CN108872176A - A kind of edible vegetable oil quality detecting method based on metalloporphyrin probe - Google Patents
A kind of edible vegetable oil quality detecting method based on metalloporphyrin probe Download PDFInfo
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- CN108872176A CN108872176A CN201810864301.7A CN201810864301A CN108872176A CN 108872176 A CN108872176 A CN 108872176A CN 201810864301 A CN201810864301 A CN 201810864301A CN 108872176 A CN108872176 A CN 108872176A
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- vegetable oil
- edible vegetable
- metalloporphyrin
- probe
- oil quality
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N2021/6417—Spectrofluorimetric devices
- G01N2021/6419—Excitation at two or more wavelengths
Abstract
Edible vegetable oil quality detecting method based on metalloporphyrin fluorescent probe technique is related to a kind of metalloporphyrin probe-type detection method for the edible vegetable oil difference state of oxidation.Utilize zinc protoporphyrin(ZnTPP)When encountering edible vegetable oil oxidation metabolites, its fluorescence spectrum generates specific variations principle, edible vegetable oil sample is added directly into ZnTPP probe organic solution, edible vegetable oil state of oxidation situation of change can determine whether according to ZnTPP fluorescence probe changing condition.The present invention provides it is a kind of it is easy to operate, detection speed is fast, low-cost edible vegetable oil state of oxidation rapid detection method.
Description
Technical field
The present invention relates to a kind of rapid detection methods for food plant oil quality, refer in particular to based on metalloporphyrin probe
Edible vegetable oil state of oxidation rapid detection method.
Technical background
Edible vegetable oil is in production, processing, storage, the fatty acid under the effect of oxygen, light, temperature and metallic atom
Double bond position carries out radical reaction, forms a series of small molecule peroxide, ultimately generates a series of acids, aldehydes, ketone
With the small molecule metabolites such as esters.These oxidation metabolites do not only result in edible vegetable oil and rancid its quality of influence occur,
Serious person can generate adverse effect to consumer health.At the same time, edible vegetable oil processing enterprise is in order to promote product competition
Power, it will usually mark edible vegetable oil and be obtained by way of cold press.Some illegal businessmans are cold in order to be substituted using hot moulding mode
It squeezes to obtain higher oil yield, and pretends to be cold press edible vegetable oil to be sold with hot moulding edible vegetable oil.Excessive temperature
The generation of the harmful substances such as cyclophane hydro carbons, acrylamide is directly resulted in, the disease incidence such as cancer, leukaemia are increased.Therefore, for edible
Vegetable oil difference processing method, the oxidation metabolites detection under the storage period become the main side of evaluation food plant oil quality
Method.
For a long time, the evaluation of edible vegetable oil degree of oxidation is mainly using physico-chemical method to acid value, peroxide and total
Polar substances are evaluated.For large-scale food enterprise edible vegetable oil, acid value, peroxide and total polar substances etc. are changed
Learning index can accurately be linked up with its food plant oil quality.Acid value is primarily directed in edible vegetable oil oxidation process
Acidic materials increase this feature, food plant oil quality is evaluated.Pass through the modes such as chemical deacidification and physical refining
Reduce edible vegetable oil acid value.Peroxide is mainly that edible vegetable oil oxidation process can generate peroxide intermediate, peroxide
Compound content to a certain extent can be directly proportional to the edible vegetable oil state of oxidation, therefore peroxide is equally the edible plant of reflection
The important indicator of object oil quality.However, peroxide is more sensitive to temperature, can be effectively reduced by high-temperature process edible
Vegetable oil peroxide numerical value.Similarly, illegal businessman can eliminate total polar compound by modes such as physical absorptions.Cause
This, above-mentioned traditional edible vegetable oil evaluation mechanism is excessively easy, and illegal businessman's WeiZhao's Notes are relatively low, it is difficult to edible plant
Object oil quality is objectively evaluated.
Summary of the invention
Present invention aim to address above-mentioned the deficiencies in the prior art, provide a kind of edible plant based on metalloporphyrin probe
Object oil quality detection method.
The present invention is achieved by the following technical solutions:
A kind of edible vegetable oil quality detecting method based on metalloporphyrin probe, includes the following steps:
(1)Preparing metal porphyrin fluorescence probe solution in organic reagent is added in metalloporphyrin;
(2)Edible vegetable oil and metalloporphyrin probe are mixed in a certain proportion;
(3)According to the food plant oil quality intelligence based on metalloporphyrin probe, quickly detection model detects edible vegetable oil to be measured
Quality.
