (en) Method for identifying two flue-cured tobaccos with different odor types in Guizhou
CN103344713B (en) Method for analyzing importance of flavoring in flue-cured tobacco fragrance type classification and forecasting fragrance type based on random forest method
CN102692488A (en) Jinhua ham grading and identifying method based on electronic nose technology
Sun et al. Comparative analysis on chemical components and sensory quality of aging flue-cured tobacco from four main tobacco areas of China
CN104316635A (en) Method for rapidly identifying flavor and quality of fruits
CN108061691A (en) A kind of method of reconstituted tobacco quality stability between evaluation batch
CN103175913A (en) Method for identifying quality of jasmine tea
CN105242011A (en) Method for evaluating inner sense quality of tobacco dusts
CN101862027A (en) Preparation method of rhododendron fastigiatum extracts and application of rhododendron fastigiatum extracts in cigarettes
CN111896657B (en) Method for screening tobacco leaf source spice style characteristic components
CN106290611B (en) A kind of Luzhou-flavor flue-cured tobacco identification method based on activity threshold
Wang et al. Zonal distribution of neutral aroma components in flue-cured tobacco leaves
Chapman The nutrient content of the soil and root system of a dry heath ecosystem
CN106198809B (en) A kind of flat-flavor flue-cured tobacco identification method based on activity threshold
CN104172465A (en) Tobacco treatment process
Österdahl et al. Tobacco‐specific N‐nitrosamines in the saliva of habitual male snuff dippers
CN103604888B (en) Method for detection analysis on tobacco leaf raw material quality
CN106290610B (en) A kind of delicate fragrance type flue-cured tobacco identification method based on activity threshold
CN106680408A (en) Method for analyzing aromatic substances of flue-cured tobacco leaves in different tobacco-growing areas

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant