CN104568815A - Method for quickly and nondestructively detecting content of volatile basic nitrogen in fresh beef - Google Patents
Method for quickly and nondestructively detecting content of volatile basic nitrogen in fresh beef Download PDFInfo
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Abstract
The invention provides a method for quickly and nondestructively detecting the content of volatile basic nitrogen in fresh beef. The method is used for detecting the content of volatile basic nitrogen in the fresh beef based on a portable near-infrared spectrometer, and has the characteristics of simplicity, quickness, high efficiency and accuracy in comparison with a national standard method for detecting the content of volatile basic nitrogen and other application methods of a table-type Fourier near-infrared spectrometer at present; the method does not have size and shape limitations on a detection sample, does not need to perform any destructive pretreatment on the detection sample, realizes nondestructive detection and reduces cost; a microprocessor with a system program is high in intelligent level, both detection and analysis are automatically finished, a detection result is displayed in real time, an operator does not need to be specially trained, and the method is simple and convenient to carry out and can be applied to online detection.
Description
Technical field
The present invention relates to spectral detection field, computer realm, Chemical Measurement and food technical field of nondestructive testing, specifically, relate to application portable near infrared spectrometer to the fast non-destructive detection method of TVB-N content in fresh beef appetizer.
Background technology
Beef is the health meat product that the maximum a kind of nutritive value of state's human consumption is higher, and it is nutritious, and protein content is very high, fat content is relatively low, and amino acid composition is more suitable for the demand of human body, and containing more mineral matter, delicious flavour, enjoys the laudatory title of " in meat favourite son ".Along with the fast development of Chinese national economy and the significantly raising of living standards of the people, the diet structure of people also there occurs respective change, the level of consumption of beef maintains sustained and rapid growth, and the quality of beef is also subject to very large attention simultaneously, and the requirement of people to fresh beef appetizer freshness constantly promotes.But due to present stage China at steer ration, butcher, transport, sell and can review in system etc. still unsound, the beef of commercial type is caused to there is quality uneven, the phenomenon of inferior quality, the beef product of current high-quality high-grade mainly relies on import, trace it to its cause and mainly contain following several respects: one, China's fresh beef appetizer quality safety detection means is single, cause beef quality on market to mix, good and the bad difficulty point, cannot embody high quality and favourable price; Two, the existing Quality Beef safety detection method of China mainly adopts physical and chemical inspection method, there is low, the consuming time length of efficiency, complex operation, product destroy the series of problems such as large, cannot meet demand that is in real time in enormous quantities and on-line quick detection; Three, although the quality safety detection technique of the various advanced person of Introduced From Abroad, at present at home still in the experimental stage that demonstration and technology are applied, do not apply in the testing of China's Beef Industry and go.Set up a kind ofly can to carry out in enormous quantities the freshness of fresh beef appetizer, safety, fast, in real time, accurately and harmless detection means put on the agenda.
China is the content of total volatile basic nitrogen (TVB-N) for the important indicator that fresh beef appetizer freshness carries out evaluating.This material is that protein in animal food is in decay process, the ammonia produced through enzyme and microbial action and amine etc. have volatile alkaline nitrogen substance, can distill from aqueous solution in the basic conditions, after boric acid absorbs, by its content of standard salt acid solution titration determination, TVB-N content can increase along with the corruption aggravation of fresh beef appetizer.At present, total volatile basic nitrogen is for evaluating unique physical and chemical index of meat freshness in GB.
