CN102353644A - Rapid near infrared spectroscopy method for simultaneously detecting moisture content and protein content of Trichiurus japonicus surimi - Google Patents
Rapid near infrared spectroscopy method for simultaneously detecting moisture content and protein content of Trichiurus japonicus surimi Download PDFInfo
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Abstract
The invention relates to a rapid near infrared spectroscopy method for simultaneously detecting the moisture content and protein content of Trichiurus japonicus surimi, comprising the following concrete steps of: (1) collecting a Trichiurus japonicus surimi sample; (2) determining the moisture content and protein content of the sample by a national standard method; (3) acquiring near infrared spectroscopy data of the collected sample by the utilization of a near infrared spectrometer; (4) associating the near infrared spectroscopy data of each sample with the determined moisture value and protein value , and establishing a quantitative calibration model by the use of a chemometric software; (5) verifying the calibration model; (6) determining the unknown surimi sample moisture and protein contents. The method provided by the invention is rapid and accurate and is simple to operate. The whole detection process only needs about one minute.
Description
[technical field]
The present invention relates to the method for quick of a kind of moisture, protein content, specifically, relate to a kind of near-infrared spectrum method that detects rotten moisture of hairtail and protein content fast simultaneously.
[background technology]
Fish is rotten, be about to the pre-service of fresh and alive raw material fish after, through adopting meat, rinsing, smart filter, dehydration, packing, freezing to form intermedin section product, be widely used in the production of surimi products such as fish ball, breaded fish stick with certain preservation term.Hairtail (Coiliaspp) aboundresources, cheap is the important source material of the rotten processing of China fish.
The frozen minced fillets of high-quality has advantages such as high protein, low fat, good springiness, whiteness height, storage tolerance.Along with the increase year by year of output and consumption figure, more and more higher to its quality requirements.In order to ensure the rotten quality of fish, production firm has formulated relevant criterion to indexs such as its main nutrient composition and elasticity.Moisture and protein are the main nutrient composition in the fish gruel, existing detection method direct drying method and Kjeldahl, and consuming time, effort can't realize that two kinds of materials detect simultaneously.Therefore be badly in need of setting up a kind of fast, convenient, accurate test method is that manufacturer is used.
(Near-Infrared Spectroscopy is to develop a kind of green analytical technology rapidly the eighties in 20th century NIRS) near infrared spectrum, has advantages such as quick, convenient, harmless, that polycomponent detects simultaneously.At present, this technology is already in full swing in Application for Field such as agricultural, medicine, chemical industry.In recent years, in grain and oil and feed detection, China is the detection method of this technology as a kind of standard.Explore, discover that this technology also can realize the fast detecting of moisture, protein content in the fish gruel through the applicant.
[summary of the invention]
Technical matters to be solved by this invention is existing to detect in the hairtail gruel moisture and method for determination of protein direct drying method and Kjeldahl is consuming time, require great effort; Two kinds of problems that composition can not detect simultaneously; And providing a kind of quick, easy to this problem, the diffuse reflection near infrared spectrometer that utilizes that polycomponent detects simultaneously combines Chemical Measurement to detect moisture and method for determination of protein in the hairtail gruel.
The objective of the invention is to realize through following technical scheme:
A kind of near-infrared spectrum method that detects fast rotten moisture of hairtail and protein content simultaneously, concrete steps do,
(1) collects the rotten sample of hairtail;
(2) adopt state's calibration method that moisture in the sample and protein content are measured;
(3) utilize near infrared spectrometer to gather the near infrared spectrum data of collected sample;
(4) with the near infrared spectrum data of each sample with the moisture value of being measured with the protein value is corresponding one by one is associated, utilize Chemical Measurement software to carry out match, set up the quantitative correction model;
(5) checking of calibration model;
(6) mensuration of rotten sample moisture of unknown fish and protein content;
Collect the rotten sample of hairtail of different manufacturers different batches in the above-mentioned steps (1).
The mensuration of moisture and protein content adopts GB 5009.3-2010 direct drying method and GB 5009.5-2010 Kjeldahl respectively in the above-mentioned steps (2).
Spectrum data gathering described in the above-mentioned steps (3), the NIRFlex N500 type near infrared spectrometer of use BUCHI company, and solid is measured accessory Pei Shi double dish; Spectra collection mode and acquisition condition are: use diffuse reflection to gather near infrared spectrum, the scanning wave-number range is 4000-10000cm
-1, scanning times is 32 times, resolution is 8cm
-1, be with reference to background with Spectralon, every 4cm
-1Gather a data points, gather 1501 altogether; Sweep limit is controlled between 20-25 ℃.Each sample parallel sweep three times is averaged as the near infrared spectrum data of sample.
