CN103760139B - A kind of method differentiating commercially available orange drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance - Google Patents
A kind of method differentiating commercially available orange drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance Download PDFInfo
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- CN103760139B CN103760139B CN201310175204.4A CN201310175204A CN103760139B CN 103760139 B CN103760139 B CN 103760139B CN 201310175204 A CN201310175204 A CN 201310175204A CN 103760139 B CN103760139 B CN 103760139B
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Abstract
The invention discloses a kind of method differentiating commercially available orange drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance, utilize the difference of orange juice composition and food additives fluorescent characteristic, first the three-dimensional fluorescence standard spectrum storehouse of fresh squeezing orange juice, qualified 100% orange juice, orange beverage is set up, spectral centroid is extracted by gravity model appoach, form the standard feature database of 100% orange juice, then measure the three-dimensional fluorescence spectrum of sample to be identified and extract gravity center characteristics data, differentiate sample to be identified by calculating its sane mahalanobis distance, discrimination threshold is 2.72.The method compensate for traditional chemical detection method process loaded down with trivial details, detect consuming time, the more high deficiency of testing cost; the rapid screening to sample to be identified and discriminating can be realized; there is the advantages such as quick, safe, reliable, simple to operate, cost is lower; be conducive to the rights and interests of specification juice drinks industry and Protection of consumer, promote the food safety Regulation of juice drinks.
Description
Technical field
The invention provides a kind of method differentiating commercially available orange drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance, belong to juice drinks detection and identification field.
Background technology
Orange drink is the juice drinks that a kind of consumer of enjoying likes, commercially available orange drink is broadly divided into 100% orange juice and the large class of orange beverage two according to juice content, performs national standard GB/T 21731.At present, due to the imperfection of 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 made " orange beverage " by food additives such as adding antiseptic, thickening agent, artificial essence after concentrated orange juice thin up in fact, or even with " three smart water " that citric acid, sweetener, orange taste essence, thickening agent, synthetic dyestuff etc. are allocated, the interests of consumer and health are caused damage.Because commercially available orange drink quality is uneven, consumer is difficult to judge to be differentiated by simple sense organ, and orange juice composition itself belongs to the potpourri material of more complicated, is difficult to chemically directly measure it.At present, for detection and the discriminating of orange drink, usual execution national standard GB/T 16771, this standard is using potassium, total phosphorus, amino-acid nitrogen, L-PROLINE, total D-isocitric acid and general flavone 6 kinds of compositions characteristic component index 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 drink authentication technique.
Summary of the invention
Object of the present invention, is to provide a kind of method differentiating commercially available orange drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance.
According to technical scheme of the present invention, the present invention is realized by following steps:
A. fluorescence spectrophotometer is utilized to carry out three-dimensional fluorescence spectrum measurement to fresh squeezing orange juice, qualified commercially available 100% orange juice, orange beverage;
B. fresh squeezing orange juice, qualified commercially available 100% orange juice, orange beverage 3 class sample three-dimensional fluorescence standard spectrum storehouse is separately set up;
C. analyze the difference of the fluorescent characteristic of fresh squeezing orange juice, 100% orange juice and orange beverage 3 class, determine the fluorescent characteristics peak of orange juice composition in orange drink;
D. adopt three-dimensional fluorescence spectrum gravity model appoach to extract the spectral centroid of commercially available 100% juice samples as characteristic index, set up the property data base of qualified 100% juice samples;
E. fluorescence spectrophotometer is utilized 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 exceedes threshold value MD=2.72, sample to be identified is judged to be non-100% orange juice, Output rusults 0, on the contrary Output rusults 1, be judged to be qualified 100% orange juice, export identification result simultaneously;
G. if desired, further spectral analysis is carried out to non-100% juice samples that Output rusults is 0, determine the drink type that non-100% juice samples is concrete.
In described step c, fluorescence spectrum analysing method is adopted to differentiate orange drink, in orange 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 drink number, other fluorescence peak occurred in three-dimensional fluorescence spectrum is all caused by food additives.
In described steps d, center of gravity parameter (x
0, y
0) extract obtain according to center of gravity formulae discovery
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:
，
,
=1,2,3…..N
=[
]
Wherein,
be respectively
with
the two-dimensional matrix (p=2) of the spectral centroid parameter composition of individual sample,
for
the inverse matrix of covariance matrix, and sane mahalanobis distance catches the sane covariance structure of body data by the method that sane minimization covariance determinant (MCD) is estimated, its definition is:
Wherein,
,
be respectively again weighted mean and sane covariance matrix.Square general obedience of mahalanobis distance is asymmetrical
distribution, therefore its critical value MD=
=
=2.72, namely equal that degree of freedom is 2, fractile is 97.5%
the square root of distribution.
In described step g, by identification result be 0 non-100% juice samples and fresh squeezing orange juice, qualified 100% orange juice, orange beverage three-dimensional fluorescence spectrum contrast, contrast content comprises whether there is 470/526nm fluorescent characteristics peak, the fluorescence intensity at this fluorescent characteristics peak, whether there is the fluorescence peak of varieties of food items adjuvant, thus determine the drink type that non-100% juice samples is concrete.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the invention will be further described.
