CN105067561A - Method for measuring content of manganese element in cotton seed meal - Google Patents
Method for measuring content of manganese element in cotton seed meal Download PDFInfo
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- CN105067561A CN105067561A CN201510497322.6A CN201510497322A CN105067561A CN 105067561 A CN105067561 A CN 105067561A CN 201510497322 A CN201510497322 A CN 201510497322A CN 105067561 A CN105067561 A CN 105067561A
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Abstract
The invention discloses a method for measuring the content of a manganese element in cotton seed meal. Different types of cotton seed meal samples planted in different regions are prepared, spectra of the cotton seed meal samples are acquired by a near infrared reflectance spectrograph, a PLS model is constructed through full cross validation in the full spectrum range, and then the PLS model is analyzed with 12 preprocessing methods; a processing method corresponding to the prediction related coefficient R<2> maximum and the RMSE (root-mean-square error) minimum are taken as the optimal preprocessing method, and an NIRS (near infrared reflectance spectroscopy) correction model is established with the optimal preprocessing method; the to-be-measured cotton seed meal is detected with the NIRS correction model constructed in the previous steps, and the content of the manganese element is obtained. A spectrum chart of the cotton seed meal is acquired by the aid of the FOSS5000 near infrared reflectance spectrograph, the measurement accuracy is high, and the method is quick, convenient and efficient and has great significance in cultivation of new cotton varieties and promotion of processing and utilization of cotton by-products.
Description
Technical field
The present invention relates to a kind of content assaying method, specifically relate to the assay method of manganese element content in a kind of cotton seed meal.
Background technology
Near infrared spectrum (NearInfraredReflectanceSpectroscopy, NIRS) analytical technology is as OH, CH, NH, SH etc. have distinctive absorption peak near infrared region performance by the hydric group in analyte, utilize the method for Chemical Measurement, the analyzing and processing that one is class is carried out to the sample spectra information of scanning, finally completes the quantitative test of this sample related component.Near infrared spectrometer can gather nearly all organic characteristic absorption signal, and absorption peak is not had for metallic element, but metallic element is not single existence in plant, often all can combine or chelating with the organism such as a lot of organized enzymes, be enriched in plant tissue, thus indirectly gathered by near infrared spectrum.Current technique has been widely used in agricultural, biology, food, medicine, field of petrochemical industry, due to it have do not destroy sample, quick, accurate, environment friendly and pollution-free etc. a little, this technology is a kind of new technology extremely rising in modern agriculture and bio-science.There is a lot of bibliographical information about Quantitative Analysis of Chemical Compositions such as moisture, albumen, fiber, fat, amino acid in the crops such as paddy rice, wheat, cotton, vegetables and fruits both at home and abroad, and little for using the relevant report of near-infrared spectrum technique mensuration metal element content.
Manganese element is the epochmaking trace element of cotton crop, it participates in the cotton photosynthetic photodissociation of water in the oxidation-reduction process of electron transport system and PSII system on directly, participate in various enzymatic reaction, promote nitrogen metabolism, appropriate manganese element is conducive to seed germination, improve seed vitality, and too high levels is unfavorable for the germination and growth of seed.So its importance exceedes other trace element.Cotton secondary product cottonseed is again a kind of important animal feed and edible oil resource, and the manganese element of excess intake has considerable influence to human body and animal.In detection cottonseed, manganese element content has larger meaning for the comprehensive utilization of cotton seeds production and cotton secondary product.
And to measure in cottonseed manganese element at present based on the chemical method of routine, as flame atomic absorption method, inductivity coupled plasma mass spectrometry assay method etc., these classic method sensitivity and degree of accuracy high, but have that preparation of samples is loaded down with trivial details, analysis time is long, testing cost is high, consume nitric acid, sulfuric acid etc. in a large number there is by force the dangerous very high reagent of corrosivity.
Summary of the invention
In cotton seed meal, Fe content is the index affecting cottonseed utilization, conveniently chemical analysis mensuration manganese element content is not only time-consuming but also require great effort, and need to consume the very high chemical reagent of a large amount of poisonous danger, somewhat expensive and contaminated environment, add difficulty often to cotton seed meal evaluation of nutrition, the object of the invention is the deficiency for existing in existing chemical analysis technology, provide the assay method of manganese element content in a kind of cotton seed meal, near infrared spectrum and Chemical Measurement multivariate calibration methods is adopted to carry out Fast Measurement to manganese element content in cottonseed, efficiently solve the problems referred to above, for the detection of manganese element in cottonseed provides fast a kind of, convenient, efficient analytical approach, have conveniently, fast, advantage accurately.
