CN103760139A - Method for identifying commercially available orange juice beverage based on three-dimensional fluorescence spectrum and robust mahalanobis distance - Google Patents
Method for identifying commercially available orange juice beverage based on three-dimensional fluorescence spectrum and robust mahalanobis distance Download PDFInfo
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Abstract
The present invention discloses a method for identifying a commercially available orange juice beverage based on a three-dimensional fluorescence spectrum and a robust mahalanobis distance. The method comprises: adopting fluorescence characteristic difference between orange juice components and food additives to establish three-dimensional fluorescence standard spectrum libraries of the freshly squeezed orange juice, the 100% qualification rate orange juice and the orange juice beverage, extracting the spectrum gravity center through a gravity center method to form the 100% orange juice standard feature database, measuring the three-dimensional fluorescence spectrum of a sample requiring identification and extracting the gravity center feature data, and calculating the robust mahalanobis distance to discriminate the sample requiring identification, wherein the discrimination threshold is 2.72. According to the method, the defects of complex process, detection time consuming, high detection cost and the like of the traditional chemical detection method are overcome, the rapid screening and identification on the sample requiring identification can be achieved, the advantages of rapidness, safety, reliability simple operation, low cost and the like are provided, the standardization on the fruit juice beverage industry and protection of consumer interests can be easily achieved, and food safety supervision on the fruit juice beverage can be promoted.
Description
Technical field
The invention provides a kind of method of differentiating commercially available orange juice drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance, belong to juice drinks detection and identification field.
Background technology
Orange juice drink is the juice drinks that a kind of consumer of enjoying likes, commercially available orange juice drink is broadly divided into 100% orange juice and the large class of orange beverage two according to juice content, carries out national standard GB/T 21731.At present, imperfection due to relevant criterion and detection method, fruit juice and fruit drink are mixed pseudo problem and are happened occasionally, some commercially available 100% orange juice is in fact by food additives such as adding antiseptic, thickening agent, artificial essence after concentrated orange juice thin up be made " orange beverage ", or even " the three smart water " that with allotments such as citric acid, sweetener, orange taste essence, thickening agent, synthetic dyestuffs, forms, consumer's interests and health are caused damage.Because commercially available orange juice beverage quality is uneven, consumer is difficult to be differentiated by simple sense organ judgement, and orange juice composition itself belongs to the potpourri material of more complicated, is difficult to by chemical method, it directly be measured.At present, detection and discriminating for orange juice drink, conventionally carry out national standard GB/T 16771, the characteristic component index of this standard using potassium, total phosphorus, amino-acid nitrogen, L-PROLINE, total D-isocitric acid and 6 kinds of compositions of general flavone as orange juice, but there is complex operation, detect consuming time, the shortcoming such as testing cost is high, result poor reproducibility in the method, therefore, be extremely necessary to find a kind of quick, convenient, stable, reliable orange juice drink authentication technique.
Summary of the invention
Object of the present invention, is to provide a kind of method of differentiating commercially available orange juice drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance.
According to technical scheme of the present invention, the present invention realizes by following steps:
A. utilize fluorescence spectrophotometer to carry out three-dimensional fluorescence spectrum measurement to fresh squeezing orange juice, qualified commercially available 100% orange juice, orange beverage;
B. set up fresh squeezing orange juice, qualified commercially available 100% orange juice, orange beverage 3 class samples three-dimensional fluorescence standard spectrum storehouse separately;
C. analyze the difference of the fluorescent characteristic of fresh squeezing orange juice, 100% orange juice and orange beverage 3 classes, determine the fluorescent characteristics peak of orange juice composition in orange juice drink;
D. adopt spectrum center of gravity that three-dimensional fluorescence spectrum gravity model appoach extracts commercially available 100% orange juice sample as characteristic index, set up the property data base of qualified 100% orange juice sample;
E. utilize fluorescence spectrophotometer to carry out three-dimensional fluorescence spectrum measurement to sample to be identified;
F. to sample extraction three-dimensional fluorescence spectrum center of gravity to be identified as sample characteristic data, the center of gravity data of this sample and qualified 100% orange juice property data base are merged into a matrix, calculate its sane mahalanobis distance, if sane mahalanobis distance surpasses threshold value MD=2.72, sample to be identified is judged to be non-100% orange juice, Output rusults 0, otherwise Output rusults 1, be judged to be qualified 100% orange juice, export identification result simultaneously;
G. if desired, the non-100% orange juice sample that is 0 to Output rusults carries out further spectral analysis, determines the concrete drink type of non-100% orange juice sample.
