CN103499609B - A kind of method that honey fragrance intelligence sense of smell dynamic response feature and differentiation information dynamic characterization are studied - Google Patents
A kind of method that honey fragrance intelligence sense of smell dynamic response feature and differentiation information dynamic characterization are studied Download PDFInfo
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Abstract
A kind of method that honey fragrance intelligence sense of smell dynamic response feature and differentiation information dynamic characterization are studied, it is characterized in that: for the volatilization feature of honey aromatic substance, optimize the parameter of Electronic Nose intelligence olfactometry system, pre-service is corrected in conjunction with collection of illustrative plates, obtain the original dynamic fingerprint collection of illustrative plates of high s/n ratio, again according to honey fragrance simulated system, in conjunction with the aroma quality migration that honey fragrance experiences in intelligent olfactory sensor, the features such as sensor array internal divergence and sensor chip physisorption, explore intelligent sense of smell fragrant at head, front end fragrance, body note is to the dynamic response feature of bottom note four-stage, instruct the selection representing the intelligent sense of smell behavioral characteristics response point of honey quality difference, simultaneously in conjunction with the mathematical feature parameter in sense of smell collection of illustrative plates, the differentiation information that the sense of smell of comprehensive seizure honey quality intelligence characterizes.
Description
Technical field
The application relates to Electronic Nose sensor technology, is specifically related to the differentiation information excavating research that the sense of smell of honey quality intelligence characterizes.
Background technology
Fragrance is one of important attribute that product quality embodies, and product fragrance characterizes needs its objectivity outstanding, authenticity and comprehensive.Current gas chromatography (GC), gas chromatography-mass spectrography (GC-MS) and gas chromatography-smell methods such as distinguishing (GC-O), monomer aroma substance that can only be limited in testing product, and there is the phenomenons such as collaborative, modified tone between these fragrance, be difficult to the flavouring essence quality reflecting sample on the whole.And Intelligent Olfaction System (Electronic Nose) can smell news feature by simulating human, the Global Information of comprehensive characterization fragrance, embodies olfactory characteristic and the overall quality of fragrance, simultaneously more objective than the sense of smell of people, reliable.At present in food freshness, the rotten differentiation of edible oil, the detection of fruits and vegetables degree of ripeness, tea-leaf producing area variety ecotype, drinks brand define etc., carry out correlative study.
Electronic Nose is adopted to carry out product quality differentiation or adulterated discriminatory analysis, its essence is the overall fragrance information utilizing intelligent sense of smell collection of illustrative plates, find the otherness of sample room, its core finds the profile information of otherness between representative sample, i.e. " differentiation information ", also cry " the differentiation profile information of intelligent sense of smell ".But the sensor array of Electronic Nose has cross-sensitivity, namely every root sensor has response in various degree to each fragrance, therefore the aroma-producing substance collection of illustrative plates gathered by Electronic Nose has the feature such as wide spectrum, overlap, be difficult to the naked eye distinguish different sample from collection of illustrative plates separately, need to carry out " signal excavation ", particularly the excavation of differentiation information " between the representative sample ", the otherness information of excavation is more, more contributes to distinguishing product feature and quality efficiently.But also very weak in differentiation information excavating at present, be also the bottleneck of restriction Electronic Nose development.
China's honey output occupies first place in the world, and output keeps the trend that increases fast always in recent years, is increased to 40.2 ten thousand tons in 2009, accounts for Gross World Product and also bring up to more than 30% by nearly 20% by 25.2 ten thousand tons of calendar year 2001.But due to the driving of economic interests, current honey market is seriously adulterated, cause adulterated honey to occupy 20% ~ 30% of honey market, the bee product of some regional adulterated fraud accounts for about 50%, badly damaged consumer's interests, affects honey industry and develops in a healthy way, hits the export trade and earn foreign exchange.
Owing to lacking the impact of detection means, cause adulterated strike difficulties, its basic reason is as follows: (1) due to the main matter of honey itself relatively simple for structure, comprise water and carbohydrate content, to adulterated condition of providing convenience, meanwhile, depend merely on detect this several content of material number can not differentiate at all whether adulterated; (2) because honey is by the temperature and humidity of nectariferous plant kind, hive gesture power, sweet time phase length, air, and the various factors such as the processing of honey, storage, crystallization, cause the content range of honey main matter to change greatly, make honey adulteration simple, convenient; (3) detection of adulterations such as C4 costly, cannot detect and law enforcement for reality on a large scale.