The technical solution used in the present invention is:
1) be prepared in different types of cotton seed meal sample of different regions plantation: cottonseed is carried out pre-service, and cottonseed (cotton seeds) lint post-drying, clays into power cottonseed with sample grinding machine, cross 60 mesh sieves, obtain cotton seed meal sample;
2) near infrared spectrometer is utilized to gather the spectral information of cotton seed meal sample;
3) in full spectral range, adopt full cross validation to build PLS model, adopt 12 kinds of preprocess methods and do not carry out any pre-service and PLS model is analyzed, and compare;
4) with the prediction related coefficient R of PLS model
2the minimum corresponding disposal route of maximum and root-mean-square error RMSE, as optimum preprocess method, sets up the near infrared spectrum calibration model of manganese element by optimum preprocess method;
5) cottonseed to be measured being adopted step 1) described same procedure prepares cotton seed meal to be measured, and detect cotton seed meal to be measured with the near infrared spectrum calibration model constructed by above-mentioned steps, obtain its manganese element content.
Described step 4) be specially: obtain spectral value by optimum preprocess method process after cotton seed meal to be measured is obtained spectrum by near infrared spectrometer, then import the manganese element content obtaining cotton seed meal to be measured near infrared spectrum calibration model.
12 kinds of described preprocess methods be respectively the combined method SavitzkyGolay of standard normal variable method, multiplicative scatter correction method, homogenization method, single order guiding method, second order guiding method, transform-based line method, SavitzkyGolay smoothing method, spectrum transform method and these methods level and smooth+single order guiding method, standard normal variable+single order guiding method, standard normal variable+SavitzkyGolay smoothing method and multiplicative scatter correction+single order guiding method
To be Monte Carlo select without information variable described near infrared spectrum calibration model two takes advantage of supporting vector machine model (MC-UVE-LS-SVM model) partially, in full spectroscopic data, and the spectral variables of not all exists significant correlativity with objective trait, wherein may exist a large amount of without information variable.Therefore, the present invention adopts Monte Carlo to carry out the selection of variable without information variable null method etc., and compared with full spectrum PLS model, redundant variables eliminated by this model, simplifies calibration model, improves the arithmetic speed of model.
Preferred described step 2) utilize the spectrum concrete steps of near infrared spectrometer collection cotton seed meal sample as follows: the collection wavelength coverage of near infrared spectrometer is 800-2500nm, adjacent band interval 2nm, totally 700 wavelength points are set, every part of cotton seed meal gathers spectrum 4 times, each applied sample amount is about 3.5g, sample cell is cylindrical, and columniform diameter is 35mm, and cylindrical height is 18mm.
Preferred near infrared spectrometer model can adopt FOSS5000, and the analysis software of spectroscopic data can adopt UnscramblerV9.7 and matlabR2011a.
Compared with prior art, the invention has the beneficial effects as follows:
1, the present invention utilizes FOSS5000 near infrared spectrometer to acquire the spectrogram of cotton seed meal, have studied modeling and the application process of manganese element in cotton seed meal, has easily and fast, advantage accurately.
2, to measure accuracy very high in the present invention, is a kind of quick, convenient, efficient assay method, for cultivation new cotton variety, promotes that the processing and utilization of cotton secondary product is significant.
Accompanying drawing explanation
Fig. 1 is manganese element content distribution figure in the inventive method.
Fig. 2 is cotton seed meal near infrared light spectrogram in the inventive method.
Fig. 3 is near infrared light spectrogram after the optimum pre-service of cotton seed meal in the inventive method.
Fig. 4 is best latent variable selection figure in the inventive method.
Fig. 5 be in the inventive method Monte Carlo without the selection figure of optimal threshold in information variable selection course.
Fig. 6 is the graph of a relation of chemical measurements and near infrared spectrum predicted value in the inventive method.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Specific embodiments of the invention are as follows:
(1) cottonseed is carried out pre-service: cotton seeds lint post-drying, with sample grinding machine, seed is clayed into power, cross 60 mesh sieves, obtain cotton seed meal sample; The cottonseed getting national planted in different ecological areas and different cultivars is sample, obtains described dry powder sample by pulverizing with sample grinding machine after above-mentioned steps freeze drying.
