CN108507967A - A method of α-and Gamma-Tocopherol content in more peanut seeds of detection - Google Patents

A method of α-and Gamma-Tocopherol content in more peanut seeds of detection Download PDF

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Publication number
CN108507967A
CN108507967A CN201810313039.7A CN201810313039A CN108507967A CN 108507967 A CN108507967 A CN 108507967A CN 201810313039 A CN201810313039 A CN 201810313039A CN 108507967 A CN108507967 A CN 108507967A
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China
Prior art keywords
tocopherol content
gamma
peanut
peanut seed
detection
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CN201810313039.7A
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Chinese (zh)
Inventor
王传堂
唐月异
胡东青
王秀贞
刘婷
吴琪
孙全喜
王志伟
张建成
杜祖波
李秋
宋国生
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Shandong Peanut Research Institute
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Shandong Peanut Research Institute
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Priority to CN201810313039.7A priority Critical patent/CN108507967A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light

Abstract

The invention discloses the methods of α and gama tocopherol content in a kind of detection peanut seed, belong to peanut processing product quality quick test technique field.It is to carry out infrared diaphanoscopy to peanut seed to be measured that the present invention, which detects the method for α and gama tocopherol content in peanut seed, spectrum after scanning is imported in the peanut seed α of structure and the near-infrared spectroscopy of gama tocopherol content, peanut seed α and gama tocopherol content are obtained through analysis.It is provided by the invention detection peanut seed α and gama tocopherol content method, can be quick, accurate, lossless detection peanut in α and gama tocopherol content, and it is easy to operate, accuracy is high.And the near-infrared spectroscopy R of the detection α and gama tocopherol content of structure2Higher, RMSECV is smaller, prediction effect preferably, it can be achieved that in peanut seed α and gama tocopherol content accurate quantitative analysis.

