CN103424374A - Method for quickly detecting freshness level of hairtail by using near-infrared spectrum technology - Google Patents
Method for quickly detecting freshness level of hairtail by using near-infrared spectrum technology Download PDFInfo
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Abstract
The invention discloses a method for quickly detecting freshness of hairtail by using the near-infrared spectrum technology, and aims to overcome defects that a conventional hairtail freshness detection method is complex in process, and the freshness can be polluted by chemical agents. The method adopts the near-infrared spectrum technology and mathematical modeling to establish a model for detecting volatile basic nitrogen content in a hairtail body, then the volatile basic nitrogen content in a sample can be calculated by using the model to analyze a near-infrared spectrum of the hairtail sample, and lastly the freshness of the hairtail can be detected according to the content of the volatile basic nitrogen. The method has the advantage that the analysis speed is high, and chemical pollution can be avoided.
Description
Technical field
The present invention relates to food freshness and detect analysis field, especially relate to a kind of method of near-infrared spectrum technique fast detecting hairtail freshness.
Background technology
Hairtail has another name called hairtail, tooth hairtail etc., and net-rope Perciformes Trichiuridae animal is one of important marine economy fingerling of China, and the tender body of its meat is fertile, delicious flavour, has very high commercial value.Yet hairtail, owing to being rich in unsaturated fatty acid, being vulnerable to the effect of biochemical reaction, microbial reproduction and enzyme and occurring putrid and deteriorated in storage.Wherein, total volatile basic nitrogen (TVBN) is the important indicator of judgement aquatic products degree of spoilage, often is used to detect the aquatic products freshness.TVB-N content is higher, and the aquatic products freshness is poorer.As Chinese patent Granted publication number: CN101892288A, in the patent document in November 24 2010 Granted publication day, the assay method of the corrupt ability of fish spoilage organisms is disclosed, comprise the pure bacterium solution preparation of spoilage organisms, aseptic fish piece preparation, inoculation and spoilage organisms growth rate and corrupt metabolic product generating rate are analyzed, it is characterized in that the aseptic fish piece of preparation is immersed in the pure bacterium liquid of spoilage organisms to be determined, after inoculating, the fish piece is preserved at 5 ℃ of temperature, get inoculation fish piece and do respectively sensory evaluation every about 24 hours, total volatile basic nitrogen (TVBN) is measured, spoilage organisms counting to be determined, the corrupt ability of spoilage organisms uses the amount of the corrupt metabolic product (TVBN) of the unit spoilage organisms generation be inoculated in aseptic fish piece to mean, the corrupt TVBN yield factor (YTVBN/CFU) of putting of the sense organ of usining is as the quantitative target of the corrupt ability of spoilage organisms.
And the method for direct-detection total volatile basic nitrogen need be taken back sample as Micro-kjoldahl method, carry out complicated chemical experiment process, directly detect fast demand in more difficult satisfied modern aquatic products industry.
Summary of the invention
The present invention is in order to overcome the deficiency that the existing procedure that detects the hairtail freshness is complicated, exist chemical reagent to pollute, provide a kind of analysis speed fast, without the method for the near-infrared spectrum technique fast detecting hairtail freshness of chemical contamination.
To achieve these goals, the present invention is by the following technical solutions:
A kind of method of near-infrared spectrum technique fast detecting hairtail freshness, is characterized in that, step is as follows:
1) set up model:
A gets fresh hairtail refrigeration, with cold preservation time, changes and regularly takes out the part hairtail as sample;
The sample that b takes out divides two parts, and a Micro-kjoldahl method that adopts is measured TVB-N content in sample, and another duplicate samples carries out with near infrared spectrometer, detecting after pre-service, detects the near infrared light spectrogram that obtains sample;
C is for data processing to the near infrared light spectrogram of sample, the data after being processed, and data processing method: first spectrum is carried out to the first order derivative processing, then do following computing:
1. calculate averaged spectrum:
2. one-variable linear regression:
3. calculation correction spectrum:
In formula: A
iFor single sample spectrum vector,
For the averaged spectrum vector of all samples, n is sample number, m
iAnd b
iBe respectively the deviation ratio and the translational movement that obtain after each sample one-variable linear regression;
Data after d will process, and the TVB-N content data that record with Micro-kjoldahl method are set up the TVB-N content detection model as modeling data by partial least square method;
2) checking: the verification sample of getting known TVB-N content, verification sample is carried out with near infrared spectrometer, detecting after pre-service, obtain the near infrared light spectrogram, near infrared light spectrogram with the model analysis verification sample established, calculate the model detected value of TVB-N content in verification sample, model detected value and the given value of TVB-N content in the comparatively validate sample, require both to be less than 5% by relative deviation;
3) testing sample analysis: get testing sample and carry out, carry out detecting with near infrared spectrometer after pre-service, obtain the near infrared light spectrogram, with the near infrared light spectrogram of the model analysis testing sample established, calculate TVB-N content in testing sample, estimate the hairtail freshness.