Semimicro nitriding and microdiffusion that the method for total volatile basic nitrogen in meat product is GB/T5009.44-2003 is measured in existing national standards, these two kinds of methods need carry out the process such as sample broke, leachable lixiviate and test substance collection to testing sample, operating process is loaded down with trivial details, time-consuming, sense cycle is long, large and there is destructiveness by interference from human factor, detected sample can not continue on for producing or selling, cause a large amount of wastes of actual production, can not meet batch, quick, real-time and harmless testing requirement.And near-infrared spectrum technique detects detection technique as a kind of novel optical, obtain applying more and more widely in agricultural product, livestock products and field of food detection.Recent domestic scientific research personnel has attempted this technology to be applied to and has carried out Primary Evaluation work to the content of total volatile basic nitrogen in fresh meat.Hou Ruifeng (2006) adopts desk-top Fourier transform near infrared instrument to detect the content of total volatile basic nitrogen in live fresh pork.The intramuscular fat of macroscopic in testing sample and manadesma need be rejected by the method, and when spectroscopic data information acquisition, the size and dimension of sample cup per sample need be repaiied type, in addition desk-top Fourier's near infrared spectrometer is not easy to carry, because this method sample pre-treatments step is complicated, restricted and have destruction to sample to the shape and size of sample, therefore adopt desk-top Fourier transform near infrared instrument to be not suitable for online Fast nondestructive evaluation to TVB-N content in sample.Ma Shibang etc. (2013) adopt the Vis/NIR detection system be made up of camera bellows, light source, objective table, spectrometer, computing machine five part of building voluntarily to detect the TVB-N content in fresh beef appetizer.This method need adopt camera bellows to shield the impact of extraneous light on testing result, installs external light source voluntarily and regulates light-source angle, need regulate the distance of objective table and fibre-optical probe during actual detection.This method sample pre-treatments step is simple, but because near infrared detection system needs being made by manufacturers or users, and need to regulate light source and the angle and distance between objective table and sample before each sample detection, therefore the Vis/NIR detection system that employing is built voluntarily is also not suitable for the online Fast nondestructive evaluation to TVB-N content in sample.At present, application near-infrared spectral analysis technology is rarely had to detect the report of TVB-N content in fresh beef appetizer both at home and abroad.
Along with the development of computer technology, infotech and modern detecting, blank for filling up the application that near-infrared spectral analysis technology is detecting TVB-N content in fresh beef appetizer, improve China's fresh beef appetizer quality safety detection technique, ensure China's fresh beef appetizer food hygiene quality safety, exploitation detects the online fast non-destructive detection method of TVB-N content in fresh beef appetizer, and tool is of great significance.
Publication number is the fast non-destructive detection method that the Chinese patent application of CN103712948A discloses TVB-N content in fresh mutton.But it is directly used as the preprocess method of optimum prediction model and optimum data by maximum group of selection Rp value, the each group of model that evaluating is the highest is used to predict even if can cause, also may produce overfitting causes parameter better, but can not obtain good result of use.
Summary of the invention
The object of this invention is to provide the fast non-destructive detection method of TVB-N content in a kind of fresh beef appetizer.
In order to realize the object of the invention, the fast non-destructive detection method of TVB-N content in a kind of fresh beef appetizer of the present invention, comprises the following steps:
1) batch capture fresh beef appetizer sample, the near infrared spectrum data information of collected specimens, detects the TVB-N content of sample according to the chemical detection method of national Specification;
2) by step 1) in the sample near infrared spectrum data information that gathers mutually corresponding with TVB-N content chemical measurements and set up sample sets, be divided into calibration set and checking to collect in proportion.After different Pretreated spectra is carried out to the sample spectral data information gathered, use spectroscopic data information and the TVB-N content chemical measurements of calibration set, set up the forecast model of TVB-N content in fresh beef appetizer; Utilize the spectroscopic data information of checking collection, TVB-N content chemical measurements and model parameter to carry out the precision of valuation prediction models, determine the best preprocess method of near infrared spectrum data information for TVB-N content in fresh beef appetizer and optimum prediction model;
3) utilize step 2) in the best preprocess method of the near infrared spectrum data information of TVB-N content and optimum prediction model in fixed fresh beef appetizer, detect the TVB-N content of fresh beef appetizer sample to be measured.
Step 1) near infrared spectrum information acquisition use carried out to sample spectral range be 1000nm ~ 1800nm.
Step 1) in the TVB-N content of chemical detection method to sample that specify according to standard GB/T/T 5009.44-2003 detect.
Step 2) in comprise at least one in the methods such as standardization (average centralization, standardization), differentiate (Savitzky-Golay first order derivative, difference first order derivative), Savitzky-Golay are level and smooth, signal correction (multiplicative scatter correction MSC, standard be change of variable SNV, clean analytic signal NAS, Orthogonal Signal Correction Analyze OSC just too, and trend of going corrects DT, baseline correction) for the near infrared spectrum data information preprocessing method of TVB-N content in fresh beef appetizer.
