CN101957316A - Method for authenticating Xiangshui rice by near-infrared spectroscopy - Google Patents
Method for authenticating Xiangshui rice by near-infrared spectroscopy Download PDFInfo
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- CN101957316A CN101957316A CN 201010033381 CN201010033381A CN101957316A CN 101957316 A CN101957316 A CN 101957316A CN 201010033381 CN201010033381 CN 201010033381 CN 201010033381 A CN201010033381 A CN 201010033381A CN 101957316 A CN101957316 A CN 101957316A
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Abstract
The invention belongs to near infrared spectrum analysis and in particular discloses a method for authenticating Xiangshui rice by near-infrared spectroscopy. The method comprises the following steps of: building a clustering discrimination and eligibility discrimination model by respectively selecting a proper spectra preprocessing way, smooth points, a spectral interval, factor number and the like; and scanning a near infrared spectrogram of an unknown sample under the same condition, pre-processing the near infrared spectrogram, and authenticating the unknown sample according to the built clustering discrimination and eligibility discrimination model by selecting the same smooth points, spectral interval, factor number and the like. The method solves the problem of unavailable protection and authentication for the Xiangshui rice, the geographical indication product in the prior art, and has the advantages of well authenticating the Xiangshui rice, along with high identification rate.
Description
Affiliated technical field
The invention belongs to the near infrared spectrum check and analysis, be meant a kind of method of differentiating Xiangshui County's rice with near-infrared spectrum technique especially.
Background technology
The geographical sign product is meant and originates from specific region that the quality that is had, reputation or other characteristic essence depend on the natural cause and the humane factor in this place of production, through the product of audit approval with the geographic name name.From first part of geographical sign product protection approval of Chinese government's issue in 2000 bulletin, ratified hundreds of geographical sign protection product, relate to more than 20 kind.These products originate from specific region, perhaps via special explained hereafter, and experience special quality control and have special quality and characteristic, thereby have higher economic worth.Wherein by the rice of geographical sign protection, the shining sun rice in Panjin rice, Jiangsu in Xiangshui County's rice, the Liaoning in area, Heilungkiang and East Sea rice, the Yutai rice in Shandong, the plum river rice in Jilin etc. are arranged.Xiangshui County's rice wherein originates from Bohai Sea town, Ningan City, Heilongjiang Province, and its grain of rice is blue or green as beautiful, glittering and translucent, matter is heavy as sand.Cook congee juice such as breast, the glossy excessive perfume (or spice) of steamed rice, meal flavor delicate fragrance is agreeable to the taste, and nutritive value is very abundant.Why best in quality Xiangshui County's rice is, has benefited from it fully and be grown in the unique ecologic environment in the world.Its soil for growth is through the rock decay in 1 years and putrid slime and form, and its mineral, organic matter, micronutrient levels are very abundant.Iirigation water source is from the Jingpo Lake, and water quality is pure limpid.The particular climate environment makes Xiangshui County's rice possess unique quality and edibility simultaneously.But also, extensively there is fake and forged product in the market just because of the reputation and the higher economic worth of geographical sign product.How to protect and differentiate geographical sign product Xiangshui County rice, rarely have report.
Near-infrared spectrum technique is a kind of Dynamic Non-Destruction Measurement of present widespread use, and it has, and speed is fast, efficient is high, cost is low, test favorable reproducibility, make things convenient for characteristics such as simple and easy, pollution-free and non-destructive.Be applied to the discriminating of sour milk kind, fast detecting sweet milk and mingle breast, the soy sauce brand is differentiated in the identification of different places of production flue-cured tobacco fast, fields such as honey brand and apple variety.But do not utilize near-infrared spectrum technique to differentiate the report of geographical sign product at present.
Summary of the invention
The object of the present invention is to provide quick and precisely a kind ofly, simple, what be easy to promote differentiates the method for Xiangshui County's rice with near-infrared spectrum technique.
Overall technical architecture of the present invention is:
A kind of method with near-infrared spectrum technique discriminating Xiangshui County rice comprises the steps:
A, set up the near infrared spectrum discriminating model of geographical sign rice
Select suitable spectrum pretreatment mode respectively, smoothly count, spectrum range, factor number etc. are set up cluster and are differentiated and the qualification discrimination model;
The discriminating of B, unknown sample
Unknown sample scans the near infrared light spectrogram under the same conditions, carries out pre-service, selects identical smoothly counting, spectrum range, factor number, the true and false that cluster differentiation that foundation is set up and qualification discrimination model are judged unknown sample.