In hairtail, TVB-N content is the important indicator of judgement hairtail degree of spoilage, often is used to detect the freshness of hairtail.Along with the prolongation of hairtail holding time, the protein in hairtail, under the effect of enzyme and bacterium, occurs to decompose and the alkaline nitrogenous things such as generation ammonia (NH) and amine (R-NH :), is total volatile basic nitrogen.By detecting TVB-N content in hairtail, can estimate the hairtail freshness.TVB-N content is higher, and the hairtail freshness is poorer.Detection principle of the present invention is: fresh hairtail is with the prolongation of cold preservation time, and quality changes, and in body, TVB-N content increases gradually.And the spectral absorption band of near-infrared region frequency multiplication, sum of fundamental frequencies and difference frequency absorption band that to be the chemical bond that in organic substance, energy is higher (being mainly CH, OH, NH) absorb at the middle infrared spectral region fundamental frequency are formed by stacking.Hairtail is carried out to the near infrared spectrum detection, can, from the near infrared light spectrogram obtained, reflect protein and amino acid composition information thereof in hairtail.So the near infrared light spectrogram to a plurality of samples carries out data analysis and process, add the TVB-N content data of these samples, use partial least square method can set up a TVB-N content detection model.After model establishes, only need to detect the near infrared spectrum of unknown sample, just can calculate by the model analysis near infrared spectrum TVB-N content of unknown sample, thereby estimate the freshness of hairtail.Than traditional chemical measure, as prior art: Micro-kjoldahl method, near infrared spectrum detects that detection time is short, analysis speed fast, without chemical contamination.
Different sample near infrared spectrum curves shift are more serious, the absorption peak of frequency multiplication, sum of fundamental frequencies and difference frequency is wider and overlapped simultaneously, understand spectrogram more difficult, need to carry out the data processing to spectrum, the near infrared original spectrum is carried out to derivative processing and can eliminate the impact that the factor such as baseline wander is brought, improve the resolution of spectrum.The near infrared original spectrum is carried out linear regression and proofreaies and correct and can remove the mirror-reflection of sample in near-infrared diffuse reflection spectrum and the noise that unevenness causes, eliminate baseline translation and the shift phenomenon of diffuse reflection spectrum.
As preferably, the evaluation criterion of hairtail freshness is: when the TVB-N content of measuring is less than or equal to 13mg/100g, be the one-level freshness; When the TVB-N content of measuring is 13 ~ 25mg/100g, it is the secondary freshness; When the TVB-N content of measuring is more than or equal to 25mg/100g, be three grades of freshnesss.According to the ministerial standard SC-T3102-1984 of Ministry of Agriculture, Animal Husbandry and Fisheries of the People's Republic of China (PRC) " bright hairtail " standard, TVB-N content is the physical and chemical index always of estimating the hairtail grade, primes≤13mg/100g, seconds≤25mg/100g.
As preferably, near infrared spectrometer adopts vehicle mounted portable near infrared detection instrument, and detection mode directly contacts pretreated sample compacting post-sampling for the fibre-optical probe with vehicle mounted portable near infrared detection instrument.Vehicle mounted portable near infrared detection instrument can carry with car, facilitates testing staff's Site Detection of going out.It is sampled by fibre-optical probe, and air disturbs when preventing from detecting, and needs with fibre-optical probe compacting sample.
As preferably, the preprocess method of sample, for sample is carried out to freeze drying, then grinds, and forms dry powder, and dry powder is crossed to 60 mesh sieves.Freeze drying, for removing the most moisture of sample, is beneficial near infrared spectrum and detects.
As preferably, the sweep limit that near infrared spectrometer detects is 4000 ~ 12000 cm
-1, resolution is 4cm
-1, scanning times is 32.At 4000 ~ 12000cm
-1In scope, its main absorbing material is protein, Fat and moisture.