Containing more than 300 kind of aromatic substance in honey, therefore it is the important sample that the intelligent sense of smell of research characterizes; Simultaneously different nectar source, its flavor substance of Different sources are different, and honey adulteration whether or quality can embody to some extent on overall fragrance, make fragrance become honey quality and detect and one of important indicator of adulterated discriminating; Absolutely prove and adopt intelligent sense of smell characterization of variation of honey quality to have feasibility, also for honey quality detects and adulterated discriminating provide a kind of fast, economical, accurately and be beneficial to the detection method applied in real time.Therefore select honey to have Practical significance as research object, far-reaching value is had more to its industry healthy development.
Summary of the invention
Domestic and international present Research analysis shows, deep not enough for the information excavating of difference " in the intelligent sense of smell collection of illustrative plates between characterizing sample " research at present.Therefore, in four release stages (head perfume, front end fragrance, body note, bottom note) that the application embodies from honey fragrance difference, research represents the intelligent olfactory characteristic response point system of selection of " sample room differentiation information " in these four different phases; And " to extract between more honey differentiation characteristic information for target ", the extraction rule of honey differentiation Electronic Nose information in heuristic data compression reduction process, open " truth " that useful signal is separated with garbage signal, eliminate the background information of interference, improve the ratio of differentiation information and background information; Thus guarantee to set up reliable honey quality intelligence sense of smell discrimination model.
Be research object with honey, carry out the differentiation information excavating research that intelligent sense of smell characterizes; Disclose in intelligent sense of smell collection of illustrative plates and embody honey fragrance from the beginning perfume, front end fragrance, body note, to the response pattern of the dynamic volatilization process of bottom note, determine the characteristic response point comprising honey differentiation information; Explore the otherness discriminating power of proper vector when TuPu method extracts, illustrate the mechanism effectively extracting honey differentiation information; Finally reach the profile information accurately finding otherness between representative sample, set up high-precision honey quality intelligence sense of smell characterization model.
According to fragrance experience head perfume, front end fragrance, body note to the dynamic release feature of bottom note, smelt the characteristic perfume distinguished in (GC-O) qualitative and quantitative analysis honey volatile ingredient in conjunction with gas phase by gaseous mass spectrum (GC-MS).Define respectively at head perfume, front end fragrance, body note in bottom note four-stage, respective representative honey fragrance component, inquires into the dynamic volatilization rule of fragrance itself, builds the miel gas system of simulation thus.
Honey fragrance intelligence sense of smell dynamic response feature and the research of differentiation information dynamic characterization:
For the volatilization feature of honey aromatic substance, optimize Electronic Nose intelligence olfactometry systematic parameter, correct pre-service in conjunction with collection of illustrative plates, obtain the original dynamic fingerprint collection of illustrative plates of high s/n ratio.According to honey fragrance simulated system, in intelligent olfactory sensor, the features such as aroma quality migration, sensor array internal divergence and sensor chip physisorption are experienced in conjunction with honey fragrance, explore intelligent sense of smell at head perfume, front end fragrance, body note to the dynamic response feature of bottom note four-stage, instruct the selection representing the intelligent sense of smell behavioral characteristics response point of honey quality difference (as: between different nectar source, Different sources, different storage and true and false honey difference).Simultaneously in conjunction with the mathematical feature parameter (slope, flex point, maximal value etc.) in sense of smell collection of illustrative plates, catch the differentiation information that the sense of smell of honey quality intelligence characterizes comprehensively.
The profile information of the characterization of variation of honey poor quality opposite sex extracts research:
Analyze the linear or nonlinear data structure character of sense of smell finger-print of different plant nectar source, Different sources, different shelf time and different adulterated composition honey.Utilize the linear data dimensionality reduction extractive technique such as Wilks criterion, independent component analysis (ICA), explore the nonlinear data dimensionality reduction extractive technique such as core principle component analysis (KPCA), Self-organizing Maps (SOM) simultaneously; Analyze represent honey differentiation, for attribute classification eigenvector information extract mechanism, find the proper vector of honey differentiation information, evaluate the otherness discriminating power of its proper vector, eliminate the not obvious information of classification and background information, thus strengthen the ratio of differentiation information in fingerprint matrix, reach the target extracting differentiation characteristic information between honey.
The intelligent sense of smell discrimination model of honey quality difference sets up research:
Adopt linear model recognition methods (linear discriminant analysis, soft independent analysis) and Nonlinear Pattern Recognition (radial basis function neural network, support vector machine), set up the intelligent sense of smell discrimination model of five class honey quality differences: (1) nectar source differential pattern; (2) place of production differential pattern; (3) different storage model; (4) adulterated discrimination model; (5) model is differentiated in fraud.By comparing, find out the best intelligence sense of smell discrimination model of different honey uneven class size, the effect of checking differentiation information excavating, the intelligent sense of smell realizing honey odor characteristic characterizes.