Concrete technical solution of the present invention also has:
Steps A comprises the steps:
The diagnosis of a, instrument
B, set up the near infrared spectrum discriminating model of geographical sign rice
B1, scanning rice near infrared light spectrogram
The rice sample mixing of effective dose is placed the non-transmission sample cup of rotation, carry out absorption spectrum scanning with the Fourier near infrared spectrometer; Scan pattern is the non-transmission mode of rotation, sweep limit 4000-12000cm
-1, resolution is 8cm
-1, each scan sample is no less than 7 times, with its averaged spectrum as final analysis spectrum;
The foundation of b2, qualification testing discrimination method model
As reference spectrum, the near infrared light spectrogram of other regional rice is as test spectral with geographical sign rice spectrogram;
Adopt preprocessing procedures to eliminate the influence of disturbing factor, improve the precision of prediction and the stability of model; Preprocess method adopts first order derivative;
Select then smoothly to count 17, spectral range 4000-11500cm
-1, calculate confidence factor CI; According to the scope of geographical sign protection rice and other regional rice CI values, determine rational qualification testing index range 5.4;
The foundation of b3, cluster discrimination model
All rice near infrared spectrogram input clusters are differentiated in the spectrogram storehouse, adopted vector normalization or preprocessing procedures, improve the precision of prediction and the stability of model to eliminate the influence of disturbing factor; Select smoothly to count 17, spectrum range 3996cm
-1-12490cm
-1, factor number selects 15, utilizes the spectrogram distance between mahalanobis distance principle calculating spectrogram, and according to result of calculation spectrogram being gathered is two classes, and area, Xiangshui County rice can access good cluster with other regional rice to be separated.
The diagnosis of instrument comprises among the step a:
A1, noise of instrument
The configuration stabilized voltage supply, it is fully stable that start is preheated to the instrument constant temperature system, guarantees suitable test environment temperature;
A2, wavelength accuracy and reappearance
With the accuracy of standard substance tuning wavelength, prevent drift.
Preprocessing procedures among the step b1 adopts the vector normalization method, first order derivative method, first order derivative+vector normalization method, a kind of in the second derivative method.
Determine among the step b2 that rational qualification testing index range is 5.4.
Preprocessing procedures among the step b3 is selected the vector normalization method for use, first order derivative method, first order derivative+vector normalization method, a kind of in the second derivative method.
Step B comprises the steps:
B1, scanning rice near infrared light spectrogram
The rice sample mixing to be measured of effective dose is placed in the non-transmission sample cup of rotation, carries out absorption spectrum scanning with the Fourier near infrared spectrometer; Scan pattern is the non-transmission mode of rotation, and sweep limit is 4000-12000cm
-1, resolution is 8cm
-1, each scan sample is no less than 7 times, with its averaged spectrum as final analysis spectrum;
B2, qualification testing are differentiated
Unknown sample near infrared light spectrogram is adopted the first order derivative preprocess method, select smoothly to count 17, spectral range 4000-11500cm
-1, calculate confidence factor CI; If the CI value is non-Xiangshui County rice greater than 5.4, if be Xiangshui County's rice less than 5.4;
B3, cluster are differentiated
Adopt vector normalization method pretreatment mode to handle unknown sample near infrared light spectrogram, select smoothly to count 17, spectrum range is 3996cm
-1-12490cm
-1, factor number selects 15; Utilize the mahalanobis distance principle to calculate spectrogram distance between spectrogram, if then be Xiangshui County's rice less than other regional rice apart from area, Xiangshui County rice, otherwise otherwise.
Substantive distinguishing features that the present invention is obtained and significant technical progress are:
This method can be good at distinguishing the true and false of Xiangshui County's rice.Clustering method is divided into the true and false two classes with sample, and resolution is 96%; Adopt qualification testing method Xiangshui County's rice of can discerning the false from the genuine, resolution is 100%.
Description of drawings
Accompanying drawing of the present invention has:
Fig. 1 is Xiangshui County's rice near infrared light spectrogram among the present invention.
Fig. 2 is the spectrogram that obtains after Xiangshui County's rice first order derivative is handled.
Fig. 3 is Xiangshui County's area rice and other regional rice cluster tree derivations.
Fig. 4 is Xiangshui County's area rice and area, non-Xiangshui County rice first derivative spectrum figure.
Fig. 5 is the maximum qualification key map of Xiangshui County's rice and non-Xiangshui County rice near infrared spectrum.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are described further, but not as a limitation of the invention.Protection scope of the present invention is as the criterion with the content of claim record.
Step a, instrument and reagent
Adopt the German BRUKER MPA of company type Fourier near infrared spectrometer, and instrument carries analysis software.
Specimen preparation and spectral scan
Present embodiment uses Xiangshui County's rice to be provided by Ningan City, Heilungkiang Administration of Quality and Technology Supervision, and non-Xiangshui County produces rice available from local supermarket in the area.