As preferably, the modeling data described in steps d is that to adopt wavelength band be 7502.3 ~ 4246.8cm
-1Data.The spectrum range of selecting while setting up model, comprise the best information amount that the sample wish detects principal ingredient, and this wavelength band has mainly reflected protein and amino acid composition information thereof in hairtail.Promoted the accuracy of institute's established model with this data modeling.
As preferably, the TVB-N content detection model preference pattern dimension of setting up in steps d is 8.The precision of model depends on selected number of principal components, i.e. the model dimension.Dimension is too small, can not effectively utilize spectral information to cause the matching deficiency, and make the modeling effect undesirable, can't explain its complete characteristic; Dimension is excessive, will cause overfitting, background interference and noise increase, the model calculation Speed Reduction of model, thereby not reach the requirement that improves model.According to experimental data relatively, the preference pattern dimension is 8.
As preferably, sample detects with near infrared spectrometer, and replication three times is got the final near infrared light spectrogram of the averaged spectrum of three scannings as sample.Eliminate accidental error, improve detection accuracy.
The accompanying drawing explanation
Fig. 1 detects the near infrared light spectrogram that 0 ℃ of hairtail sample (0 ~ 8d) obtains in the present invention.
Fig. 2 is the near infrared light spectrogram of the 0 ℃ of hairtail sample (0 ~ 8d) after the data processing in the present invention.
Fig. 3 adopts the impact effect figure of modeler model dimension of the present invention to model.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Fresh hairtail in the present embodiment is purchased from Zhejiang Prov Xingye Group Co.,Ltd.Select that body surface is rich in that gloss, the cheek are scarlet, mucus is transparent, eyeball is full, cornea fish body clearly.
In the present embodiment near infrared spectrometer adopt Mat rix-F type near infrared spectrometer (German Bruker company), be vehicle mounted portable near infrared detection instrument.
In the present embodiment, the evaluation criterion of hairtail freshness is with reference to the ministerial standard SC-T3102-1984 of Ministry of Agriculture, Animal Husbandry and Fisheries of the People's Republic of China (PRC) " bright hairtail " standard, specific as follows: when the TVB-N content of measuring is less than or equal to 13mg/100g, be the one-level freshness; When the TVB-N content of measuring is 13 ~ 25mg/100g, it is the secondary freshness; When the TVB-N content of measuring is more than or equal to 25mg/100g, be three grades of freshnesss.
Get fresh hairtail 0 ℃ of lower stored refrigerated 0,1,2,3,4,5,6,7,8 day.Every day, 1 ~ 2 of hairtail was taken out as sample in interval 5 hours, and each sample divides two parts of A, B.
The A sample, after taking-up, is measured TVB-N content in sample according to Micro-kjoldahl method, obtains the sample TVB-N content, and replicate determination three times, as given value.
The B sample takes out 5.0 grams, puts into freeze drier, and dry 10 hours, become laminarly, remove moisture in sample.Then thin slice is ground, be dry powder-shaped, after crossing 60 mesh sieves, with the fibre-optical probe of near infrared detection instrument, contact sample compacting, selecting sweep limit is 4000 ~ 12000 cm
-1, resolution is 4cm
-1, scanning times is 32, each sample replication three times and each all scanning backgrounds, get the near infrared light spectrogram of the averaged spectrum of three scannings as sample.After collecting on a spectrogram, the results are shown in Figure 1 to the near infrared light spectrogram of all samples in 0 ~ 8 day.Visible in Fig. 1,8418cm
-1With 6603 cm
-1Stronger absorption peak is arranged, represent that respectively C-H sum of fundamental frequencies and N-H frequency multiplication absorb; 4595cm
-1Be the sum of fundamental frequencies peak of primary amine and tertiary amine stretching vibration, mainly reflected protein and amino acid composition information thereof in hairtail; 5772cm
-1The first overtone peak of methylene C-H stretching vibration, 5138cm
-1For the secondary frequency multiplication peak of C=O stretching vibration, 4354cm
-1For the sum of fundamental frequencies peak of methylene C-H stretching vibration and flexural vibrations, be mainly the absorption peak of fatty material.