Preferably, step(1)The metalloporphyrin is tetraphenyl zinc protoporphyrin(ZnTPP)Or tetraphenyl silver porphyrin.
Preferably, step(1)The organic reagent is chloroform, n-hexane or methanol.
Preferably, step(2)The ratio of the edible vegetable oil and metalloporphyrin probe is 1 ~ 9:1~9.
Preferably, step(3)The quick detection model of food plant oil quality intelligence based on metalloporphyrin probe
Foundation includes the following steps:
(31)Select sample:A series of different edible vegetable oil sample of states of oxidation, every kind of place are obtained by a kind processing mode
Reason mode aoxidizes b gradient as gradient using the time respectively, and c sample of each gradient then amounts to a*b*c sample, each sample
It is configured with probe with certain proportion;Wherein, a, b, c are natural number;
(32)It obtains modeling and outputs and inputs data:Three-dimensional fluorescence spectrum detection parameters are set, three-dimensional fluorescence spectrum data are acquired
As mathematical model input value;The edible vegetable oil physical and chemical index of the different states of oxidation is obtained as mathematical modulo according to national standard
Type output valve;
(33)Establish Nonlinear Intelligent detection model:Using three-dimensional fluorescence spectrum detection data as input value, in national standard
Physical and chemical index as output valve, nonlinear mathematical model is trained, establish the food plant based on metalloporphyrin probe
The intelligent quick detection model of oil quality.
Preferably, step(32)The three-dimensional fluorescence spectrum detection parameters are:Excitation wavelength is 200 ~ 900nm, between wavelength
It is divided into 10nm, scanning speed 6000nm/min, exciting slit and transmite slit are 5nm.
Preferably, step(32)The physical and chemical index includes acid value, peroxide and polar component.
Preferably, step(33)The nonlinear mathematical model includes neural network, support vector machine, offset minimum binary
Method.
The beneficial effects of the present invention are:
Fluorescence spectrum probe technology is a kind of relatively new type Fast Detection Technique to grow up in recent years, in food quality
There are important application potentiality in terms of quality safety.Metalloporphyrin etc. is representative Fluorescence spectrum probe and edible vegetable oil one
Class or a few class metabolites carry out targeting combination, and generate a series of fluorescence spectrum variation.Observe by the naked eye fluorescence spectrum
Spectrogram variation intuitively can carry out qualitative evaluation to food plant oil quality, can establish edible plant by mathematical modeling mode
The oily qualitative and quantitative detection model of object.The detection of this method and traditional edible vegetable oil compare can have it is many excellent
Gesture can overcome WeiZhao's Notes caused by one or several chemical index lower or detect the defects of speed is slower.The present invention
One kind of offer is based on metalloporphyrin class fluorescence probe, and the intelligence of edible vegetable oil kind and quickly detection may be implemented.The hair
It is bright to China's edible vegetable oil processing enterprise core competitiveness is improved, improving consumer confidence etc. has important society's meaning
Justice and economic value.
Detailed description of the invention
Fig. 1 is typical case's ZnTPP fluorescent probe molecule structure chart;
Fig. 2 is typical case ZnTPP Fluorescence spectrum probe three-dimensional fluorescence spectrum figure;
Fig. 3 is the typical edible vegetable oil three-dimensional fluorescence spectrum figure based on ZnTPP probe;
The mathematics training model that Fig. 4 is established based on support vector machines(Circle is model prediction as a result, triangle is actually detected knot
Fruit);
The mathematics test model that Fig. 5 is established based on support vector machines(Circle is model prediction as a result, triangle is actually detected knot
Fruit).
Specific embodiment
In order to be best understood from the present invention, below with reference to examples and drawings, the invention will be further described, implements below
Example is only that the present invention will be described rather than is limited to it.
A kind of edible vegetable oil quality detecting method based on metalloporphyrin probe, includes the following steps:
Step 1, the configuration of metalloporphyrin fluorescence probe:Select the metalloporphyrins such as tetraphenyl zinc protoporphyrin, tetraphenyl silver porphyrin as glimmering
Light probe selects the organic reagents such as chloroform, n-hexane and methanol as solvent, is configured to the metalloporphyrin probe of 0.01mol/L.
