CN102854290A - Method for predicting release amount of crotonaldehyde in mainstream smoke of flue-cured tobaccos - Google Patents
Method for predicting release amount of crotonaldehyde in mainstream smoke of flue-cured tobaccos Download PDFInfo
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Abstract
The invention relates to a method for predicting the release amount of crotonaldehyde in mainstream smoke of flue-cured tobaccos. The method comprises the following steps of: performing sample pretreatment on the flue-cured tobaccos to be tested through three steps of manual tearing, stem removal, shredding; detecting five chemical components comprising palmitic acid, tobacco moisture, total polyphenol, total nitrogen and protein of a sample to be tested; calculating network values of eight nodes of a hidden layer by combining the measurement results of the five chemical components with the coefficients of each input layer of a model; converting the network values of the eight nodes of the hidden layer into the output values of the eight nodes of the hidden layer; and calculating to obtain the predicted value of the release amount of the tobacco crotonaldehyde by combining the output values of the eight nodes of the hidden layer with the coefficients of the output layers of the model. According to the method, the five chemical component constants of the tobacco in the sample to be tested are detected, prediction calculation is performed by matching the established model structure with the model coefficients, and the crotonaldehyde accumulation content to be formed in the future can be effectively predicted through the flue-cured tobacco raw materials, so that raw material selection in the production process is guided.
Description
Technical field
The present invention relates to the Forecasting Methodology of crotonaldehyde burst size in a kind of junior tobacco leaf main flume, belong to technical field of tobacco.
Background technology
Crotonaldehyde is a kind of important objectionable impurities in the cigarette mainstream flue gas, the control composition inventory that is put into 46 kinds of objectionable constituent lists of Canadian government and WHO " tobacco product control research group " suggestion, China national tobacco monopoly bureau also with crotonaldehyde as one of 7 kinds of objectionable constituent of evaluating cigarette security.China has set up the industry standard that phenol is measured in the cigarette mainstream flue gas at present.But the content of usually measuring crotonaldehyde in the flue gas need to roll sample, the smoking machine suction captures and capture the comparatively loaded down with trivial details steps such as thing sample introduction pre-treatment.Comparatively speaking, the determination step of some Chemistry ingredients in the tobacco is just comparatively easy.And the result that the aldehyde in the flue gas, ketone are seemingly directly shifted by tobacco, yet, most of this class volatile compound be from those precursor compounds such as sugar, pectin, protein and triglyceride formation that may be from tobacco, the variation of these tobacco compounds finally can impact smoke components content.Hence one can see that, experienced the chemical reaction of series of complex and substance decomposition, generative process in tobacco components is converted to the process of smoke components by burning, and everything process all belongs to the nonlinearities change system of a complexity.But from lot of documents and related data, also less for the relation research between this complicated variation system.
Summary of the invention
The object of the present invention is to provide the Forecasting Methodology of crotonaldehyde burst size in a kind of junior tobacco leaf main flume.After several chemical constitutions of junior tobacco leaf (being determined by this method) are measured, predict crotonaldehyde burst size in its flue gas by this method, so that the cigarette composition personnel in time understand the crotonaldehyde burst size level of this raw material, and the later stage select materials and tobacco leaf formulation design in effective application, reduce a kind of harm reduction measure of crotonaldehyde burst size thereby reach to select materials.
Modern neural network is a kind of Nonlinear Statistical data modeling tool, is commonly used to relation complicated between input and output is carried out modeling, and network self all is approaching certain algorithm of nature or function usually.By utilizing the constructed tobacco components of great amount of samples and flue gas crotonaldehyde burst size neural network model, testing sample flue gas crotonaldehyde burst size level is predicted, thereby avoided carrying out some equipment requirements and loaded down with trivial details treatment step in the flue gas inspection process.
The Forecasting Methodology particular content of crotonaldehyde burst size is as follows in the junior tobacco leaf main flume that the present invention proposes:
One, the foundation of Forecasting Methodology
(1) modeling sample source
176 junior tobacco leaf samples in 2009 cover 47 places of production, the whole nation, 9 kinds, 3 tobacco leaf positions, upper, middle and lower.