Use the NIRCal5.2 software of BUCHI company in the above-mentioned steps (4), moisture and protein model all adopt the method for setting up the checking collection to carry out internal verification, and offset minimum binary (PLS) method is set up regression model.Before setting up calibration model, need to select wavelength, main cause subnumber and spectrum pre-service.Concrete parameter is following.
| Composition | Wave-number range (cm -1) | The main cause subnumber | Preprocessing procedures | Homing method |
| Moisture | ?400-4800，5400-6600，7800-10000 | 10 | ncl | PLS |
| Protein | 4400-4800，5400-6600，7800-10000 | 10 | mf | PLS |
The rotten sample of hairtail 10 (content needs within the calibration model content range) of choosing known moisture and protein content in the above-mentioned steps (5) is as the external certificate sample.Near infrared spectra collection parameter in (3) is carried out near infrared spectrum scanning set by step, and each sample parallel sweep is averaged for 3 times.10 sample spectra are imported in the calibration model of moisture, obtain the near infrared predicted value of moisture, spectrum is imported in the calibration model of protein content, obtain the near infrared predicted value of protein content.Near infrared predicted value and direct drying method or Kjeldahl measured value are carried out paired t-test, when setting degree of confidence and be 95%, utilize the difference between the measured value that predicted value that the inventive method obtains and direct drying method or Kjeldahl obtain not remarkable.Moisture and protein content that this explanation utilizes near infrared spectroscopy of the present invention to measure in the hairtail gruel are feasible.Can replace direct drying method and Kjeldahl measured value in other words.
Get the rotten sample of hairtail of moisture to be measured and protein content in the above-mentioned steps (6), carry out near infrared spectrum scanning according to the near infrared spectra collection parameter in the step (3).Spectrum is imported respectively in moisture and the protein content calibration model, just can obtain the analysis result of moisture and protein fast.In addition, all content is meant mass percent among the present invention.
Near infrared spectroscopy provided by the invention is measured moisture and the method for determination of protein in the hairtail gruel, and is quick, accurate, easy and simple to handle.Whole testing process only needs about 1 minute, and direct drying method or Kjeldahl need continue more than 4 hours.This method can be applicable in the rotten manufacturer of fish.
It should be noted that the present invention is applicable to the rotten moisture of hairtail between 73.97%～80.05%, protein content is between 10.39%～17.14%.Moisture and the protein content scope rotten with common on the market hairtail are consistent.
[description of drawings]
Fig. 1 is the rotten near infrared primary light spectrogram of hairtail;
Fig. 2 is the near-infrared reflection spectrogram of hairtail gruel after ncl handles;
Fig. 3 is the near-infrared reflection spectrogram of hairtail gruel after mf handles;
Fig. 4 is the correlationship figure of direct drying method moisture value and near infrared prediction moisture value;
Fig. 5 is the correlationship figure of Kjeldahl protein value and near infrared PPV;
Marginal data: ◇ representes calibration collection sample, and representes checking collection sample.
[embodiment]
The embodiment of the method for a kind of near-infrared spectrum method that detects fast rotten moisture of hairtail and protein content simultaneously of the present invention below is provided.
Embodiment 1
Below in conjunction with accompanying drawing 1-5 and embodiment the present invention is further specified.
1, the collection of calibration set sample:
The rotten sample of hairtail of a plurality of batches of 4 different manufacturers has been collected in this experiment, amounts to the rotten samples of 125 portions of hairtails.
2, the mensuration of calibration set sample chemical reference value:
The mensuration of moisture adopts GB 5009.3-2010 direct drying method, and the mensuration of protein content adopts GB 5009.5-2010 Kjeldahl.The moisture of final all samples and the mensuration result such as the following table of protein content.
3, the collection of calibration set sample spectral data:
Spectrum data gathering, the NIRFlex N500 type near infrared spectrometer of use BUCHI company, and solid is measured accessory Pei Shi double dish.Get the rotten sample 60g of fish and put into the Pei Shi double dish, fully compacting.Spectra collection mode and acquisition condition are: use diffuse reflection to gather near infrared spectrum, the scanning wave-number range is 4000-10000cm
-1, scanning times is 32 times, resolution is 8cm
-1, be with reference to background with Spectralon, every 4cm
-1Gather a data points, gather 1501 altogether.Sweep limit is controlled between 20-25 ℃.Each sample parallel sweep three times is averaged as the near infrared spectrum data of sample.The primary light spectrogram of the rotten sample of the hairtail that collects is referring to Fig. 1, and Fig. 2 is the near-infrared reflection spectrogram of hairtail gruel after ncl handles; Fig. 3 is the near-infrared reflection spectrogram of hairtail gruel after mf handles.