If Fig. 1 and 2 is respectively typical case's ZnTPP fluorescent probe molecule structure chart and typical case's ZnTPP Fluorescence spectrum probe three-dimensional fluorescence spectrum
Figure.
Step 2 determines oil sample and probe ratio:It is 9 according to oil sample and probe ratio:1 ,8:2 ,7:3, 6:4 ,5:5
,4:6 ,3:7, 2:8 ,1:9 are configured, and are scanned three-dimensional fluorescence spectrum figure and are compared the three-dimensional fluorescence spectrum under different proportion
Feature peak type and Strength Changes, it is final to determine oil sample and probe optimal proportion.If Fig. 3 is typical edible based on ZnTPP probe
Vegetable oil three-dimensional fluorescence spectrum figure.
Step 3 selects representative edible vegetable oil sample:It is obtained by high temperature, baking oven and room temperature processing mode a series of
The edible vegetable oils samples such as the different peanut oil of the state of oxidation, rapeseed oil and soybean oil, each mode of oxidizing is using the time as gradient
5 gradients are aoxidized respectively, and 20 samples of each gradient gradient amount to 300 samples, and each oxidation sample and probe are centainly to compare
Example is configured, for establishing the edible vegetable oil intelligent measurement model based on fluorescence probe.
Step 4 obtains modeling and outputs and inputs data:Three-dimensional fluorescence spectrum detection parameters are set, wherein excitation wavelength is
200-900nm, wavelength interval 10nm, scanning speed 6000nm/min, exciting slit and transmite slit are 5nm, acquisition
Three-dimensional fluorescence spectrum data are as mathematical model input value;Pass through acid value, peroxide and the polar component etc. in national standard
Edible vegetable oil quality evaluation standard, the edible vegetable oil progress physical and chemical index for obtaining the different states of oxidation are defeated as mathematical modeling
It is worth out.
Step 5 establishes Nonlinear Intelligent detection model:Using three-dimensional fluorescence spectrum detection data as input value, with country
The physical and chemical indexes such as acid value, peroxide and polar component in standard are as output valve.To neural network, support vector machine, partially
The nonlinear mathematical models such as least square are trained, and it is intelligently quick to establish the food plant oil quality based on metalloporphyrin probe
Detection model.Following introductions are the edible vegetable oil intelligent measurement model foundation mistakes on MATLAB platform based on supporting vector
Journey, the modeling process such as other neural network methods, offset minimum binary are similar to following modeling process, so this patent is not only
It is limited to the Mathematical Modeling Methods based on support vector machines.
Using MATLAB software as computing platform, by three-dimensional fluorescence spectrum numerical value and acid value index with 2:1 ratio cut partition is instruction
Practice collection and test set, train_x, test_x and train_y and test_y is respectively labeled as, by inputting y in command windowmin
=0, ymax=1, normalized parameter is set.Using(1)Formula sentence carries out fluorescence data and physical and chemical index data
Normalization pretreatment.Train_scale in sentence is the training set after normalization, and test_scale is the test after normalization
Collection, ps is normalized mapping.
[train_scale,test_scale,ps]=scaleForSVM(train_x,test_x,ymin,ymax) (1)
With(2)Formula sentence obtains the 90% principal component dimensionality reduction data for explaining degree, train_pca and test_pca in sentence
The respectively pretreated training set of dimensionality reduction and test set.
[train_pca,test_pca] = pcaForSVM(train_scale,test_scale,90) (2)
Pass through(3)Formula sentence optimizes support vector machines parameter, obtains under bestCVaccuracy, bestc and bestg
Best accuracy rate, optimal parameter c and optimal parameter g under CV meaning.Train_y in above-mentioned formula is acid corresponding to training set
Valence physical and chemical index value, train are training set, and cmin and cmax are the variation range of penalty parameter c, gmin and gmax and kernel function
The variation range of g, V are the parameter for carrying out cross-validation process, and cstep and gstep are the step-length during c and g parameter optimization,
Accstep is the display step number interval of the last selection result of parameter.