Simultaneously, observe Fig. 1 and also find, the curves shift of spectrogram is more serious, and the absorption peak of frequency multiplication, sum of fundamental frequencies and difference frequency is wider and overlapped simultaneously.Therefore, with OPUS/QUANT-2 software, spectrum is carried out to the data processing, first spectrum is carried out to the first order derivative processing, then do following computing:
1. calculate averaged spectrum:
2. one-variable linear regression:
3. calculation correction spectrum:
In formula: A
iFor single sample spectrum vector,
For the averaged spectrum vector of all samples, n is sample number, m
iAnd b
iBe respectively the deviation ratio and the translational movement that obtain after each sample one-variable linear regression;
After data are processed, obtain the data after a series of processing.Data after processing are reverted on the near infrared light spectrogram, obtain Fig. 2.Curves shift phenomenon in spectrogram obviously improves.The near infrared original spectrum is carried out to derivative processing and can eliminate the impact that the factor such as baseline wander is brought, improve the resolution of spectrum.The near infrared original spectrum is carried out linear regression and proofreaies and correct and can remove the mirror-reflection of sample in near-infrared diffuse reflection spectrum and the noise that unevenness causes, eliminate baseline translation and the shift phenomenon of diffuse reflection spectrum.
Then the data after processing, and TVB-N content in the sample of measuring with Micro-kjoldahl method, given value, as modeling data, is set up model by partial least square method, in model with coefficients R
2, the cross-validation root-mean-square error RMSECV overall target that is the evaluation model accuracy.R
2The predicted value that more approaches 100 explanation models is more accurate, and RMSECV is less shows that the model prediction precision is higher.And with coefficients R
2, cross-validation root-mean-square error RMSECV is that evaluation index is carried out Optimized model, improves model accuracy.
Optimization Modeling one, select the best band scope.
While setting up model, select four different spectral band intervals to be respectively 11996 ~ 4246.8cm
-1, 7502.3 ~ 4246.8cm
-1, 7502.3 ~ 5446.4cm
-1, 6102.1 ~ 4246.8cm
-1, carry out modeling.Table 1 as a result:
Select modeling scope 7502.3 ~ 4246.8cm
-1, coefficient of determination R
2Maximum, cross-validation root-mean-square error RMSECV minimum.
Optimization Modeling two, select the best model dimension.
Model is verified model after setting up.Get the verification sample of 4 known TVB-N contents, measure the near infrared spectrum of verification sample, detect the TVB-N content of sample according to the model of setting up.Comparison model detected value and given value, as shown in table 2,
In table, 4 groups of verification samples, relative deviation all is less than 5%, illustrates that the model detected value is accurate.
Detect the hairtail of unknown freshness with the model established.Get 5.0g as testing sample, put into freeze drier, dry 10 hours, grind and be dry powder-shaped, then cross 60 mesh sieves, with the fibre-optical probe of near infrared detection instrument, contact sample compacting, selecting sweep limit is 4000 ~ 12000 cm
-1, resolution is 4cm
-1Scanning times is 32, each sample replication three times and each all scanning backgrounds, get the near infrared light spectrogram of the averaged spectrum of three scannings as sample, near infrared light spectrogram with the model analysis testing sample established, calculating TVB-N content in testing sample is 16.93 mg/100g, in 13 ~ 25mg/100g scope, is evaluated as the secondary freshness.
Claims (8)
1. the method for a near-infrared spectrum technique fast detecting hairtail freshness, is characterized in that, step is as follows:
1) set up model:
A gets fresh hairtail refrigeration, with cold preservation time, changes and regularly takes out the part hairtail as sample;
The sample that b takes out divides two parts, and a Micro-kjoldahl method that adopts is measured TVB-N content in sample, and another duplicate samples carries out with near infrared spectrometer, detecting after pre-service, detects the near infrared light spectrogram that obtains sample;
C is for data processing to the near infrared light spectrogram of sample, the data after being processed, and data processing method: first spectrum is carried out to the first order derivative processing, then do following computing:
1. calculate averaged spectrum:
2. one-variable linear regression:
3. calculation correction spectrum:
In formula: A
iFor single sample spectrum vector,
For the averaged spectrum vector of all samples, n is sample number, m
iAnd b
iBe respectively the deviation ratio and the translational movement that obtain after each sample one-variable linear regression;
Data after d will process, and the TVB-N content data that record with Micro-kjoldahl method are set up the TVB-N content detection model as modeling data by partial least square method;
2) checking: the verification sample of getting known TVB-N content, verification sample is carried out with near infrared spectrometer, detecting after pre-service, obtain the near infrared light spectrogram, near infrared light spectrogram with the model analysis verification sample established, calculate the model detected value of TVB-N content in verification sample, model detected value and the given value of TVB-N content in the comparatively validate sample, require both to be less than 5% by relative deviation;
3) testing sample analysis: get testing sample and carry out, carry out detecting with near infrared spectrometer after pre-service, obtain the near infrared light spectrogram, with the near infrared light spectrogram of the model analysis testing sample established, calculate TVB-N content in testing sample, estimate the hairtail freshness.