Description

A method of α-and Gamma-Tocopherol content in more peanut seeds of detection
Technical field
The invention belongs to peanut processing product quality quick test technique fields, and in particular in a kind of detection peanut seed α-and The method of Gamma-Tocopherol content.
Background technology
Peanut is the important sources of main oil crops and quality plant oil and high digestibility protein in the world. Vitamin E (Vitamin E) is a kind of liposoluble vitamin, have strengthen immunity, anti-aging, reduce angiocardiopathy and The effect of cancer morbidity.α-and Gamma-Tocopherol are the important component of vitamin E, the physiological activity of alpha-tocopherol in human body Highest, but in vitro especially under the high temperature conditions, the oxidation resistance of Gamma-Tocopherol is higher than alpha-tocopherol.
Traditional assay method of vitamin E includes fluorescent spectrometry, high performance liquid chromatography, blocks method, gas chromatography Deng, of high cost, time-consuming, have certain destructiveness, this hinders the development of peanut homovitamin E breedings to a certain extent, and Near infrared technology has many advantages, such as at low cost, lossless, quick.Near infrared technology has been applied to the quality-improving of multiple crops, The near-infrared model of energy Accurate Prediction oleic acid, fat, protein content is successfully established on peanut, but similar peanut always ties up life Plain E contents or various content of isomer near-infrared models have not been reported so far.
Invention content
Purpose of the present invention is to utilize near infrared spectrometer, accurate quantitative analysis is carried out to peanut seed α-and Gamma-Tocopherol content.
In order to achieve the above object, the technical scheme is that:
A method of detection peanut seed α-and Gamma-Tocopherol content carry out infrared diaphanoscopy to peanut seed to be measured, Spectrum after scanning is imported in the peanut seed α-of structure and the near-infrared spectroscopy of Gamma-Tocopherol, is spent through analysis The sub- α-of non-hibernating eggs and Gamma-Tocopherol content.
On the basis of said program, the near-infrared spectroscopy of the peanut seed α-and Gamma-Tocopherol is by with lower section Method is built-up:
(1) peanut sample of different cultivars, solar drying are collected;
(2) near infrared ray is carried out to above-mentioned peanut sample, collects near infrared light spectrum information;
(3) α-and Gamma-Tocopherol content for detecting all peanut samples respectively, obtain the change of α-and Gamma-Tocopherol content Value;
(4) chemical score to α-and Gamma-Tocopherol content and (2) middle near infrared spectrum data acquired are fitted spectrum Processing uses cross-validation abnormal value elimination, by comparing the coefficient of determination (R of model repeatedly2) and standard deviation (RMSECV) model quality is weighed, best model is screened;
(5) accuracy of model is verified.
On the basis of said program, the near infrared spectrum scanning parameter is:Scanning Spectral range 4000~ 12000cm-1(centimetre wave number), scanning times 64 times, resolution ratio 8cm-1
On the basis of said program, the peanut sample is:
On the basis of said program, the chemical score of the peanut sample alpha-tocopherol content is with predicted value:
The chemical score of the peanut sample Gamma-Tocopherol content is with predicted value:
On the basis of said program,
The optimal spectrum preprocess method of the near-infrared spectroscopy of the alpha-tocopherol content is " first derivative+vector Normalization ".Spectral range is 7506~4242.8cm-1, dimension 10, the R of model2For 90.05, RMSECV 0.203;
The optimal spectrum preprocess method of the near-infrared spectroscopy of the Gamma-Tocopherol content is " first derivative+vector Normalization ", Spectral range are 7506~4242.8cm-1, dimension 8, the R of model2For 83.27, RMSECV 0.458.
On the basis of said program, the near infrared spectrum scanning, each sample 30-50, multiple scanning 3 times, and And peanut is poured out when scanning for the second time and for the third time and is reloaded in specimen cup, to obtain multiple near-infrareds of same sample Spectrum.
The method of detection peanut seed α-and Gamma-Tocopherol content provided by the invention, can be quick, accurate, lossless Detect peanut in α-and Gamma-Tocopherol content, and it is easy to operate, accuracy is high.
The near-infrared spectroscopy R for the detection α-and Gamma-Tocopherol content that the present invention is built2Higher, RMSECV is smaller, in advance Survey effect preferably, it can be achieved that in peanut seed α-and Gamma-Tocopherol accurate quantitative analysis.
Near-infrared spectroscopy data used when depending on establishing model to the prediction effect of sample.Moreover, establishing close Infrared spectrum model is not that the sample number that uses is The more the better, introduced dry in model with the increase of modeling sample number Disturbing factor and anomalous differences will increase, and excessive interference information can cover useful information, reduce model performance.The present invention selects Peanut sample size it is suitable, the compatible degree between different cultivars is preferable, constructed model prediction peanut seed α-and γ-fertility Phenol content error is small, and accuracy is high.
Description of the drawings
The infrared diaphanoscopy spectrogram of Fig. 1 peanut samples, wherein abscissa represent centimetre wave number (cm-1), ordinate represents Absorbance;
The near-infrared predicted value of Fig. 2 alpha-tocopherol contents and chemical score scatter plot, wherein abscissa represent actual value, indulge and sit Mark represents predicted value;
The near-infrared predicted value of Fig. 3 Gamma-Tocopherol contents and chemical score scatter plot, wherein abscissa represent actual value, indulge Coordinate represents predicted value.
Specific implementation mode
Term as used in the present invention generally has those of ordinary skill in the art usual unless otherwise specified The meaning of understanding.