Cottonseed sample gathers from area, 11, the whole nation, comprises the different ecological growing areas such as Zhejiang Hangzhou, Wuhu, Yancheng, Jiangsu Province, Lixian County, Hunan, multiple cotton variety, totally 288 cottonseed samples.
(2) sample spectra collection
Loaded by cotton seed meal in sample cell, each scan sample four times, sample light spectrogram as shown in Figure 2.
Near-infrared spectrum analysis parameter: near infrared spectrometer model is FOSS5000, collection wavelength coverage is 800-2500nm, adjacent band interval 2nm, totally 700 wavelength points.Every part of cotton seed meal gathers spectrum 4 times, and each applied sample amount is about 3.5g, and sample cell is cylindrical (diameter 35mm, height 18mm), and data analysis software is UnscramblerV9.7 and matlabR2011a.
(3) calibration set and checking collect choosing of sample
Near infrared spectrometer is utilized to gather the spectrum of above-mentioned sample, for near infrared modeling, calibration set and checking collection sample must can both represent the Data distribution8 situation of original sample, and the sample content scope of calibration set will comprise checking collection sample content scope, use Kennard-Stone algorithm that cotton seed meal sample is divided into calibration set sample and checking collection sample according to the ratio of 3:1, be about to originally carry out diversity to 288 increments, obtain 216 parts, calibration set sample, checking collection 72 parts, sample, set up described near-infrared model, modeling collection and checking collection sample distribution are as table 1.
Table 1 calibration set and checking collect manganese element distribution in sample
(4) Establishment and optimization of model
For the calibration set sample of 216 parts, in full spectral range, adopt full cross validation to set up PLS model, investigate 12 kinds respectively without the impact of preprocessing procedures on PLS model, 12 kinds of preprocess methods are respectively standard normal variable method, multiplicative scatter correction method, homogenization method, single order guiding method, second order guiding method, transform-based line method, SavitzkyGolay smoothing method, spectrum transform method, and the combined method SavitzkyGolay of these methods level and smooth+single order guiding method, standard normal variable+single order guiding method, standard normal variable+SavitzkyGolay smoothing method and multiplicative scatter correction+single order guiding method.
Then all with R
2with RMSE value as reference index, R
2maximum and RMSE is minimum chooses the preprocess method of optimum preprocess method as modeling, in the present invention, optimum preprocess method is the method that standard normal conversion (SNV) and single order lead combination, and Fig. 3 is the spectrogram of original spectrum after optimum preprocess method process.And then the calibration model of MC-UVE-LS-SVM model as manganese element of manganese element is set up by optimum preprocess method.The model reference metrics evaluation of 12 kinds of preprocess method foundation is in table 2.
The PLS model parameter evaluation index that table 212 kind of preprocess method is set up
(5) checking of model
Pretreated spectroscopic data is imported in matlab software, first best latent variable number is calculated according to press value, see Fig. 4, then utilize the method establishment least square method supporting vector machine model (MC-UVE-LS-SVM) that Monte Carlo is selected without information variable.Wherein Fig. 5 is the determination of Monte Carlo without optimal threshold in information variable system of selection processing procedure, and optimal threshold is 3.
The present invention, by repeatedly specifically implementing, specifically preferably can set up MC-UVE-LS-SVM model, this model R
2the highest with RPD value, model evaluation parameter is in table 3.
The performance index of the different calibration model of table 3 cotton seed meal manganese element content
In table: RMSECV represents cross validation root-mean-square error (numerical value is the smaller the better); RMSEP represents predicted root mean square error (numerical value is the smaller the better); R
2represent prediction related coefficient (R
2>0.9 can substitute traditional assay method completely); RPD represents remaining predicted deviation (robustness of RPD>2.5 model is fine).
(6) prepare cotton seed meal to be measured, detect cotton seed meal to be measured with the near infrared spectrum calibration model constructed by above-mentioned steps, obtain its manganese element content.
In order to accuracy of measurement of the present invention is described, embodiment uses the above-mentioned Powder samples of ICP-MS instrumental analysis, to contrast, specific as follows: manganese element condition determination: accurate weighing 0.4000g cotton seed meal, add the pure nitric acid of 6mL and 0.2mL superoxol, in superoxol, the volumetric concentration of hydrogen peroxide is 10%, 120 DEG C and clears up 30min in advance, then sample is put into microwave dissolver and clear up 1.5 hours, sample acid discharge was dissolved to 30mL after 1 hour.ICP-MS instrument type is: ICP-MS (ElanDCR-ePekinElmerUSA).Its chemical measurements and the graph of a relation with near infrared ray value of the present invention are as shown in Figure 6.