4, the foundation of calibration model
(1) foundation of the rotten moisture calibration model of fish
The NIRCal5.2 software of operation BUCHI company, the near infrared spectrum data of each sample is corresponding one by one with the moisture value of being measured, import the rotten near infrared light spectrogram of the fish that respective value is arranged.And the parameter of above-mentioned software done setting as described in Table 1.This experiment adopt to be set up checking collection method and is carried out internal verification, and all samples is divided into calibration collection and checking collection with 2: 1 ratio, and wherein to be selected into calibration concentrated for maximal value and minimum value.Table 2 is the modeling result of moisture under this parameter.The near infrared predicted value of this calibration model moisture and the correlationship figure of chemical assay value see Fig. 4.
The setting of table 1 parameter
The modeling result of table 2 moisture
Rc representative calibration related coefficient in the table 2, R
VRepresentative checking related coefficient, SEC representative calibration standard deviation, SEP represents validation criteria poor, and RSD represents relative standard deviation, and RPD represents relative analytical error.
If RSD＜10%, RPD＞3, then the explanation calibration is respond well, and precision of prediction is high, and the NIRS that is set up (near-infrared spectrum technique) calibration model can be used for actual detected.Can know by last explanation verify it is to can be used in the rotten moisture of unknown hairtail is carried out quantitative test internally according to the rotten moisture calibration model of hairtail that the present embodiment method is set up.
(2) foundation of the rotten protein content calibration model of fish
The NIRCal5.2 software of operation BUCHI company, the near infrared spectrum data of each sample is corresponding one by one with the protein value of being measured, import the rotten near infrared light spectrogram of the hairtail that respective value is arranged.And the parameter of above-mentioned software done setting as described in Table 3.This experiment employing leaving-one method carries out internal verification, and the ratio of all samples with 2: 1 is divided into the calibration collection and verifies collection, and wherein maximal value and minimum value are selected into to calibrate and concentrate.Table 4 is the modeling result of protein content under this parameter.The near infrared predicted value of this calibration model protein content and the correlationship figure of chemical assay value see Fig. 5.
The setting of table 3 parameter
The modeling result of table april protein content
The calibration collection of the rotten protein calibration model of hairtail and checking collection all meet RSD＜10%, RPD＞3, so this model can be applied to the quantitative test of the rotten protein content of hairtail.
5, the checking of calibration model
Other gets the rotten sample of hairtail 10 (content is within the calibration model content ranges) of known moisture and protein content as the external certificate sample.Carry out near infrared spectrum scanning by the identical near infrared spectra collection parameter of calibration set sample.Each sample parallel sweep 3 times is averaged.Near infrared spectrum is imported respectively in moisture calibration model and the protein calibration model, analyze the near infrared predicted value that obtains moisture and protein.The result sees table 5.
The rotten external certificate result of table 5 hairtail
The moisture that utilizes the rotten samples of 10 hairtails that the SPSS of statistical software obtains present embodiment method (being near-infrared method) and direct drying method and Kjeldahl (chemical method) and protein content result match T and check, and the result sees table 6.
The chemical reference value and the near infrared method predicted value paired t-test result of rotten moisture of table 6 hairtail and protein content.
Annotate: t0.05 (9)=2.262
Can find out that from table 6 setting degree of confidence is at 95% o'clock, no matter the moisture calibration model still is the protein calibration model, and the difference between its near infrared predicted value and the chemical assay value is remarkable (p＞0.05) not.
Therefore, rotten moisture of the described near infrared method mensuration of present embodiment hairtail and protein content result have good accuracy.
6, the mensuration of rotten sample moisture of unknown hairtail and protein content
Get the rotten sample of hairtail of moisture to be measured and protein content, carry out near infrared spectrum scanning according to the identical near infrared spectra collection parameter of calibration set sample.Spectrum is imported respectively in moisture and the protein content calibration model, just can obtain the analysis result of moisture and protein fast.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the present invention's design; Can also make some improvement and retouching, these improvement and retouching also should be considered as in protection scope of the present invention.
Claims (4)
1. a near-infrared spectrum method that detects fast rotten moisture of hairtail and protein content simultaneously is characterized in that, concrete steps do,
(1) collects the rotten sample of hairtail;
(2) adopt state's calibration method that moisture in the sample and protein content are measured;
(3) utilize near infrared spectrometer to gather the near infrared spectrum data of collected sample;
(4) with the near infrared spectrum data of each sample with the moisture value of being measured with the protein value is corresponding one by one is associated, utilize Chemical Measurement software to carry out match, set up the quantitative correction model;
(5) external certificate of calibration model;
(6) mensuration of rotten sample moisture of unknown fish and protein content.