With reference to specific embodiment, and with reference to the data further detailed description present invention.Following embodiment only be It illustrates the present invention, rather than limits the scope of the invention in any way.
Embodiment
Illustrate by taking the MATRIX-I type near infrared spectrometers of German Brooker company production as an example below, but the patent scope of application Also include the similar products of other manufacturers.
1. materials and methods
1.1 material
The test material used in α-and the near-infrared model of Gamma-Tocopherol content is built, is from peanut product both domestic and external Kind (being) amounts to 42 parts, as shown in table 1.
Table 1 builds peanut seed sample used in peanut α-and the near-infrared model of Gamma-Tocopherol content
1.2 method
1.2.1 spectra collection
The MATRIX-I type Fourier transforms that modeling spectroscopic data used is produced in German Brooker spectral instrument company It is acquired near infrared spectrometer.Scanning spectrum area ranging from 4000~12000cm-1, scanning times 64 times, resolution ratio 8cm-1.It opens Sample is detected after machine preheating 30min.Acquire the sample that peanut seed used in spectrum is natural daylight drying, every part of material about 30- 50, multiple scanning 3 times.The results are shown in Figure 1 for the near infrared spectrum scanning of peanut sample.
1.2.2 α-and Gamma-Tocopherol assay
1.2.2.1 alpha-tocopherol assay
Alpha-tocopherol content in 42 parts of Ecological Property of Peanut Seeds samples is measured using HPLC methods, sample chemical value relevant parameter is shown in Table 2.Alpha-tocopherol content mean value is 5.48mg/100g, and maximum, minimum value is respectively 7.38mg/100g, 4.12mg/100g.Show It is fine to model peanut sample alpha-tocopherol content luffing, can be used for near-infrared spectroscopy structure.
2 peanut seed alpha-tocopherol content chemical score pertinent statistical parameters of table
1.2.2.2 Gamma-Tocopherol assay
Gamma-Tocopherol content in 42 parts of Ecological Property of Peanut Seeds samples is measured using HPLC methods, sample chemical value relevant parameter is shown in Table 3.Gamma-Tocopherol content mean value is 4.85mg/100g, and maximum, minimum value is respectively 9.37mg/100g, 1.55mg/100g. Show that modeling peanut sample Gamma-Tocopherol content luffing is fine, can be used for near-infrared spectroscopy structure.
3 peanut seed Gamma-Tocopherol content chemical score pertinent statistical parameters of table
1.2.3 model construction and optimization
Spectral manipulation and model construction use 5.5 softwares of OPUS of German Brooker MATRIX-I type near infrared spectrometers, It is optimized with NIR options.Using cross-validation abnormal value elimination (outlier).Selection optimal spectrum pretreatment method, Optimized spectrum area, dimension, and make further verification.By comparing the coefficient of determination (R of model2) and standard deviation (RMSECV) measurement mould Type quality.
1.2.3.1 the chemical score and predicted value of peanut sample alpha-tocopherol content
The chemical score and predicted value of each peanut sample alpha-tocopherol content are as shown in table 4.
The chemical score of 4 peanut sample alpha-tocopherol content of table is with predicted value:
Optimized, the optimal spectrum preprocess method of peanut seed alpha-tocopherol content is " first derivative+vector normalizing Change ".Spectral range is 7506~4242.8cm-1, dimension 10, the R of model2It is 0.203 (Fig. 2) for 90.05, RMSECV.
1.2.3.2 the chemical score and predicted value of peanut sample Gamma-Tocopherol content
The chemical score and predicted value of each peanut sample Gamma-Tocopherol content are as shown in table 5.
The chemical score of 5 peanut sample Gamma-Tocopherol content of table is with predicted value:
Through Automatic Optimal, the optimal spectrum preprocess method of peanut seed Gamma-Tocopherol content is " first derivative+vector Normalization ".Spectral range is 7506~4242.8cm-1, dimension 8, the R of model2It is 0.458 (Fig. 3) for 83.27, RMSECV.
1.2.4 the verification of model
1.2.4.1 the near-infrared spectroscopy of alpha-tocopherol content is examined
6 parts of peanut sample external samples separately are taken, testing model prediction effect, the results are shown in Table 6.Alpha-tocopherol content is inclined Difference is -0.6~0.4mg/100g, and prediction deviation is relatively low.Paired data t tests, two groups of data are carried out to chemical score and predicted value Equal value difference is 0.0159, degree of freedom 5, and t values are 0.112<t0.05=2.571, two groups of data differences are not notable.
6 peanut seed sample alpha-tocopherol content chemical score of table is compared with predicted value
Serial number Chemical score Predicted value Bias
A3PI210555 6.10 6.38 0.28
A5PI331189 5.40 5.31 0.31
A7PI219824 5.81 5.72 -0.09
A19PI219823 4.93 5.33 0.40
A4PI298639 6.00 5.40 -0.60
A54PI262133 4.53 4.54 0.01
1.2.4.2 the near-infrared spectroscopy of Gamma-Tocopherol content is examined
6 parts of peanut sample external samples separately are taken, testing model prediction effect, the results are shown in Table 7.Gamma-Tocopherol content Deviation is -1.35~2.25mg/100g, and prediction deviation is relatively low.Paired data t tests are carried out to chemical score and predicted value, two groups Data mean value difference is -0.7061, degree of freedom 5, and t values are 1.272<t0.05=2.571, two groups of data differences are not notable.
7 peanut seed sample Gamma-Tocopherol content chemical score of table is compared with predicted value
Serial number Chemical score Predicted value Bias
A3PI210555 4.64 5.63 0.99
A9PI210555 2.9 3.8 0.9
A17PI263133 4.37 3.97 -0.4
A20PI331193 5.09 6.91 1.82
A34PI337308 5.6 4.25 -1.35
A19PI219823 4.8 7.05 2.25
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc. Imitate embodiment.But it is every without departing from technical solution of the present invention content, according to the technical essence of the invention to above example institute Any simple modification, equivalent variations and the remodeling made, still fall within the protection domain of technical solution of the present invention.