In 288 parts of cotton seed meals that the present embodiment mainly provides, the ICP-MS analysis result of heavy metal element manganese is shown in Fig. 1; Because cotton product come from different regions, different cultivars, the content of element has larger difference, the results are shown in Table 4, provides condition for setting up spectral model.
Manganese element content difference in table 4 cotton seed meal
As can be seen here, the inventive method, wherein sample material manganese element content is across width large (10.2519-48.9918mg/g), there is good representativeness, utilizing near infrared spectrum modeling, by comparing different pretreatments method, determining that optimum preprocess method is that SNV and single order lead the method combined, adopt optimum preprocessing procedures to set up different manganese element calibration models, wherein MC-UVE-LS-SVM model has the highest R
2with RPD value, RMSECV and RMSEP value is all minimum, can measure manganese element content in cotton seed meal accurately.The present invention utilizes near infrared spectrometer, the spectrogram of scanning cotton seed meal, according to optimum preprocess method process spectral information, and then the content of manganese element in Fast Measurement cotton seed meal, there is outstanding technique effect that is quick, convenient, accurate, environmental protection, for cultivation new cotton variety, promote that the processing and utilization of cotton secondary product is significant and be worth.
Claims (5)
1. the assay method of manganese element content in cotton seed meal, is characterized in that comprising the steps:
1) different types of cotton seed meal sample of different regions plantation is prepared in:
Cottonseed is carried out pre-service, and cottonseed (cotton seeds) lint post-drying, clays into power cottonseed with sample grinding machine, crosses 60 mesh sieves, obtains cotton seed meal sample;
2) near infrared spectrometer is utilized to gather the spectrum of cotton seed meal sample;
3) in full spectral range, adopt full cross validation to build PLS model, adopt 12 kinds of preprocess methods and do not carry out any pre-service and PLS model is analyzed respectively, and compare;
4) with the prediction related coefficient R of PLS model
2the minimum corresponding disposal route of maximum and root-mean-square error RMSE, as optimum preprocess method, sets up the near infrared spectrum calibration model of manganese by optimum preprocess method;
5) cottonseed to be measured being adopted step 1) described same procedure prepares cotton seed meal to be measured, and detect cotton seed meal to be measured with the near infrared spectrum calibration model constructed by above-mentioned steps, obtain its manganese element content.
2. the assay method of manganese element content in a kind of cotton seed meal according to claim 1, it is characterized in that: described step 4) be specially: obtain spectral value by optimum preprocess method process after cotton seed meal to be measured is obtained spectrum by near infrared spectrometer, then import the manganese element content obtaining cotton seed meal to be measured near infrared spectrum calibration model.
3. the assay method of manganese element content in a kind of cotton seed meal according to claim 1, it is characterized in that: 12 kinds of described preprocess methods are respectively standard normal variable method, multiplicative scatter correction method, homogenization method, single order guiding method, second order guiding method, transform-based line method, SavitzkyGolay smoothing method, spectrum transform method, and the combined method SavitzkyGolay of these methods level and smooth+single order guiding method, standard normal variable+single order guiding method, standard normal variable+SavitzkyGolay smoothing method and multiplicative scatter correction+single order guiding method.
4. the assay method of manganese element content in a kind of cotton seed meal according to claim 1, is characterized in that: described near infrared spectrum calibration model be Monte Carlo select without information variable two take advantage of supporting vector machine model partially.
5. the assay method of manganese element content in a kind of cotton seed meal according to claim 1, it is characterized in that: described step 2) utilize the spectrum concrete steps of near infrared spectrometer collection cotton seed meal sample as follows: the collection wavelength coverage of near infrared spectrometer is 800-2500nm, adjacent band interval 2nm, totally 700 wavelength points are set, every part of cotton seed meal gathers spectrum 4 times, each applied sample amount is about 3.5g, and sample cell is cylindrical.
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| CN105588818A (en) * | 2016-01-28 | 2016-05-18 | 浙江大学 | Near-infrared determination method for content of gossypol in cottonseed powder |
| CN114460116A (en) * | 2021-12-30 | 2022-05-10 | 电子科技大学 | Element content quantitative analysis method for regression and sensitivity analysis of support vector machine |
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Application publication date: 20151118 |