Step 2) in calibration set and verify that the ratio that integrates is as 2:1 or 3:1, preferred 3:1.
Step 2) in include but are not limited to calibration set standard deviation (SEC), validation-cross standard deviation (SECV), checking collection standard deviation (SEP), calibration set related coefficient (Rc), checking collection related coefficient (Rp) for the precision evaluating of the optimum prediction model of TVB-N content in fresh beef appetizer.
Step 2) in collect related coefficient (Rp) descending sort according to the arrangement of calibration set standard deviation (SEC) ascending order, the arrangement of validation-cross standard deviation (SECV) ascending order, standard deviation (SEP) the ascending order arrangement of checking collection, calibration set related coefficient (Rc) descending sort, checking, obtain five groups of array datas, often group gets front 10 models, bring each for inspection set spectroscopic data into each model, obtain the predicted value of fresh beef appetizer total volatile basic nitrogen.The chemical score of the fresh beef appetizer total volatile basic nitrogen of inspection set is divided into two groups: 1, be less than 10mg/100g; 2, be more than or equal to 10mg/100g and be less than or equal to 15mg/100g, and by each group of predicted value comparison corresponding with chemical score, to determine predictablity rate, choose one group of near infrared spectrum data information optimum prediction model as TVB-N content in fresh beef appetizer that predictablity rate is the highest, the spectroscopic data information preprocessing method of this group is best preprocess method.
In the present invention, the device realizing the fast non-destructive detection method of TVB-N content in above-mentioned fresh beef appetizer is portable near infrared spectrometer (Fig. 1), and this device is made up of six parts such as light source (halogen tungsten lamp) and grating 1, output optical fibre 2, detection probe 3, input optical fibre 4, detecting device 5 and microprocessors 6.Wherein, detection probe 3 is connected with detecting device 5 with input optical fibre 4 by output optical fibre 2; During collected specimens near infrared light spectrum information, sample is without the need to carrying out any destructive pre-treatment, sample surfaces is close in detection probe 3, form the monochromatic light near infrared spectral range through grating beam splitting after light is sent by light source, monochromatic light arrives detection probe 3 through output optical fibre 2 and is radiated on sample, diffusing that its surface is formed is gathered by detection probe 3, arrives detecting device 5 through input optical fibre 4, and detecting device 5 records the spectral information of sample under this wavelength and is sent to microprocessor 6; Microprocessor 6 converts spectral information to spectroscopic data information, after in the fresh beef appetizer be loaded into, the best preprocess method of the spectroscopic data information of TVB-N content and optimum prediction model carry out pre-service to the testing sample near infrared spectrum data information gathered automatically, be input in optimum prediction model, the TVB-N content of sample is detected.This device can be used as the portable near infrared spectrometer carried with, thus reaches the requirement of online Fast nondestructive evaluation.
This method detects TVB-N content in fresh beef appetizer based on portable near infrared spectrometer, compared with traditional national standard detection method, has that detection time is short, detection speed is fast, the simple feature of step; The size and dimension detecting sample not being limited, without the need to carrying out any destructive pre-treatment to detection sample, realizing Non-Destructive Testing, cost-saving; Microprocessor (system program) intelligence degree is high, and detect and automatically complete, automatic analysis display results in real time, testing staff is without the need to Special Training, simple to operate, convenient, can be applicable to on-line checkingi.
Accompanying drawing explanation
Fig. 1 is the operating diagram of portable near infrared spectrometer; Wherein, 1 is light source and grating, and 2 is output optical fibre, and 3 is detection probe, and 4 is input optical fibre, and 5 is detecting device, and 6 is microprocessor (system program), and 7 is fresh beef appetizer measuring samples.
Fig. 2 is the process flow diagram setting up forecast model in the embodiment of the present invention 1 for TVB-N content in fresh beef appetizer.
Fig. 3 is the near infrared spectrum hum pattern of all fresh beef appetizer samples in the embodiment of the present invention 1.