The method that the application proposes not only facilitates the adulterated discriminating of honey and detects fast, also to comprehensive, objectivity, authenticity and validity that intelligent sense of smell characterizes other food aromas, there is directive significance, especially to open intelligent sense of smell information excavating new approaches, to the in-depth of Electronic Nose Technology with apply there is realistic meaning.The achievement of this project not only can be promoted the use of as intermediate product separately, and also will play a role in promoting for the development and perfection of intelligent sense of smell technology.
Accompanying drawing explanation
Fig. 1 Technology Roadmap
embodiment
(1) about sample collection and preparation
In order to from nectar source, the place of production, storage time, adulterated discriminating angularly study intelligent sense of smell differentiation information excavating under the different difference degree of honey quality, intend gathering current domestic honey and produce three kinds of representative honey samples.1) largeization product, throughout the year can the in all parts of the country rape honey of gathering honey, place of production distribution, 2) excellent flavor, extensively welcome by Market Consumer, simultaneously be also domestic main exported product, be adulterated acacia honey the most frequently in honey types again, 3) one of four your name's honey, the main honey product in the north, the representative of wild flower honey chaste honey.In order to guarantee the authenticity of sample from source, Chinese bee product association and honey research institute of the Chinese Academy of Agricultural Sciences is entrusted to gather the natural honey required for testing.
Because adulterated material common in honey is HFCS, fructose and glucose etc., according to the proportioning close to different adulterant in the adulterated honey in market, establishes the adulterated scheme based on these adulterants, configure corresponding adulterated honey sample; Explore miel to progress greatly the phenomenon that row directly fakes simultaneously, also gather rape honey essence, acacia honey essence and chaste honey essence.
(2) honey characteristic perfume is analyzed and the foundation of honey fragrance simulated system
Application Dynamic headspace (Itex) extracts honey aroma-producing substance in conjunction with circulation collection technology, after chromatographic column end carries out the distribution of 1:1 fragrance content, application gas chromatography mass spectrometry (GC-MS) and gas chromatography-its volatility of measurement of olfaction (GC-Olfactometry, GC-O) technology Simultaneously test are fragrant composition and sensory characteristic.Crystallized honey carries out heating water bath, is then cooled to room temperature rapidly, and in holding chamber, temperature constant state gathers aroma-producing substance.
Wherein in GC-MS, utilize mass spectrum (library searching), Relative Retention Indices (RI) and smell the volatile ingredient of news three kinds of method determination honey, and carry out inner mark method ration.GC-O technology is the method adopting frequency detecting and detected intensity to combine, and preferably smells the GC-O that the person of distinguishing forms evaluate group by 5, determines to represent respectively the characteristic flavor on basis activity fragrance of honey head perfume, front end fragrance, body note and bottom note four volatilization period.
According to the characteristic perfume contamination ratio of four volatilization period, proportioning builds basic honey fragrance simulated system A.On the basis of system A, build the four group systems variant with it.The difference often organizing system and primary structure A is embodied in two aspects, and namely in certain volatilization period or its characteristic perfume content difference, or its characteristic perfume component is different, and the aroma component of other three phases and content are all constant.
(3) the intelligent sense of smell collection of illustrative plates Dynamic Selection of characterization of variation of honey otherness
Utilize Static Headspace to gather honey volatile substance, obtained by orthogonal design and embody the best head space parameter of the maximum electric nasus system of honey quality differentiation and sample introduction parameter combinations.
According to this parameter combinations, gather the intelligent sense of smell collection of illustrative plates of five groups of honey fragrance simulated systems, after the pre-service of standardization collection of illustrative plates, determine the differentiation information characteristics response point of every root sensor collection of illustrative plates at head perfume, front end fragrance, body note and bottom note four volatilization period by significance test analysis.
Utilize the intelligent sense of smell finger-print of identical electric nasus system parameter acquisition natural honey, adulterated honey and honey essence; Heating water bath is carried out for crystallized honey, is then cooled to room temperature rapidly, and in holding chamber, temperature constant state gathers intelligent sense of smell finger-print.By collection of illustrative plates pre-service such as baseline correction, differentiate process, revise finger-print response error, improve the signal to noise ratio (S/N ratio) of collection of illustrative plates.Then according to the differentiation characteristic response point that fragrance simulated system obtains, the differentiation information that the sense of smell of honey quality intelligence characterizes is selected.