2. the method for a kind of near-infrared spectrum technique fast detecting hairtail freshness according to claim 1, is characterized in that, the evaluation criterion of hairtail freshness is: when the TVB-N content of measuring is less than or equal to 13mg/100g, be the one-level freshness; When the TVB-N content of measuring is 13 ~ 25mg/100g, it is the secondary freshness; When the TVB-N content of measuring is more than or equal to 25mg/100g, be three grades of freshnesss.
3. the method for a kind of near-infrared spectrum technique fast detecting hairtail freshness according to claim 1, it is characterized in that, near infrared spectrometer adopts vehicle mounted portable near infrared detection instrument, and detection mode directly contacts pretreated sample compacting post-sampling for the fibre-optical probe with vehicle mounted portable near infrared detection instrument.
4. according to the method for claim 1 or 2 or 3 described a kind of near-infrared spectrum technique fast detecting hairtail freshnesss, it is characterized in that, the preprocess method of sample, for sample is carried out to freeze drying, then grinds, and forms dry powder, and dry powder is crossed to 60 mesh sieves.
5. according to the method for claim 1 or 2 or 3 described a kind of near-infrared spectrum technique fast detecting hairtail freshnesss, it is characterized in that, the sweep limit that near infrared spectrometer detects is 4000 ~ 12000 cm
-1, resolution is 4cm
-1, scanning times is 32.
6. according to the method for claim 1 or 2 or 3 described a kind of near-infrared spectrum technique fast detecting hairtail freshnesss, it is characterized in that, the modeling data described in steps d is that the employing wavelength band is 7502.3 ~ 4246.8cm
-1Data.
7. according to the method for claim 1 or 2 or 3 described a kind of near-infrared spectrum technique fast detecting hairtail freshnesss, it is characterized in that, the TVB-N content detection model preference pattern dimension of setting up in steps d is 8.
8. according to the method for claim 1 or 2 or 3 described a kind of near-infrared spectrum technique fast detecting hairtail freshnesss, it is characterized in that, sample detects with near infrared spectrometer, and replication three times is got the final near infrared light spectrogram of the averaged spectrum of three scannings as sample.
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| CN104964962A (en) * | 2015-07-14 | 2015-10-07 | 华中农业大学 | Raman spectrum-based method for quickly detecting umami substance inosine monophosphate in fresh fish flesh |
| WO2018019312A1 (en) * | 2016-07-28 | 2018-02-01 | 华南理工大学 | Near infrared dual-band ratio-based method for rapidly predicting frozen pork storage time |
| US11448592B2 (en) | 2016-07-28 | 2022-09-20 | South China University Of Technology | Method for rapidly predicting freezer storage time of frozen pork based on reflectance ratio of two near-infrared bands |
| CN107688008A (en) * | 2017-07-19 | 2018-02-13 | 北京化工大学 | A kind of quick, method of infrared spectrophotometry of accurate measurement animal glue drying time |
| CN107688008B (en) * | 2017-07-19 | 2020-12-11 | 北京化工大学 | Infrared spectrum method for quickly and accurately measuring drying time of animal glue |
| CN109856079A (en) * | 2018-12-14 | 2019-06-07 | 华南理工大学 | The method of near infrared multispectral imaging quick nondestructive evaluation flesh of fish fat oxidation degree |
| CN111521580A (en) * | 2020-06-16 | 2020-08-11 | 海南大学 | Fillet freshness detection method based on portable near-infrared spectrometer |
| CN112213281A (en) * | 2020-11-16 | 2021-01-12 | 湖北省农业科学院农产品加工与核农技术研究所 | Comprehensive evaluation method for rapidly determining freshness of freshwater fish based on transmission near infrared spectrum |
| CN113791049A (en) * | 2021-08-30 | 2021-12-14 | 华中农业大学 | Method for rapidly detecting freshness of chilled duck meat by combining NIRS and CV |
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