Claims (7)

1. a kind of method of detection peanut seed α-and Gamma-Tocopherol content, it is characterised in that:Peanut seed to be measured is carried out close Infrared scan imports the spectrum after scanning in the peanut seed α-of structure and the near-infrared spectroscopy of Gamma-Tocopherol content, Peanut seed α-and Gamma-Tocopherol content are obtained through analysis.
2. the method for detection peanut seed α-and Gamma-Tocopherol content according to claim 1, it is characterised in that:The flower The sub- α-of non-hibernating eggs and the near-infrared spectroscopy of Gamma-Tocopherol content are built-up by following methods:
(1) peanut sample of different cultivars, solar drying are collected;
(2) near infrared ray is carried out to above-mentioned peanut sample, collects near infrared light spectrum information;
(3) α-and Gamma-Tocopherol content for detecting all peanut samples respectively, obtain the chemical score of α-and Gamma-Tocopherol content;
(4) chemical score to α-and Gamma-Tocopherol content and (2) middle near infrared spectrum data acquired are fitted at spectrum Reason establishes model with Partial Least Squares optimization, uses cross-validation abnormal value elimination repeatedly, by comparing determining for model Determine coefficient (R2) and standard deviation (RMSECV) measurement model quality, screen best model;
(5) accuracy of model is verified.
3. the method for detection peanut seed α-and Gamma-Tocopherol content according to claim 1 or claim 2, it is characterised in that:
The near infrared spectrum scanning parameter is:Scan 4000~12000cm of Spectral range-1(centimetre wave number), scanning times 64 It is secondary, resolution ratio 8cm-1
4. the method for detection peanut seed α-and Gamma-Tocopherol content according to claim 3, it is characterised in that:
The peanut sample is:
5. the method for detection peanut seed α-and Gamma-Tocopherol content according to claim 4, it is characterised in that:
The chemical score of the peanut sample alpha-tocopherol content is with predicted value:
The chemical score of the peanut sample Gamma-Tocopherol content is with predicted value:
6. the method for detection peanut seed α-and Gamma-Tocopherol content according to claim 5, it is characterised in that:
The optimal spectrum preprocess method of the near-infrared spectroscopy of the alpha-tocopherol content is " first derivative+vector normalizing Change ".Spectral range is 7506~4242.8cm-1, dimension 10, the R of model2For 90.05, RMSECV 0.203;
The optimal spectrum preprocess method of the near-infrared spectroscopy of the Gamma-Tocopherol content is " first derivative+vector normalizing Change ", Spectral range is 7506~4242.8cm-1, dimension 8, the R of model2For 83.27, RMSECV 0.458.
7. according to the method for any one of the claim 1~6 detection peanut seed α-and Gamma-Tocopherol content, feature exists In:The near infrared spectrum scanning, each sample 30-50, multiple scanning 3 times, and second is wanted with when scanning for the third time Peanut is poured out and is reloaded in specimen cup, to obtain multiple near infrared spectrums of same sample.
CN201810313039.7A 2018-04-09 2018-04-09 A method of α-and Gamma-Tocopherol content in more peanut seeds of detection Pending CN108507967A (en)

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