The further Dynamic Selection differentiation information such as the quadratic term system of the relative mean values of combined with intelligent sense of smell finger-print, relative integral value, average differential value, curve quadratic fit and Monomial coefficient.Utilize genetic algorithm to be optimized combination to Dynamic Response Information simultaneously, reduce the interference of redundancy gas signal, final selection can at the characteristic information collection of illustrative plates of head perfume, front end fragrance, body note and bottom note four volatilization period embodiment honey fragrance differences.
(4) the TuPu method vector of the characterization of variation of honey poor quality opposite sex extracts
Intelligence sense of smell collection of illustrative plates belongs to broad spectrum response, and its information overlap is serious, needs to carry out Data Dimensionality Reduction and feature extraction.At this, feature extraction dimensionality reduction mode from " with retain the original fragrance information of honey for main target and dimensionality reduction " be converted to " to extract between more honey differentiation characteristic information for target ", mainly take the feature extracting method that four kinds are different.
First, obtain the score vector after dimensionality reduction not directly as proper vector through principal component analysis (PCA), and adopt Wilks criterion to calculate the deviation ratio of any two score vectors.Deviation is than less, and these are more to honey otherness information contained by score vector, thus judge the discriminating power that each score vector is right, extract embody at utmost classifying quality score vector as proper vector.
Secondly, utilize independent component analysis (ICA), according to the principle of statistical iteration, from superposed signal, isolate each independent information component, extract first kind tagsort information, get rid of Equations of The Second Kind and to classify unconspicuous information and the 3rd class error message.
Then, adopt core principle component analysis (KPCA), select gaussian radial basis function kernel function that PCA is expanded to high dimensional nonlinear space, be separated the non-linear differentiation information that superposition is serious.
Finally, utilize Self-organizing Maps (SOM) that the characteristic of division information of reflection honey original flavor data is generated cluster.By Nonlinear feature extraction means, the relevant classified information be dispersed in numerous primitive character or authentication information are focused in a small amount of new feature.
(5) the intelligent sense of smell characterization model about honey sources, the place of production, shelf time, the different aromas difference such as adulterated is set up
Adopt Kennard-Stone method that honey and adulterated goods sample set are divided into calibration set and forecast set, calibration set is used for the foundation of follow-up honey quality intelligence sense of smell characterization model, and forecast set is used for the follow-up estimated performance evaluation to characterization model.
Adopt the linear model recognition methods such as linear discriminant analysis (LDA), soft independent analysis (SIMCA) respectively, with radial basis function neural network (RBF-ANN), support vector machine (SVM) Nonlinear Pattern Recognition, set up the qualitative mathematics model between characterization of variation of honey qualitative characteristics and intelligent sense of smell collection of illustrative plates.
Verify through the differentiation information selection of intelligent sense of smell collection of illustrative plates and after extracting, the discriminant classification performance of five class characterization model (nectar source differential pattern, place of production differential pattern, different storage model, adulterated discrimination model, fraud differentiate model).By model optimization, draw the optimal mode method for building up of sign five class honey quality difference.
Claims (1)
1., to the method that honey fragrance intelligence sense of smell dynamic response feature and differentiation information dynamic characterization are studied, it is characterized in that comprising the steps:
(1) about sample collection and preparation
Gather current domestic honey and produce three kinds of representative honey samples: 1) largeization product, throughout the year can the in all parts of the country rape honey of gathering honey, place of production distribution; 2) excellent flavor, extensively welcome by Market Consumer, simultaneously be also domestic main exported product, be adulterated acacia honey the most frequently in honey types again; 3) chaste honey of one of four your name's honey, the main honey product in the north, the representative of wild flower honey;
According to the proportioning close to different adulterant in the adulterated honey in market, establish the adulterated scheme based on HFCS, fructose and glucose, configure corresponding adulterated honey sample; Gather rape honey essence, acacia honey essence and chaste honey essence, be respectively used to be mixed with corresponding false rape honey, false acacia honey, false chaste honey, the phenomenon that row is directly faked thus embodiment employing miel progresses greatly;
(2) honey characteristic perfume is analyzed and the foundation of honey fragrance simulated system
Application Dynamic headspace extracts honey aroma-producing substance in conjunction with circulation collection technology, and after chromatographic column end carries out the distribution of 1:1 fragrance content, application gas chromatography mass spectrometry and gas chromatography-its volatility of measurement of olfaction technology Simultaneously test are fragrant composition and sensory characteristic; Crystallized honey carries out heating water bath, is then cooled to room temperature rapidly, and in holding chamber, temperature constant state gathers aroma-producing substance;