Table 1 rice sample information table
Step b, set up the near infrared spectrum discriminating model of geographical sign rice
B1, scanning rice near infrared light spectrogram
Place the non-transmission sample cup of rotation with getting 50g behind the rice sample mixing, adopt the German BRUKER MPA of company type Fourier near infrared spectrometer to carry out absorption spectrum scanning.Sweep limit 4000-10000cm
-1, resolution is 8cm
-1Each scan sample 10 times, with its averaged spectrum as final transmitted spectrum.Adopt OPUS chemometrics application software that the spectrum of sample is handled.
Step b3, cluster discriminating model are set up
Its near infrared spectrum naked eyes seem to be more or less the same as can be seen from Figure 1, can not directly analyze the difference of rice from the spectrogram, therefore must come it is handled by Chemical Measurement software, present embodiment adopts OPUS chemometrics application software that spectrogram is handled.
Be subjected to for reducing near infrared spectrum that sample is inhomogeneous, the factor affecting such as random noise of light scattering and instrument, improve the precision of prediction and the stability of model.Adopt the first order derivative method can keeping sample raw information, and eliminated the influence of disturbing factor.The spectrogram that Fig. 2 obtains after handling for first order derivative.
By to the full wave investigation of spectrum, find at 3996cm
-1-12490cm
-1The wavelength band quantity of information is abundanter, and therefore choosing this SPECTRAL REGION carries out subsequent treatment.
To carry out cluster analysis through pretreated near infrared spectrum, and select factorization as analytical approach, factor number selects 15, and area, Xiangshui County rice can obtain good cluster with other regional rice to be separated, and sees Fig. 3.
The cluster analysis of as can be seen from Figure 3 adopting the factorization analytical approach has been divided into two classes with the near infrared spectrum of Xiangshui County's area rice and other regional rice.Because the distance table of spectrum is understood the similarity of spectrogram, the distance of spectrum increases along with the increase of spectrogram difference, so non-Xiangshui County rice and Xiangshui County's rice obvious difference.
4, the qualification discriminating model is set up
As reference spectrum, other regional rice near infrared spectrums are as test spectral with area, Xiangshui County rice near infrared spectrogram, and first order derivative is selected in pre-service, and smoothly counting is 17, and the gained spectrogram as shown in Figure 4.
The qualification testing index range selects 5.4, and the maximum qualification index that can get reference spectra and test spectral as shown in Figure 5.
Fig. 5 show the index value of reference spectra stable be distributed in CI=5.4 near, show that Xiangshui County's rice quality is more stable, and the index value of test spectral is distributed between the 20-27.Therefore this model can separate Xiangshui County's rice and non-Xiangshui County area rice.
Step B, unknown sample are differentiated
Select 22 kinds of rice samples as testing sample, wherein Xiangshui County's rice is 11 kinds, 11 kinds in non-Xiangshui County rice.Place the non-transmission sample cup of rotation with getting 50g behind the rice sample mixing, carry out absorption spectrum scanning with the Fourier near infrared spectrometer.Scan pattern is the non-transmission mode of rotation, and sweep limit is 4000-12000cm
-1, resolution is 8cm
-1Each scan sample 10 times, with its averaged spectrum as final analysis spectrum.
Step B1, qualification testing are differentiated
Unknown sample near infrared light spectrogram is adopted the first order derivative preprocess method, select smoothly to count 17, spectral range 4000-11500cm-1 calculates confidence factor CI.If the CI value is non-Xiangshui County rice greater than 5.4, if be Xiangshui County's rice less than 5.4.The result shows that 22 kinds of testing samples adopt the qualification testing method to differentiate that all correctly resolution is 100%;
Step B2, cluster are differentiated
Adopt vector normalization method pretreatment mode to handle unknown sample near infrared light spectrogram, select smoothly to count 17, spectrum range 3996cm
-1-12490cm
-1, factor number selects 15.Utilize the mahalanobis distance principle to calculate spectrogram distance between spectrogram, if then be Xiangshui County's rice less than other regional rice apart from area, Xiangshui County rice, otherwise otherwise.The result shows that 22 kinds of testing samples adopt 21 kinds of cluster method of discrimination to differentiate that correctly resolution is 96%.All the other contents as described above.
Claims (7)
1. the method with near-infrared spectrum technique discriminating Xiangshui County rice is characterized in that comprising the steps:
A, set up the near infrared spectrum discriminating model of geographical sign rice
Select suitable spectrum pretreatment mode respectively, smoothly count, spectrum range, factor number etc. are set up cluster and are differentiated and the qualification discrimination model;
The discriminating of B, unknown sample
Unknown sample scans the near infrared light spectrogram under the same conditions, carries out pre-service, selects identical smoothly counting, spectrum range, factor number, the true and false that cluster differentiation that foundation is set up and qualification discrimination model are judged unknown sample.