In described step c, adopt fluorescence spectrum analysing method to differentiate orange juice drink, in orange juice drink, the fluorescent characteristics peak of orange juice composition is 470/526nm, the fluorescence intensity of this fluorescence peak disclose orange juice content in orange juice drink number, other fluorescence peak occurring in three-dimensional fluorescence spectrum is all to be caused by food additives.
In described steps d, center of gravity parameter (x
0, y
0) extract and to calculate according to center of gravity formula
In formula, x is excitation wavelength, and y is emission wavelength,
for Excitation-emission matrix data.
In described step f, general mahalanobis distance is expressed as:
Wherein,
be respectively
with
the two-dimensional matrix (p=2) that the spectrum center of gravity parameter of individual sample forms,
for
the inverse matrix of covariance matrix, and the method that sane mahalanobis distance is estimated by sane minimization covariance determinant (MCD) catches the sane covariance structure of body data, its definition is:
Wherein,
,
be respectively again weighted mean and sane covariance matrix.Square general obedience of mahalanobis distance is asymmetrical
distribute, so its critical value MD=
=
=2.72, equal degree of freedom and be 2, fractile is 97.5%
the square root distributing.
In described step g, the three-dimensional fluorescence spectrum of the non-100% orange juice sample that is 0 by identification result and fresh squeezing orange juice, qualified 100% orange juice, orange beverage contrasts, contrast content comprises whether there is 470/526nm fluorescent characteristics peak, the fluorescence intensity at this fluorescent characteristics peak, the fluorescence peak that whether has varieties of food items adjuvant, thus determine the concrete drink type of non-100% orange juice sample.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the invention will be further described.
Fig. 1 orange juice drink identification flow figure.
Fig. 2, Fig. 3, Fig. 4 are respectively the three-dimensional fluorescence spectrum figure of fresh squeezing orange juice, commercially available certain brand 100% orange juice, certain brand orange beverage, and in figure, (a) is isogonism three-dimensional projection, (b) is contour map.
Fig. 5 is the gravity centre distribution of commercially available 100% orange juice standard three-dimensional fluorescence spectrum and sample three-dimensional fluorescence spectrum figure to be identified, and adds the sane tolerance ellipse of 97.5% degree of confidence, and the spectrum center of gravity of qualified 100% orange juice is in elliptic region.
Fig. 6 schemes by calculating the discriminating of the sample to be identified that sane mahalanobis distance obtains.