2. the near-infrared spectrum method that detects rotten moisture of hairtail and protein content fast simultaneously as claimed in claim 1 is characterized in that moisture and protein content adopt direct drying method and Kjeldahl to obtain in the above-mentioned steps (2).
3. the near-infrared spectrum method that detects rotten moisture of hairtail and protein content fast simultaneously as claimed in claim 1, the scanning spectrum district wave-number range of near infrared spectrometer is 4000-10000cm in the above-mentioned steps (3)
-1, collected specimens near-infrared diffuse reflection spectrum information, used accessory is the Pei Shi double dish.
4. the near-infrared spectrum method that detects rotten moisture of hairtail and protein content fast simultaneously as claimed in claim 1 utilizes NIRCal5.2 software to carry out data fitting in the above-mentioned steps (4); Moisture and protein model all adopt to set up verifies that diversity method carries out internal verification, and offset minimum binary (PLS) method is set up regression model; Before setting up calibration model, need to select optimal wavelength, main cause subnumber and preprocessing procedures; Concrete parameter is following: the wave-number range (cm of moisture and protein
-1) be respectively 4400-4800,5400-6600,7800-10000 and 4400-4800,5400-6600,7800-10000; The main cause subnumber of moisture and protein is respectively 10 and 10, and the preprocessing procedures of moisture and protein is respectively ncl and mf, and the homing method of moisture and protein is respectively PLS and PLS.
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| CN103344597A (en) * | 2013-05-06 | 2013-10-09 | 江南大学 | Anti-flavored-interference near infrared non-destructive testing method for internal components of lotus roots |
| CN103364369A (en) * | 2013-07-22 | 2013-10-23 | 天津长芦海晶集团有限公司 | Quantitative test method for components of additives in PA6 producing process |
| CN103424374A (en) * | 2013-06-19 | 2013-12-04 | 浙江省海洋开发研究院 | Method for quickly detecting freshness level of hairtail by using near-infrared spectrum technology |
| CN103592255A (en) * | 2013-11-22 | 2014-02-19 | 山东东阿阿胶股份有限公司 | Soft method for measuring total protein content of donkey-hide gelatin skin solution on basis of near infrared spectrum technology |
| CN104062256A (en) * | 2013-04-15 | 2014-09-24 | 山东东阿阿胶股份有限公司 | Soft measurement method based on near infrared spectroscopy |
| CN104101579A (en) * | 2014-05-06 | 2014-10-15 | 浙江省海洋开发研究院 | Hairtail producing area rapid detection method |
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| CN103344597A (en) * | 2013-05-06 | 2013-10-09 | 江南大学 | Anti-flavored-interference near infrared non-destructive testing method for internal components of lotus roots |
| CN103424374B (en) * | 2013-06-19 | 2015-10-21 | 浙江省海洋开发研究院 | A kind of near-infrared spectrum technique detects the method for hairtail freshness fast |
| CN103424374A (en) * | 2013-06-19 | 2013-12-04 | 浙江省海洋开发研究院 | Method for quickly detecting freshness level of hairtail by using near-infrared spectrum technology |
| CN103364369A (en) * | 2013-07-22 | 2013-10-23 | 天津长芦海晶集团有限公司 | Quantitative test method for components of additives in PA6 producing process |
| CN103592255A (en) * | 2013-11-22 | 2014-02-19 | 山东东阿阿胶股份有限公司 | Soft method for measuring total protein content of donkey-hide gelatin skin solution on basis of near infrared spectrum technology |
| CN104101579A (en) * | 2014-05-06 | 2014-10-15 | 浙江省海洋开发研究院 | Hairtail producing area rapid detection method |
| CN104819953A (en) * | 2015-04-21 | 2015-08-05 | 通威股份有限公司 | DL-methionine rapid detecting method based on near-infrared spectroscopy |
| CN104949936A (en) * | 2015-07-13 | 2015-09-30 | 东北大学 | Sample component determination method based on optimizing partial least squares regression model |
| CN104949936B (en) * | 2015-07-13 | 2017-10-24 | 东北大学 | Sample component assay method based on optimization Partial Least-Squares Regression Model |
| CN105588819A (en) * | 2016-03-11 | 2016-05-18 | 江西出入境检验检疫局检验检疫综合技术中心 | Method for conducting near-infrared rapid detection on component content in infant formula rice flour |
| CN106092962A (en) * | 2016-08-17 | 2016-11-09 | 山西省农业科学院农作物品种资源研究所 | A kind of near infrared spectroscopy quickly detects the method for millet crude protein content |
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Application publication date: 20120215 |