(2) modeling sample pre-treatment
With junior tobacco leaf to be measured carry out sample pre-treatments by artificial sheet, pick stalk, three steps of chopping.The smoked sheet of handling well (silk) is sealing, labelled at once, and unified depositing do not obscured.All equipment is cleaned in earnest before and after different cigarette sample moisture regain and the chopping, pretty good to go here and there between assurance cigarette sample.
The unified processing of collected junior tobacco leaf raw material, Unified coding, the respectively chopping and roll into pure cigarette (for eliminate cigarette supplementary to the interference of research as far as possible, selecting unified air permeability is 60CU, grammes per square metre 28g/m of single raw material
2Same batch of cigarette paper, tobacco sample is rolled into without filter tip cigarette, and selects cigarette with the cigarette weight index), flavoring and casing not, the cigarette after selecting is housed in temperature (18 ± 1) ℃; In the environment of humidity (50 ± 10) %, take out before analyzing that to press flue gas national standard method balance 48 hours for subsequent use.
(3) modeling sample chemical constitution and flue gas crotonaldehyde burst size are measured
Because some tobacco components is to generate the precursor compound of smoke components (such as carbohydrates, nitrogen-containing compound, organic acid, phenols etc.), its content is larger to the content influence of smoke components, therefore chooses 25 kinds of junior tobacco leaf chemical constitution (total reducing sugars, reducing sugar, chlorine, potassium, total nitrogen, nicotine, volatilization alkali, moisture, protein, volatile acid, cellulose, chlorogenic acid, scopoletin, rutin sophorin, total polyphenols, oxalic acid, malonic acid, succinic acid, malic acid, citric acid, palmitic acid, linoleic acid, oleic acid, leukotrienes, stearic acid) as the index that will study.Measure water-soluble sugar by the YC/T159-2002 continuous flow method; Measure total nitrogen by the YC/T161-2002 continuous flow method; Measure potassium by the YC/T217-2007 continuous flow method; Measure chlorine by the YC/T162-2002 continuous flow method; By GB/T 23225-2008 spectrphotometric method for measuring nicotine; The YC/T35-1996 back titration is measured volatilization alkali; YC/T 31-1996 oven method measuring moisture; YC/T 166-2003 Ke Daerfa measures protein; YC/T 202-2006 high effective liquid chromatography for measuring polyphenolic substances (chlorogenic acid, scopoletin, rutin sophorin, total polyphenols); Adopt the steam distillation back titration to measure volatile acid; Cellulose is measured in coarse-fibred method for measuring in the tobacco; Microwave assisted derivatization-gas chromatography determination non-volatile organic acids (oxalic acid, malonic acid, succinic acid, malic acid, citric acid, palmitic acid, linoleic acid, oleic acid, leukotrienes, stearic acid), the tobacco components unit conversion that determines is %.YC/T 254-2008 high effective liquid chromatography for measuring flue gas crotonaldehyde burst size, the flue gas crotonaldehyde burst size that the flue gas crotonaldehyde burst size that determines is scaled every gram pipe tobacco is μ g/g.
(4) modeling variable and abnormal sample screening
Variable Selection on the one hand can simplified model, is the less variable of smoke components impact is rejected on the other hand, makes the predictive ability of model stronger, robustness is better.The principle that this research variable is selected is to carry out Variable Selection by genetic algorithm, and farthest keep the precursor compound variable that produces smoke components according to mechanism result of study in the past, determine that finally rational modeling set of variables becomes 5 chemical constitutions (palmitic acid, moisture in cut tobacco, total polyphenols, total nitrogen, protein).
Abnormal sample is the sample away from model integral body, and is obvious on the regretional analysis impact of model, at first picks out by the concentration residual analysis, then repetitive operation in modeling process, again reject, until obtain the optimum prediction effect, the final sample that enters modeling of determining has 128.