Fig. 1 orange drink identification flow figure.
Fig. 2, Fig. 3, Fig. 4 are respectively the three-dimensional fluorescence spectrum figure of fresh squeezing orange juice, certain brand 100% orange juice commercially available, certain brand orange beverage, and in figure, (a) is isogonism three-dimensional projection, and (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 the sane tolerance of adding 97.5% degree of confidence is oval, and the spectral centroid of qualified 100% orange juice is in elliptic region.
Fig. 6 is the discriminating figure by calculating the sample to be identified that sane mahalanobis distance obtains.
Embodiment
Below in conjunction with accompanying drawing and the invention will be further described according to the sequence of operation of process flow diagram:
A. sample is fresh squeezing orange juice, commercially available 100% orange juice, orange beverage 3 class, after centrifugal treating, fluorescence spectrophotometer is utilized 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 relative to excitation wavelength, and all samples is all measured under identical optimum configurations 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 the matching of Origin or MATLAB software simulating three-dimension curved surface, 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 drink;
D. utilize MATLAB software, write spectral centroid extraction procedure, obtain qualified commercially available 100% juice samples spectrogram gravity centre distribution separately, set up its spectrum characteristic data storehouse, as shown in Figure 5;
E., under identical measuring condition, fluorescence spectrophotometer is utilized to measure the three-dimensional fluorescence spectrum of sample to be identified;
F. MATLAB center of gravity extraction procedure is utilized to extract the characteristic of spectral centroid as this sample of sample to be identified, 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 export discriminating figure, 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, by further spectral analysis, be the three-dimensional fluorescence spectrum of the sample to be identified of 0 and fresh squeezing orange juice by Output rusults, the three-dimensional fluorescence spectrum of qualified 100% orange juice, orange beverage contrasts, determine the drink type that non-100% juice samples is concrete.
In described step c, by relatively can finding of the three-dimensional fluorescence spectrum to fresh squeezing orange juice, commercially available 100% orange juice, orange beverage 3 class sample, in orange drink, the fluorescence spectrum peak of orange juice composition is 470/526nm, the fluorescence intensity of this fluorescence peak discloses the number of orange juice content in sample, if not this fluorescence peak appearance in drink to be measured, then think that sample to be identified is interior only containing minute quantity orange juice or not containing orange juice.Simultaneously; the three-dimensional fluorescence spectrum of commercially available 100% orange juice and orange beverage is except the fluorescent characteristics peak containing orange juice composition; usually the fluorescent characteristics peak also containing 1 to 2 food additives; as shown in Figure 3; except the fluorescent characteristics peak (470/526nm) containing 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 obtain according to center of gravity formulae discovery
In formula
for excitation wavelength,
for emission wavelength,
for Excitation-emission matrix data.
In described step f, general mahalanobis distance is expressed as:
，
,
=1,2,3…..N
=[
]
Wherein,
be respectively
with
the two-dimensional matrix (p=2) of the spectral centroid parameter composition of individual sample,
for
the inverse matrix of covariance matrix, and sane mahalanobis distance catches the sane covariance structure of body data by the method that sane minimization covariance determinant (MCD) is estimated, its definition is:
Wherein,
,
be respectively again weighted mean and sane covariance matrix.Square general obedience of mahalanobis distance is asymmetrical
distribution, therefore its critical value MD=
=
=2.72, namely equal that degree of freedom is 2, fractile is 97.5%
the square root of distribution.
In described step g, by identification result be 0 non-100% juice samples and fresh squeezing orange juice, qualified 100% orange juice, orange beverage three-dimensional fluorescence spectrum contrast, contrast content comprises whether there is 470/526nm fluorescent characteristics peak, the fluorescence intensity at 470/526nm fluorescent characteristics peak, whether there is the fluorescence peak of varieties of food items adjuvant, thus determine the drink type that non-100% juice samples is concrete.
Example is implemented:
(1) three-dimensional fluorescence standard spectrum storehouse and property data base is set up.Choose fresh squeezing orange juice, commercially available qualified 100% orange juice, orange beverage as standard model, FLS920 type fluorescence spectrophotometer is utilized 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 three-dimensional fluorescence spectrum gravity model appoach to extract the three-dimensional fluorescence spectrum center of gravity of commercially available qualified 100% juice samples, 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 calculating sample to be identified is differentiated it.The spectral centroid data of the spectral centroid data of 6 samples to be identified and 100% orange juice property data base are merged into a matrix, calculates the sane mahalanobis distance of sample to be identified, and export discriminating figure, as shown in Figure 6, export identification result simultaneously;
(4) if desired, by further spectral analysis, determine that identification result is the concrete drink type of non-100% juice samples of 0.As in this example, all there is difference relative to qualified 100% orange juice in 6 samples, is therefore non-100% orange juice.Can be found by spectrum comparison, the three-dimensional fluorescence spectrum of No. 1 sample and the three-dimensional fluorescence spectrum of qualified 100% orange juice basically identical, the fluorescence peak of other food additives is not had 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, and therefore its drink type is orange beverage; The spectral centroid of No. 6 samples far deviates from qualified 100% orange juice, found by comparison 470/526nm orange juice ingredient fluorescence characteristic peak, this sample is without obvious 470/526nm fluorescence peak, and namely this sample does not contain or contains minute quantity orange juice composition, and therefore its drink type is orange taste soda.