According to the characteristic perfume contamination ratio of honey head perfume, front end fragrance, body note and bottom note four volatilization period, proportioning builds basic honey fragrance simulated system A; On the basis of described fragrance simulated system A, build the four group systems variant with it; The difference wherein often organizing system and fragrance simulated system A is embodied in two aspects, one is different from fragrance simulated system A at its characteristic perfume content of certain volatilization period, or its characteristic perfume component is different from fragrance simulated system A, and the aroma component of other three phases is identical with fragrance simulated system A with content;
(3) the intelligent sense of smell collection of illustrative plates Dynamic Selection of characterization of variation of honey otherness
Utilize Static Headspace to gather honey volatile substance, obtained by orthogonal design and embody the best head space parameter of the maximum electric nasus system of honey quality differentiation and sample introduction parameter combinations;
According to this best head space parameter and sample introduction parameter combinations, gather the intelligent sense of smell collection of illustrative plates of five groups of honey fragrance simulated systems, after the pre-service of standardization collection of illustrative plates, determine the differentiation information characteristics response point of every root sensor collection of illustrative plates at head perfume, front end fragrance, body note and bottom note four volatilization period by significance test analysis;
Utilize the intelligent sense of smell finger-print of identical electric nasus system parameter acquisition natural honey, adulterated honey and honey essence; Heating water bath is carried out for crystallized honey, is then cooled to room temperature rapidly, and in holding chamber, temperature constant state gathers intelligent sense of smell finger-print; By baseline correction, differentiate process, revise finger-print response error, improve the signal to noise ratio (S/N ratio) of collection of illustrative plates; Then according to the differentiation characteristic response point that fragrance simulated system obtains, the differentiation information that the sense of smell of honey quality intelligence characterizes is selected;
The quadratic term coefficient of the relative mean values of combined with intelligent sense of smell finger-print, relative integral value, average differential value, curve quadratic fit and Monomial coefficient further Dynamic Selection differentiation information; Utilize genetic algorithm to be optimized combination to Dynamic Response Information simultaneously, reduce the interference of redundancy gas signal, final selection can at the characteristic information collection of illustrative plates of head perfume, front end fragrance, body note and bottom note four volatilization period embodiment honey fragrance differences;
(4) the TuPu method vector of the characterization of variation of honey poor quality opposite sex extracts
Mainly take the feature extracting method that four kinds are different:
One, Wilks criterion is adopted to calculate the deviation ratio of any two score vectors; Deviation is than less, and these are more to honey otherness information contained by score vector, thus judge the discriminating power that each score vector is right, extract and embody the score vector of at utmost classifying quality as proper vector;
Two, utilize independent component analysis (ICA), according to the principle of statistical iteration, from superposed signal, isolate each independent information component, extract first kind tagsort information, get rid of Equations of The Second Kind and to classify unconspicuous information and the 3rd class error message;
Three, adopt core principle component analysis (KPCA), select gaussian radial basis function kernel function that PCA is expanded to high dimensional nonlinear space, be separated the non-linear differentiation information that superposition is serious;
Four, utilize Self-organizing Maps (SOM) that the characteristic of division information of reflection honey original flavor data is generated cluster; By Nonlinear feature extraction means, the relevant classified information be dispersed in numerous primitive character or authentication information are focused in a small amount of new feature;
(5) the honey quality intelligence sense of smell characterization model about honey sources, the place of production, shelf time, adulterated different aromas difference is set up, adopt Kennard-Stone method that honey and adulterated goods sample set are divided into calibration set and forecast set, calibration set is used for the foundation of follow-up honey quality intelligence sense of smell characterization model, and forecast set is used for the follow-up estimated performance evaluation to honey quality intelligence sense of smell characterization model;
Adopt linear discriminant analysis (LDA), the recognition methods of soft independent analysis (SIMCA) linear model respectively, with radial basis function neural network (RBF-ANN), support vector machine (SVM) Nonlinear Pattern Recognition, set up the qualitative mathematics model between characterization of variation of honey qualitative characteristics and intelligent sense of smell collection of illustrative plates;
Verify through the differentiation information selection of intelligent sense of smell collection of illustrative plates and after extracting, the discriminant classification performance of nectar source differential pattern, place of production differential pattern, different shelf time model, adulterated discrimination model, this five classes honey quality intelligence sense of smell characterization model of fraud discriminating model; By model optimization, draw the optimal mode method for building up of sign five class honey quality difference.
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