(5) modeling parameters optimization and model internal performance are estimated
Adopt the modeling of neural network mode to utilize the duplicate sampling method that power attenuation coefficient and hidden layer node number are in optimized selection, final argument is defined as table 1.Adopt the coefficient of determination (R of constructed forecast model
2) and prediction standard deviation (SEC) (seeing formula 1) valuation prediction models internal performance, the coefficient of determination (R
2) larger, prediction standard deviation (SEC) is less, and then model is better, sees table 2 for details.
Table 1 model parameter, weight number and network structure
In the formula (1), y
I, actualBe i modeling sample measured value, y
I, perdictedFor using institute's established model to i sample predicted value in the modeling sample, n is the modeling sample number.
(6) model external certificate
Employing has neither part nor lot in 28 external certificate samples of modeling the predictive ability of model is verified.Wherein adopt 1. SEP/SEC, 2. RPD, 3. paired t-test, 4. consensus forecast relative deviation, four kinds of parameters come the generalization ability of model and applicability to verify, see Table 3.
①SEP/SEC
The ratio of the prediction standard deviation (SEC) of prediction standard deviation (SEP) (seeing formula 2) and the modeling sample of checking sample is less than or equal to 1.2, and namely SEP can not be greater than 1.2 times SEC, with this whether over-fitting of model is described.
In the formula (2), y
I, actualBe i verification sample measured value, y
I, perdictedFor using i verification sample predicted value in the checking sample forecasting process, m is the checking number of samples.
②RPD
SD
vFor the standard deviation of all checking sample measured values, at SD
vUnder the identical prerequisite, the checking sample coefficient of determination (R
2) larger, the model prediction accuracy is higher; SD
vWith the ratio R PD (seeing formula 3) of the prediction standard deviation (SEP) of verifying sample, RPD is larger, and the model prediction accuracy is higher.If it has been generally acknowledged that RPD＜2, then showing predicts the outcome is unacceptable;
In the formula (3), SD
vBe the standard deviation of all checking sample measured values, SEP is less, and RPD is larger.
3. paired t-test
The prediction the result verifies by paired t-test, when level of significance greater than 0.05 the time, the absolute value of t is less than its relevant critical value (t
0.05,27=2.051831), show that there are not significant difference in standard method of measurement and Forecasting Methodology, namely there is not systematic error in the measurement result of two kinds of methods.
4. consensus forecast relative deviation
The consensus forecast relative deviation of Calculation Verification sample measured value and predicted value (seeing formula 4), the consensus forecast relative deviation is less, and the model prediction accuracy is higher.
In the formula (4), y
I, actualBe i verification sample measured value, y
I, perdictedFor using i verification sample predicted value in the checking sample forecasting process, m is the checking number of samples.
Table 3 model external certificate situation gathers
Two, the application of Forecasting Methodology
(1) testing sample pre-treatment
With junior tobacco leaf to be measured carry out sample pre-treatments by artificial sheet, pick stalk, three steps of chopping.The smoked sheet of handling well (silk) is sealing, labelled at once, and unified depositing do not obscured.All equipment is cleaned in earnest before and after different cigarette sample moisture regain and the chopping, pretty good to go here and there between assurance cigarette sample.
(2) 5 kinds of chemical constituents determinations of testing sample
5 kinds of junior tobacco leaf chemical constitutions (palmitic acid, moisture in cut tobacco, total polyphenols, total nitrogen, protein) are assisted Yan Shengization – gas chromatography determination non-volatile organic acids (palmitic acid) by microwave; By YC/T 31-1996 oven method measuring moisture (moisture in cut tobacco); By YC/T 202-2006 high effective liquid chromatography for measuring polyphenolic substances (total polyphenols); Measure total nitrogen by the YC/T161-2002 continuous flow method; YC/T 166-2003 Ke Daerfa measure protein, and its analytical unit all is scaled %.
(3) testing sample is by model coefficient prediction crotonaldehyde burst size
Three-decker network model by foundation: ground floor is input layer, and nodes is 5, and corresponding input variable is palmitic acid, moisture in cut tobacco, total polyphenols, total nitrogen, protein; The second layer is hidden layer, and nodes is 8; The 3rd layer is output layer, and nodes is 1, and corresponding output variable is the crotonaldehyde burst size.