Fig. 4 is the PRESS value of the different main cause subnumbers of TVB-N content optimum prediction model in fresh beef appetizer in the embodiment of the present invention 1.
Fig. 5 is the optimum prediction model tuning collection parameter of TVB-N content in fresh beef appetizer in the embodiment of the present invention 1.
Fig. 6 is the optimum prediction modelling verification collection parameter of TVB-N content in fresh beef appetizer in the embodiment of the present invention 1.
Embodiment
Following examples for illustration of application of the present invention, but do not limit the scope of the present invention's use.If do not specialize, the conventional means that technological means used in embodiment is well known to the skilled person, is raw materials usedly commercial goods.
The foundation of the fast non-destructive detection method of TVB-N content in embodiment 1 fresh beef appetizer
In application portable near infrared spectrometer Fast nondestructive evaluation fresh beef appetizer, the method establishment schematic flow sheet of TVB-N content as shown in Figure 2.
(1) sample collection
Gather 252 parts of fresh beef appetizer samples from the market.
(2) sample near infrared spectrum information acquisition
The near infrared light spectrum information (Fig. 3) of 252 parts of fresh beef appetizer samples in acquisition step (1).Before gathering near infrared light spectrum information, beef sample to be checked is without the need to any destructive pre-treatment.In near infrared spectrum information acquisition process, beef sample surface to be checked is close in the detection probe 3 of portable near infrared spectrometer (Fig. 1), avoids because light leak causes the spectral information of collection inaccurate.The collection of sample temperature near infrared spectrum has a significant effect, and near infrared spectrum information acquisition process, the temperature of all beef samples to be checked must remain at 0-4 DEG C.The near-infrared spectrum wavelength scope gathered is 1000nm-1800nm, and resolution is 10nm, and every part of measuring samples carries out 3 spectra collections, every minor tick 5 second, and gather, spectral scan number of times is 10 times at every turn.
(3) detection of TVB-N content chemical score
The microdiffusion introduced in GB GB/T 5009.44-2003 meat quail hygienic standard is adopted 252 fresh beef appetizer samples in step (1) to be carried out to the detection of total volatile basic nitrogen chemical measurements.
(4) division of calibration set and checking collection
The near infrared spectrum data information of all fresh beef appetizer samples gathered in step (2) is mutual corresponding with the chemical measurements of the fresh beef appetizer sample TVB-N content detected in step (3) and set up sample sets, be divided into calibration set and checking to collect the TVB-N content chemical measurements of the near infrared spectrum data information and correspondence being about to wherein 190 samples as calibration set according to the ratio of 3:1, the near infrared spectrum data information of 62 samples and the TVB-N content chemical measurements of correspondence are as checking collection.
(5) pre-service of spectrum and model are set up
Pre-service carried out to the near infrared spectrum data information of calibration set in step (4) and checking collection, removes the unrelated interruptions information in spectrum, reduce random noise and strengthening bands of a spectrum feature.Choose that different preprocess methods comprises that standardization (average centralization, standardization), differentiate (Savitzky-Golay first order derivative, difference first order derivative), Savitzky-Golay are level and smooth, signal corrects that (multiplicative scatter correction MSC, standard be change of variable SNV, clean analytic signal NAS, Orthogonal Signal Correction Analyze OSC just too, trend of going corrects DT, baseline correction), and combine accordingly, TVB-N content forecast model in multiple fresh beef appetizer is set up in application partial least square method (PLS).
(6) evaluation of model
0 is leveled off to according to numerical value such as model tuning collection standard deviation (SEC), validation-cross standard deviation (SECV), checkings collection standard deviation (SEP); Calibration set related coefficient (Rc), that checking collection related coefficient (Rp) levels off to is 1 better, evaluates the performance such as forecasting accuracy, repeatability, robustness of institute's established model in step (5).Often organize after parameter sorts and get front 10 kinds of combinations, amount to 50 groups, by calibration set and each model of inspection set data importing, optimum prediction model and the best preprocess method of near infrared spectrum data information of TVB-N content in fresh beef appetizer is selected from the combination that predictablity rate is the highest, apply student's residual error to reject the exceptional value in model, Optimized model simultaneously.Table 1 ~ table 5 is the top 10 of each evaluating group.