[bestacc,bestc,bestg]=SVMcgForClass(train_y,train,cmin,cmax,gmin,
gmax,v,cstep,gstep,accstep) (3)
Finally by sentence(4)Food plant oil quality intelligent measurement model based on support vector machines.
model = svmtrain(train_x_labels,train_scale,'-c 2 -g 0.1') (4)
Established model result can be analyzed by the difference between legitimate reading and prediction result, and Fig. 4 and Fig. 5 are right respectively
Answer training set interpretation of result and forecast set interpretation of result.Circle in figure meets for predicted value, and triangle meets for true value, leads to
It crosses Fig. 4 and can be seen that true value is consistent substantially with predicted value with Fig. 5, so that demonstrating established model can be used in unknown sample
This food plant oil quality intelligent measurement.
The present invention, which uses metalloporphyrin fluorescence probe to carry out intelligent measurement for food plant oil quality, has certain lead to
With property, but since fluorescence probe and edible vegetable oil type are more, the present invention has only lifted metalloporphyrin probe and peanut
Case study on implementation of the oil as the invention, the other types of food plant oil quality intelligent detecting method based on fluorescence probe can be with
It is carried out referring to the implementation case, specific to specific food plant sample, selects a suitable fluorescence probe, establish new
Edible vegetable oil Quality Detection model can carry out intelligent measurement to food plant oil quality using similar technological means.
Embodiment described above is only that preferred embodiments of the present invention will be described, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made, should fall within the scope of protection determined by the claims of the present invention.
Claims (8)
1. a kind of edible vegetable oil quality detecting method based on metalloporphyrin probe, which is characterized in that include the following steps:
(1)Preparing metal porphyrin fluorescence probe solution in organic reagent is added in metalloporphyrin;
(2)Edible vegetable oil and metalloporphyrin probe are mixed in a certain proportion;
(3)According to the food plant oil quality intelligence based on metalloporphyrin probe, quickly detection model detects edible vegetable oil to be measured
Quality.
2. a kind of edible vegetable oil quality detecting method based on metalloporphyrin probe according to claim 1, feature
It is:Step(1)The metalloporphyrin is tetraphenyl zinc protoporphyrin or tetraphenyl silver porphyrin.
3. a kind of edible vegetable oil quality detecting method based on metalloporphyrin probe according to claim 1, feature
It is:Step(1)The organic reagent is chloroform, n-hexane or methanol.
4. a kind of edible vegetable oil quality detecting method based on metalloporphyrin probe according to claim 1, feature
It is:Step(2)The ratio of the edible vegetable oil and metalloporphyrin probe is 1 ~ 9:1~9.
5. a kind of edible vegetable oil quality detecting method based on metalloporphyrin probe according to claim 1, feature
It is, step(3)The foundation of the quick detection model of the food plant oil quality intelligence based on metalloporphyrin probe include with
Lower step:
(31)Select sample:A series of different edible vegetable oil sample of states of oxidation, every kind of place are obtained by a kind processing mode
Reason mode aoxidizes b gradient as gradient using the time respectively, and c sample of each gradient then amounts to a*b*c sample, each sample
It is configured with probe with certain proportion;Wherein, a, b, c are natural number;
(32)It obtains modeling and outputs and inputs data:Three-dimensional fluorescence spectrum detection parameters are set, three-dimensional fluorescence spectrum data are acquired
As mathematical model input value;The edible vegetable oil physical and chemical index of the different states of oxidation is obtained as mathematical modulo according to national standard
Type output valve;
(33)Establish Nonlinear Intelligent detection model:Using three-dimensional fluorescence spectrum detection data as input value, in national standard
Physical and chemical index as output valve, nonlinear mathematical model is trained, establish the food plant based on metalloporphyrin probe
The intelligent quick detection model of oil quality.
6. a kind of edible vegetable oil quality detecting method based on metalloporphyrin probe according to claim 5, feature
It is, step(32)The three-dimensional fluorescence spectrum detection parameters are:Excitation wavelength is 200 ~ 900nm, and wavelength interval 10nm is swept
Retouching speed is 6000nm/min, and exciting slit and transmite slit are 5nm.
7. a kind of edible vegetable oil quality detecting method based on metalloporphyrin probe according to claim 5, feature
It is:Step(32)The physical and chemical index includes acid value, peroxide and polar component.
8. a kind of edible vegetable oil quality detecting method based on metalloporphyrin probe according to claim 5, feature
It is:Step(33)The nonlinear mathematical model includes neural network, support vector machine, Partial Least Squares.
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