Table 4 input layer is to each node coefficient value of hidden layer
The hidden layer network values is calculated by formula (5).
x
j=ZW
Input(j=[1 wherein, 2 ..., 8]) (5)
In the formula:
Z-represents input vector [pipe tobacco palmitic acid, moisture in cut tobacco, pipe tobacco total polyphenols, pipe tobacco total nitrogen, pipe tobacco protein, b], and wherein b is the input layer bias, and its value is 1;
W
Input-expression input layer matrix of coefficients
(seeing table 4 for details);
x
j-be the network values of j Nodes of hidden layer.
The hidden layer output valve is calculated by formula (6).
In the formula:
E-is the truth of a matter of natural logarithm.
O
j-be j node output valve of hidden layer.
Annotate: formula (6) if in x
jValue greater than 15 o'clock, O
jBy 1, if x
jValue less than-15 o'clock, O
jBy 0.
Table 5 output layer coefficient value
The output layer output valve is calculated by formula (7).
y
Phenol=O
jW
Output(7)
In the formula:
O
j---expression hidden layer output valve vector [O
1, O
2, O
3, O
4, O
5, O
6, O
7, O
8, b], wherein b is the output layer bias, its value is 1;
W
Output---be output layer coefficient vector [W
1, W
2, W
3, W
4, W
5, W
6, W
7, W
8, W
0] (seeing table 5 for details);
y
Phenol---be the output layer output valve, i.e. the burst size predicted value of flue gas crotonaldehyde.
Adopt 5 chemical constitutions in the junior tobacco leaf that crotonaldehyde burst size in its flue gas is predicted to possess following advantage in application process by the present invention:
A. tobacco sample to be measured is carried out 5 tobacco components constants and detect, i.e. crotons aldehyde in measurable its flue gas need not to carry out that cigarette rolls and aspirate to capture granule phase substance matter with smoking machine equipment.
B. use the model structure that has made up and cooperate model coefficient to analyze, the simple computation that only need to carry out 3 steps can obtain the burst size predicted value of crotonaldehyde, and simple operation can be adopted counter or artificial calculating, need not to use complicated software for calculation.
C. can rely on present junior tobacco leaf raw material that possible crotonaldehyde cumulative amount in the cigarette finished product that will form future is carried out effective anticipation, thereby instruct the raw material in the production run to select, have important practical significance to improving the cigarette product quality safety.
Embodiment
Embodiment:
(1) testing sample pre-treatment
With junior tobacco leaf to be measured carry out sample pre-treatments by artificial sheet, pick stalk, three steps of chopping.The smoked sheet of handling well (silk) is sealing, labelled at once, and unified depositing do not obscured.All equipment is cleaned in earnest before and after different cigarette sample moisture regain and the chopping, pretty good to go here and there between assurance cigarette sample.
(2) choose 1 part of junior tobacco leaf sample to be measured, carried out 5 kinds of chemical constituents determinations
5 kinds of junior tobacco leaf chemical constitutions (palmitic acid, moisture in cut tobacco, total polyphenols, total nitrogen, protein) are assisted Yan Shengization – gas chromatography determination non-volatile organic acids (palmitic acid) by microwave; By YC/T 31-1996 oven method measuring moisture (moisture in cut tobacco); By YC/T 202-2006 high effective liquid chromatography for measuring polyphenolic substances (total polyphenols); Measure total nitrogen by the YC/T161-2002 continuous flow method; YC/T 166-2003 Ke Daerfa measure protein, and it the results are shown in Table 6;
(3) by model coefficient prediction crotonaldehyde burst size
Three-decker network model by foundation: ground floor is input layer, and nodes is 5, and corresponding input variable is palmitic acid, moisture in cut tobacco, total polyphenols, total nitrogen, protein; The second layer is hidden layer, and nodes is 8; The 3rd layer is output layer, and nodes is 1, and corresponding output variable is the crotonaldehyde burst size.