Table 1: the comparison (sorting according to Rp value: descending) of total volatile basic nitrogen model different pretreatments method
Table 2: the comparison (sorting according to Rc value: descending) of total volatile basic nitrogen model different pretreatments method
Table 3: the comparison (sorting according to SEC value: ascending order) of total volatile basic nitrogen model different pretreatments method
Table 4: the comparison (sorting according to SECV value: ascending order) of total volatile basic nitrogen model different pretreatments method
Table 5: the comparison (sorting according to SEP value: ascending order) of total volatile basic nitrogen model different pretreatments method
By in each model of the spectroscopic data information importing table 1 ~ table 5 of 58 fresh beef appetizer samples of gathering from the market, obtain the TVB-N content predicted value of sample, detect according to the TVB-N content of microdiffusion to measuring samples of national regulations simultaneously, and sample detection result is divided into is less than 10mg/100g and be more than or equal to 10mg/100g and be less than or equal to 15mg/100g two parts, by each predicted value and chemical score are contrasted, two parts predictablity rate of Confirming model 1 is respectively 80.00% and 82.14%, model macro-forecast accuracy rate is 81.03%.Following table is the predicted value accuracy rate of each model.
Table 6: the predictablity rate of the predicted value of each model testing collection
By table 6, can show that the best preprocess method of near infrared spectrum data information is standardization, Savitzky-Golay first order derivative, trend of going correct (DT).The main cause subnumber of the optimum prediction model of TVB-N content is 13 (Fig. 4), calibration set coefficient R c=0.99, calibration set standard deviation S EC=0.47 (Fig. 5), checking collection coefficient R p=0.82, checking collection standard deviation S EP=1.63 (Fig. 6).
Best for the near infrared spectrum data information of TVB-N content in fresh beef appetizer preprocess method and optimum prediction model are imported in the system program in portable near infrared spectrometer, by the near infrared spectrum detection method set up, Fast nondestructive evaluation is carried out to the TVB-N content in fresh beef appetizer sample.Result is as shown in table 7.
Table 7: in fresh beef appetizer sample, TVB-N content predicted value and chemical measurements compares
Application in the Fast nondestructive evaluation of embodiment 2 portable near infrared spectrometer TVB-N content in fresh beef appetizer
The best near infrared spectrum data information preprocessing method of the portable near infrared spectrometer in Application Example 1 and importing and the TVB-N content of best TVB-N content forecast model to other 58 the fresh beef appetizer samples gathered from the market detect, and detect according to the TVB-N content of national regulations detection method to sample simultaneously.Result is as shown in table 8.
Table 8: in fresh beef appetizer sample, TVB-N content predicted value and chemical measurements compares
The contrast of embodiment 3 portable near infrared spectrometer forecast model in the Fast nondestructive evaluation of fresh beef appetizer and fresh mutton TVB-N content
Adopt the level and smooth and clean analytic signal (NAS) of the best preprocess method of the spectroscopic data information in the fast non-destructive detection method of TVB-N content in publication number fresh mutton disclosed in the Chinese patent application of CN103712948A and standardization, Savitzky-Golay first order derivative, Savitzky-Golay, set up fresh beef appetizer TVB-N content forecast model.Contrast with the optimal spectrum forecast model of TVB-N content in the fresh beef appetizer set up in the application, the predictablity rate of both judgements on fresh beef appetizer TVB-N content.In table 9:
Table 9: the predictablity rate of the predicted value of the two
The spectroscopic data information of 58 fresh beef appetizer samples in embodiment 2 is imported in two models of table 9 respectively, obtain the TVB-N content predicted value of sample, and sample detection result is divided into is less than 10mg/100g and be more than or equal to 10mg/100g and be less than or equal to 15mg/100g two parts, by each predicted value and chemical score are contrasted, two parts predictablity rate of Confirming model 1 is respectively 80.00% and 82.14%, and model macro-forecast accuracy rate is 79.31%; Two parts predictablity rate of Confirming model 2 is respectively 50.00% and 75.00%, and model macro-forecast accuracy rate is 62.07%.