2. a kind of method with near-infrared spectrum technique discriminating Xiangshui County rice according to claim 1 is characterized in that described steps A comprises the steps:
The diagnosis of a, instrument
B, set up the near infrared spectrum discriminating model of geographical sign rice
B1, scanning rice near infrared light spectrogram
The rice sample mixing of effective dose is placed the non-transmission sample cup of rotation, carry out absorption spectrum scanning with the Fourier near infrared spectrometer; Scan pattern is the non-transmission mode of rotation, sweep limit 4000-12000cm
-1, resolution is 8cm
-1, each scan sample is no less than 7 times, with its averaged spectrum as final analysis spectrum;
The foundation of b2, qualification testing discrimination method model
As reference spectrum, the near infrared light spectrogram of other regional rice is as test spectral with geographical sign rice spectrogram;
Adopt preprocessing procedures to eliminate the influence of disturbing factor, improve the precision of prediction and the stability of model; Preprocess method adopts first order derivative;
Select then smoothly to count 17, spectral range 4000-11500cm
-1, calculate confidence factor CI; According to the scope of geographical sign protection rice and other regional rice CI values, determine rational qualification testing index range 5.4;
The foundation of b3, cluster discrimination model
All rice near infrared spectrogram input clusters are differentiated in the spectrogram storehouse, adopted vector normalization or preprocessing procedures, improve the precision of prediction and the stability of model to eliminate the influence of disturbing factor; Select smoothly to count 17, spectrum range 3996cm
-1-12490cm
-1, factor number selects 15, utilizes the spectrogram distance between mahalanobis distance principle calculating spectrogram, and according to result of calculation spectrogram being gathered is two classes, and area, Xiangshui County rice can access good cluster with other regional rice to be separated.
3. a kind of method with near-infrared spectrum technique discriminating Xiangshui County rice according to claim 2 is characterized in that the diagnosis of instrument among the described step a comprises:
A1, noise of instrument
The configuration stabilized voltage supply, it is fully stable that start is preheated to the instrument constant temperature system, guarantees suitable test environment temperature;
A2, wavelength accuracy and reappearance
With the accuracy of standard substance tuning wavelength, prevent drift.
4. a kind of method of differentiating Xiangshui County's rice with near-infrared spectrum technique according to claim 2, it is characterized in that the preprocessing procedures among the described step b1 adopts the vector normalization method, the first order derivative method, first order derivative+vector normalization method, a kind of in the second derivative method.
5. a kind of method with near-infrared spectrum technique discriminating Xiangshui County rice according to claim 2 is characterized in that determining among the described step b2 that rational qualification testing index range is 5.4.
6. a kind of method of differentiating Xiangshui County's rice with near-infrared spectrum technique according to claim 2, it is characterized in that the preprocessing procedures among the described step b3 selects the vector normalization method for use, the first order derivative method, first order derivative+vector normalization method, a kind of in the second derivative method.
7. a kind of method with near-infrared spectrum technique discriminating Xiangshui County rice according to claim 1 is characterized in that described step B comprises the steps:
B1, scanning rice near infrared light spectrogram
The rice sample mixing to be measured of effective dose is placed in the non-transmission sample cup of rotation, carries out absorption spectrum scanning with the Fourier near infrared spectrometer; Scan pattern is the non-transmission mode of rotation, and sweep limit is 4000-12000cm
-1, resolution is 8cm
-1, each scan sample is no less than 7 times, with its averaged spectrum as final analysis spectrum;
B2, qualification testing are differentiated
Unknown sample near infrared light spectrogram is adopted the first order derivative preprocess method, select smoothly to count 17, spectral range 4000-11500cm
-1, calculate confidence factor CI; If the CI value is non-Xiangshui County rice greater than 5.4, if be Xiangshui County's rice less than 5.4;
B3, cluster are differentiated
Adopt vector normalization method pretreatment mode to handle unknown sample near infrared light spectrogram, select smoothly to count 17, spectrum range is 3996cm
-1-12490cm
-1, factor number selects 15; Utilize the mahalanobis distance principle to calculate spectrogram distance between spectrogram, if then be Xiangshui County's rice less than other regional rice apart from area, Xiangshui County rice, otherwise otherwise.
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| CN101532954B (en) * | 2008-03-13 | 2011-11-30 | 天津天士力现代中药资源有限公司 | Method for identifying traditional Chinese medicinal materials by combining infra-red spectra with cluster analysis |
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| CN110084227A (en) * | 2019-05-22 | 2019-08-02 | 黑龙江八一农垦大学 | Mode identification method based on near-infrared spectrum technique |
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