5 chemical constitution results that 1) will detect gained cooperate the coefficient of each input layer in the table 4, calculate the network values of 8 nodes of hidden layer by formula (5), and it the results are shown in Table 7;
2) network values of gained is calculated the output valve of 8 nodes of hidden layer by formula (6), it the results are shown in Table 8;
3) the hidden layer output valve of gained is cooperated coefficient in the table 5, calculate the output layer output valve by formula (7), i.e. the burst size predicted value of flue gas crotonaldehyde, it the results are shown in Table 9.
5 chemical constitution testing results of table 6 junior tobacco leaf sample to be measured
The network values of 8 nodes of table 7 junior tobacco leaf sample to be measured hidden layer
The output valve of 8 nodes of table 8 junior tobacco leaf sample to be measured hidden layer
Table 9 junior tobacco leaf sample to be measured output layer output valve (flue gas crotonaldehyde burst size predicted value)
Claims (4)
1. the Forecasting Methodology of crotonaldehyde burst size in the junior tobacco leaf main flume is characterized in that comprising following steps:
1) with junior tobacco leaf to be measured by artificial sheet, pick stalk, three steps of chopping are carried out sample pre-treatments;
2) 5 tobacco components of testing sample are detected, described 5 tobacco components are palmitic acid, moisture in cut tobacco, total polyphenols, total nitrogen, protein;
3) with the network values of 8 nodes of each input layer coefficient calculations hidden layer of 5 tobacco components measurement results of testing sample combination model;
4) network values that will calculate 8 nodes of gained hidden layer is converted to the output valve of 8 nodes of hidden layer;
5) will calculate the burst size predicted value that 8 node output valves of gained hidden layer combination model output layer coefficient calculations obtains the flue gas crotonaldehyde.
According to claim 1 described a kind of junior tobacco leaf chemical constitution to the Forecasting Methodology of crotonaldehyde burst size in its flue gas, it is characterized in that described Artificial Neural Network Structures is 5-8-1, i.e. 5 input layers, 8 hidden layer nodes, 1 output layer node.
3. described a kind of junior tobacco leaf chemical constitution is characterized in that to the Forecasting Methodology of crotonaldehyde burst size in its flue gas described each input layer coefficient 8 is followed successively by from node 1 to node: palmitic acid :-0.983,3.2711 ,-6.8093 ,-4.643,2.5933,3.4842 ,-12.6112,0.7025 according to claim 1; 8.6244 ,-0.9048 ,-0.3861 ,-5.8622 ,-0.5407 ,-2.1619,3.9261 ,-2.1411 moisture in cut tobacco:; Total polyphenols :-2.6491,0.2623,3.3110,7.1684 ,-1.678,0.2639 ,-1.3943,1.6987; Total nitrogen :-1.1227,15.0432,2.3615,0.0335 ,-4.1247 ,-0.7224 ,-9.6026,5.3285;-2.3807 ,-3.6561,0.9038,4.7422,0.253,0.2014,1.8548 ,-1.4746 protein:; Input layer biasing coefficient :-2.7908,2.9324 ,-1.4009 ,-2.1805,11.1459,6.5016,2.8062,7.7844, wherein the input layer bias is 1.
4. described a kind of junior tobacco leaf chemical constitution is characterized in that described output layer coefficient is: hidden layer node 1 input layer coefficient 9.032 to the Forecasting Methodology of crotonaldehyde burst size in its flue gas according to claim 1; Hidden layer node 2 input layer coefficients 14.0068; Hidden layer node 3 input layer coefficients-6.7807; Hidden layer node 4 input layer coefficients 4.1487; Hidden layer node 5 input layer coefficients 13.2319; Hidden layer node 6 input layer coefficients 5.0411; Hidden layer node 7 input layer coefficients 15.6396; Hidden layer node 8 input layer coefficients 6.9897; Output layer biasing coefficient input layer coefficient-5.6833, wherein the output layer bias is 1.
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