Embodiment
Below in conjunction with accompanying drawing and according to the sequence of operation of process flow diagram, the invention will be further described:
A. sample is fresh squeezing orange juice, commercially available 100% orange juice, orange beverage 3 classes, after centrifugal treating, utilize fluorescence spectrophotometer to carry out three-dimensional fluorescence spectrum measurement to all samples, excitation wavelength range is set to 300nm-600nm, and step-length is set to 5nm, and emission wavelength ranges is set to 300nm-700nm, step-length is set to 1nm, for eliminating the impact of Rayleigh scattering, emission wavelength scanning position postpones 15nm with respect to excitation wavelength, and all samples is all measured under identical parameter setting and experiment condition.Fig. 2, Fig. 3, Fig. 4 are respectively the three-dimensional fluorescence spectrum figure of fresh squeezing orange juice, commercially available 100% orange juice, orange beverage, and horizontal ordinate represents emission wavelength, and scope is 300nm-600nm, is spaced apart 1nm; Ordinate represents excitation wavelength, and scope is 300nm-700nm, is spaced apart 5nm;
B. utilize Origin or MATLAB software to realize three-dimension curved surface matching, obtain the three-dimensional fluorescence spectrum of fresh squeezing orange juice, 100% orange juice, orange beverage, set up 3 class samples three-dimensional fluorescence standard spectrum storehouse separately;
C. analyze the fluorescent characteristic difference of 3 class samples, determine the fluorescent characteristics peak of orange juice composition in orange juice drink;
D. utilize MATLAB software, write spectrum center of gravity extraction procedure, obtain qualified commercially available 100% orange juice sample spectrum diagram gravity centre distribution separately, set up its spectrum characteristic data storehouse, as shown in Figure 5;
E. under identical measuring condition, utilize fluorescence spectrophotometer to measure the three-dimensional fluorescence spectrum of sample to be identified;
F. utilize MATLAB center of gravity extraction procedure to extract the spectrum center of gravity of sample to be identified as the characteristic of this sample, the center of gravity data of this sample and qualified 100% orange juice property data base are merged into a matrix, calculate its sane mahalanobis distance, and figure is differentiated in output, as shown in Figure 6, if the sane mahalanobis distance of sample to be identified is greater than critical value MD=2.72, sample to be identified is judged to be non-100% orange juice, Output rusults 0, otherwise Output rusults 1, be judged to be qualified 100% orange juice, export identification result simultaneously;
G. if desired, can be by further spectral analysis, the three-dimensional fluorescence spectrum of the three-dimensional fluorescence spectrum of the sample to be identified that is 0 by Output rusults and fresh squeezing orange juice, qualified 100% orange juice, orange beverage contrasts, and determines the concrete drink type of non-100% orange juice sample.
In described step c, by relatively can find the three-dimensional fluorescence spectrum of fresh squeezing orange juice, commercially available 100% orange juice, orange beverage 3 class samples, in orange juice drink, the fluorescence spectrum peak of orange juice composition is 470/526nm, the fluorescence intensity of this fluorescence peak disclosed orange juice content in sample number, if this fluorescence peak occurs in drink to be measured, think in sample to be identified and only contain minute quantity orange juice or do not contain orange juice.Simultaneously; the three-dimensional fluorescence spectrum of commercially available 100% orange juice and orange beverage is except the fluorescent characteristics peak that contains orange juice composition; conventionally also contain the fluorescent characteristics peak of 1 to 2 food additives; as shown in Figure 3; except the fluorescent characteristics peak (470/526nm) that contains orange juice composition, also there is the fluorescent characteristics peak (420/677nm) of thickening agent carragheen in the three-dimensional fluorescence spectrum of commercially available 100% orange juice.
In described steps d, center of gravity parameter (x
0, y
0) extract and to calculate according to center of gravity formula
In formula
for excitation wavelength,
for emission wavelength,
for Excitation-emission matrix data.
In described step f, general mahalanobis distance is expressed as:
Wherein,
be respectively
with
the two-dimensional matrix (p=2) that the spectrum center of gravity parameter of individual sample forms,
for
the inverse matrix of covariance matrix, and the method that sane mahalanobis distance is estimated by sane minimization covariance determinant (MCD) catches the sane covariance structure of body data, its definition is:
Wherein,
,
be respectively again weighted mean and sane covariance matrix.Square general obedience of mahalanobis distance is asymmetrical
distribute, so its critical value MD=
=
=2.72, equal degree of freedom and be 2, fractile is 97.5%
the square root distributing.