In sum, the present invention first measures and establishes the three-dimensional fluorescence standard spectrum storehouse of fresh squeezing orange juice, qualified 100% orange juice, orange beverage, the standard feature database of 100% orange juice is formed by three-dimensional fluorescence spectrum gravity model appoach extraction spectral centroid, then measure the three-dimensional fluorescence spectrum of sample to be identified and extract gravity center characteristics data, sane mahalanobis distance is utilized to differentiate sample to be identified, to being judged to be that the sample of non-100% orange juice carries out further spectral analysis, its concrete drink type can be determined simultaneously.Therefore; relative to existing juice drinks discrimination method; the discriminating to sample to be identified and screening can be realized; there is the advantages such as quick, reliable, simple to operate, cost is lower; compensate for traditional chemical detection method process loaded down with trivial details, detect consuming time, the more high deficiency of testing cost; for specification juice drinks industry and Protection of consumer rights and interests provide technical guarantee, promote the food safety Regulation of juice drink.
Claims (5)
1. differentiate a method for commercially available orange drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance, described discrimination method step is as follows:
A. fluorescence spectrophotometer is utilized to carry out three-dimensional fluorescence spectrum measurement to fresh squeezing orange juice, qualified commercially available 100% orange juice, orange beverage;
B. fresh squeezing orange juice, qualified commercially available 100% orange juice, orange beverage 3 class sample three-dimensional fluorescence standard spectrum storehouse is separately set up;
C. analyze the difference of the fluorescent characteristic of fresh squeezing orange juice, 100% orange juice and orange beverage 3 class, determine the fluorescent characteristics peak of orange juice composition in orange drink;
D. adopt three-dimensional fluorescence spectrum gravity model appoach to extract the spectral centroid of commercially available 100% juice samples as characteristic index, set up the property data base of qualified 100% juice samples;
E. fluorescence spectrophotometer is utilized 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 exceedes threshold value MD=2.72, sample to be identified is judged to be non-100% orange juice, Output rusults 0, on the contrary Output rusults 1, be judged to be qualified 100% orange juice, export identification result simultaneously;
G. further spectral analysis is carried out to non-100% juice samples that Output rusults is 0, determine the drink type that non-100% juice samples is concrete.
2. a kind of method differentiating commercially available orange drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance according to claim 1, it is characterized in that: in described step c, fluorescence spectrum analysing method is adopted to differentiate orange drink, in orange 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 drink number, other fluorescence peak occurred in three-dimensional fluorescence spectrum is all caused by food additives.
3. a kind of method differentiating commercially available orange drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance according to claim 1, is characterized in that: in described steps d, center of gravity parameter (x
0, y
0) extract obtain according to center of gravity formulae discovery
In formula, x is excitation wavelength, and y is emission wavelength, and f (x, y) is Excitation-emission matrix data.
4. a kind of method differentiating commercially available orange drink based on three-dimensional fluorescence spectrum and sane mahalanobis distance according to claim 1, it is characterized in that: in described step f, general mahalanobis distance is expressed as:
MD(x
i，x
j)＝[(x
i-x
j)S
-1(x
i-x
j)
T]
1/2，i,j＝1,2,3…..N
x
i，x
j＝[y
0x
0]
Wherein, x
i, x
jbe respectively the i-th two-dimensional matrix (p=2) formed with the spectral centroid parameter of a jth sample, S
-1for the inverse matrix of x covariance matrix, and sane mahalanobis distance catches the sane covariance structure of body data by the method that sane minimization covariance determinant (MCD) is estimated, its definition is:
Wherein, μ
mCD, S
mCDbe respectively again weighted mean and sane covariance matrix, square asymmetrical χ of general obedience of mahalanobis distance
2distribution, its critical value
namely equal that degree of freedom is 2, fractile is the χ of 97.5%
2the square root of distribution.
5. a kind of method differentiating commercially available orange 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, whether there is the fluorescence peak of varieties of food items adjuvant, thus determine the drink type that non-100% juice samples is concrete.
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| CN104749150A (en) * | 2015-04-01 | 2015-07-01 | 宁波工程学院 | Edible oil quality fast identification method and identification device based on three-dimensional fluorescence spectrum |
| CN105184004B (en) * | 2015-09-18 | 2018-01-23 | 南京富岛信息工程有限公司 | A kind of method for judging the renewal of octane number model maintenance |
| CN110554013B (en) * | 2019-08-29 | 2022-05-20 | 华夏安健物联科技(青岛)有限公司 | Method for realizing rapid identification and comparison by using fluorescence spectrum characteristic information |
| CN113960007B (en) * | 2021-10-29 | 2024-03-05 | 杭州食疗晶元生物科技有限公司 | Method for identifying organic food based on food structure energy and processing energy storage |
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