Table 10: model 1 and model 2 pairs of TVB-N content predicted values compare with chemical measurements
Contrasted by above two model predication values and chemical measurements, obviously can find out the best preprocess method of the spectroscopic data information of establishing in the fresh beef appetizer TVB-N content fast non-destructive detection method of the application and optimum prediction model reliability in actual applications and robustness, predictablity rate is higher, is applicable to on-line checkingi and repeatability is good.
Above with a general description of the specific embodiments detailed description has been done to the present invention, but on basis of the present invention, can carry out some amendments according to actual conditions or improve, this it will be apparent to those skilled in the art that.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (7)
1. the fast non-destructive detection method of TVB-N content in fresh beef appetizer, comprises the following steps:
1) batch capture fresh beef appetizer sample, gathers the near infrared spectrum data information of described sample, and detects the TVB-N content of described sample;
2) by step 1) described in the chemical measurements of near infrared spectrum data information and described TVB-N content mutually corresponding and set up sample sets, be divided into calibration set and checking collection in proportion, after carrying out different Pretreated spectra to the near infrared spectrum data information of described sample, the near infrared spectrum data information of described calibration set and TVB-N content chemical measurements is used to set up the forecast model of TVB-N content in fresh beef appetizer; The near infrared spectrum data information of described checking collection, TVB-N content chemical measurements and model parameter is utilized to carry out the precision of valuation prediction models; By the model predication value of described inspection set and the contrast of chemical score, select the model that in fresh beef appetizer, TVB-N content predictablity rate is the highest, determine the best preprocess method of near infrared spectrum data information for TVB-N content in fresh beef appetizer and optimum prediction model;
3) utilize step 2) in the best near infrared spectrum data information preprocessing method of TVB-N content and optimum prediction model in fixed fresh beef appetizer, detect the TVB-N content of fresh beef appetizer sample to be measured.
2. detection method according to claim 1, it is characterized in that, step 2) in comprise calibration set standard deviation, validation-cross standard deviation, checking collection standard deviation, calibration set related coefficient or checking collection related coefficient for the precision evaluating of the optimum prediction model of TVB-N content in fresh beef appetizer, and determine model to be selected by the sequence of each group of parameter, inspection set is imported model to be selected to the model determining that in each model to be checked, in fresh beef appetizer, TVB-N content predictablity rate is the highest.
3. detection method according to claim 1 and 2, is characterized in that, step 1) near infrared spectrum data information acquisition use carried out to sample spectral range be 1000nm ~ 1800nm.
4. detection method according to claim 3, is characterized in that, step 1) in the TVB-N content of chemical detection method to sample that specify according to standard GB/T/T 5009.44-2003 detect.
5. detection method according to claim 4, it is characterized in that, step 2) in comprise for the near infrared spectrum data information preprocessing method of TVB-N content in fresh beef appetizer that average centralization, standardization, Savitzky-Golay first order derivative, difference first order derivative, Savitzky-Golay are level and smooth, multiplicative scatter correction MSC, standard just too change of variable SNV, clean analytic signal NAS, Orthogonal Signal Correction Analyze OSC, trend of going corrects at least one in DT and baseline correction method.
6. detection method according to claim 5, is characterized in that, step 2) in calibration set and verify that the ratio that integrates is as 2-3:1, preferred 3:1.
7. the detection method according to any one of claim 4-6, is characterized in that, step 1)-3) in, utilize portable near infrared spectrometer to carry out Fast nondestructive evaluation to the content of total volatile basic nitrogen in fresh beef appetizer.
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| CN114112989A (en) * | 2021-12-03 | 2022-03-01 | 四川启睿克科技有限公司 | Near-infrared detection method and system based on composite vision |
| CN114264630A (en) * | 2021-12-31 | 2022-04-01 | 内蒙古自治区农畜产品质量安全中心 | Establishment method and application of database for rapidly detecting mutton volatile basic nitrogen based on near infrared |
| CN114371144A (en) * | 2021-12-31 | 2022-04-19 | 中国农业科学院草原研究所 | Establishment method and application of database for detecting mutton biogenic amine content based on near infrared spectrum imaging technology |
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