In described step g, the three-dimensional fluorescence spectrum of the non-100% orange juice sample that is 0 by identification result and fresh squeezing orange juice, qualified 100% orange juice, orange beverage contrasts, contrast content comprises whether there is 470/526nm fluorescent characteristics peak, the fluorescence intensity at 470/526nm fluorescent characteristics peak, the fluorescence peak that whether has varieties of food items adjuvant, thus determine the concrete drink type of non-100% orange juice sample.
Example is implemented:
(1) set up three-dimensional fluorescence standard spectrum storehouse and property data base.Choose fresh squeezing orange juice, commercially available qualified 100% orange juice, orange beverage as standard model, utilize FLS920 type fluorescence spectrophotometer to measure three-dimensional fluorescence spectrum, set up 3 class samples three-dimensional fluorescence standard spectrum storehouse separately, its collection of illustrative plates form respectively as shown in Figure 2, Figure 3, Figure 4.Meanwhile, adopt the three-dimensional fluorescence spectrum center of gravity of the commercially available qualified 100% orange juice sample of three-dimensional fluorescence spectrum gravity model appoach extraction, set up the property data base of 100% orange juice;
(2) three-dimensional fluorescence spectrum of sample to be identified is measured and feature extraction.Choose 6 samples to be identified (sample number into spectrum 1-6) that supermarket is bought, utilize FLS920 type fluorescence spectrophotometer to measure the three-dimensional fluorescence spectrum of each sample to be identified, meanwhile, adopt three-dimensional fluorescence spectrum gravity model appoach to extract three-dimensional fluorescence spectrum center of gravity as characteristic index;
(3) the sane mahalanobis distance that calculates sample to be identified is differentiated it.The spectrum center of gravity data of the spectrum center of gravity data of 6 samples to be identified and 100% orange juice property data base are merged into a matrix, calculate the sane mahalanobis distance of sample to be identified, and output discriminating figure, as shown in Figure 6, export identification result simultaneously;
(4) if desired, can, by further spectral analysis, determine that identification result is 0 the concrete drink type of non-100% orange juice sample.As in this example, all there is difference with respect to qualified 100% orange juice in 6 samples, is therefore non-100% orange juice.By spectrum, compare and can find, the three-dimensional fluorescence spectrum of the three-dimensional fluorescence spectrum of No. 1 sample and qualified 100% orange juice is basically identical, do not have the fluorescence peak of other food additives to occur, but the fluorescence intensity of 470/526nm orange juice ingredient fluorescence characteristic peak is starkly lower than qualified 100% orange juice, this sample drink type is orange juice, but orange juice content is on the low side; All there is the fluorescent characteristics peak of food additives in 2-5 sample, and the fluorescence intensity of 470/526nm orange juice ingredient fluorescence characteristic peak approximately only has 1/5 of qualified 100% orange juice, so its drink type is orange beverage; The spectrum center of gravity of No. 6 samples far deviates from qualified 100% orange juice, by comparison 470/526nm orange juice ingredient fluorescence characteristic peak, find, this sample is without obvious 470/526nm fluorescence peak, and this sample does not contain or contain minute quantity orange juice composition, so its drink type is orange taste soda.
In sum, the present invention first measures and has set up the three-dimensional fluorescence standard spectrum storehouse of fresh squeezing orange juice, qualified 100% orange juice, orange beverage, by three-dimensional fluorescence spectrum gravity model appoach, extract the standard feature database that spectrum center of gravity forms 100% orange juice, then measure the three-dimensional fluorescence spectrum of sample to be identified and extract gravity center characteristics data, utilize sane mahalanobis distance to differentiate sample to be identified, can carry out further spectral analysis to being judged to be the sample of non-100% orange juice, determine the drink type that it is concrete simultaneously.Therefore; with respect to existing juice drinks discrimination method; can realize the discriminating of sample to be identified and screening; there is the advantages such as quick, reliable, simple to operate, cost is lower; made up traditional chemical detection method process loaded down with trivial details, detect consuming time, the more high deficiency of testing cost; for standard juice drinks industry and Protection of consumer rights and interests provide technical guarantee, promote the food safety Regulation of fruit juice class drink.
Claims (5)
1. based on three-dimensional fluorescence spectrum and sane mahalanobis distance, differentiate a method for commercially available orange juice drink, described discrimination method step is as follows:
A. utilize fluorescence spectrophotometer to carry out three-dimensional fluorescence spectrum measurement to fresh squeezing orange juice, qualified commercially available 100% orange juice, orange beverage;
B. set up fresh squeezing orange juice, qualified commercially available 100% orange juice, orange beverage 3 class samples three-dimensional fluorescence standard spectrum storehouse separately;
C. analyze the difference of the fluorescent characteristic of fresh squeezing orange juice, 100% orange juice and orange beverage 3 classes, determine the fluorescent characteristics peak of orange juice composition in orange juice drink;
D. adopt spectrum center of gravity that three-dimensional fluorescence spectrum gravity model appoach extracts commercially available 100% orange juice sample as characteristic index, set up the property data base of qualified 100% orange juice sample;
E. utilize fluorescence spectrophotometer to carry out three-dimensional fluorescence spectrum measurement to sample to be identified;
F. to sample extraction three-dimensional fluorescence spectrum center of gravity to be identified as sample characteristic data, the center of gravity data of this sample and qualified 100% orange juice property data base are merged into a matrix, calculate its sane mahalanobis distance, if sane mahalanobis distance surpasses threshold value MD=2.72, sample to be identified is judged to be non-100% orange juice, Output rusults 0, otherwise Output rusults 1, be judged to be qualified 100% orange juice, export identification result simultaneously;
G. if desired, the non-100% orange juice sample that is 0 to Output rusults carries out further spectral analysis, determines the concrete drink type of non-100% orange juice sample.
2. a kind of method of differentiating commercially available orange juice drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance according to claim 1, it is characterized in that: in described step c, adopt fluorescence spectrum analysing method to differentiate orange juice drink, in orange juice drink, the fluorescent characteristics peak of orange juice composition is 470/526nm, the fluorescence intensity of this fluorescence peak disclose orange juice content in orange juice drink number, other fluorescence peak occurring in three-dimensional fluorescence spectrum is all to be caused by food additives.
3. a kind of method of differentiating commercially available orange juice drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance according to claim 1, is characterized in that: in described steps d, and center of gravity parameter (x
0, y
0) extract and to calculate according to center of gravity formula
In formula, x is excitation wavelength, and y is emission wavelength,
for Excitation-emission matrix data.
4. a kind of method of differentiating commercially available orange juice drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance according to claim 1, is characterized in that: in described step f, general mahalanobis distance is expressed as:
Wherein,
be respectively
with
the two-dimensional matrix (p=2) that the spectrum center of gravity parameter of individual sample forms,
for
the inverse matrix of covariance matrix, and the method that sane mahalanobis distance is estimated by sane minimization covariance determinant (MCD) catches the sane covariance structure of body data, its definition is:
Wherein,
,
be respectively again weighted mean and sane covariance matrix, square general obedience of mahalanobis distance is asymmetrical
distribute, its critical value MD=
=
=2.72, equal degree of freedom and be 2, fractile is 97.5%
the square root distributing.
5. a kind of method of differentiating commercially available orange juice drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance according to claim 1, it is characterized in that: in described step g, by the three-dimensional fluorescence spectrum of sample to be identified and fresh squeezing orange juice, commercially available 100% orange juice, orange beverage three-dimensional fluorescence standard spectrum storehouse are compared, relatively content comprises whether there is 470/526nm fluorescent characteristics peak, the fluorescence intensity at this fluorescent characteristics peak, the fluorescence peak that whether has varieties of food items adjuvant, thus determine the concrete drink type of non-100% orange juice sample.
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