CN104990877A - Method for detecting irradiation dose of shrimp and shellfish peeled aquatic products on basis of multi-spectral imaging technology - Google Patents
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Abstract
本发明公开了一种基于多光谱成像技术测定虾贝类去壳水产品辐照剂量的方法,该方法通过对虾贝类去壳水产品进行不同剂量辐照处理,应用多光谱成像系统采集虾贝类去壳水产品的光谱图像,结合化学计量学方法建立虾贝类去壳水产品辐照剂量的模型,从而实现对虾贝类去壳水产品辐照剂量的快速无损检测。该方法具有操作简单、分析速度快、测试重现性好、样品无需预处理等优点,有效的测定虾贝类去壳水产品辐照剂量。此方法有助于提高辐照虾贝类去壳水产品的质量控制和真伪鉴别水平,将进一步推动辐照虾贝类去壳水产品的国际贸易。
The invention discloses a method for measuring the irradiation dose of shelled shrimp and shellfish aquatic products based on multi-spectral imaging technology. In the method, the shelled shrimp and shellfish aquatic products are irradiated with different doses, and the shrimp and shellfish are collected by using a multi-spectral imaging system. The spectral images of shell-like aquatic products were combined with chemometrics to establish a model of the radiation dose of shelled shrimp and shellfish, so as to realize the rapid non-destructive detection of the radiation dose of shelled shrimp and shellfish. The method has the advantages of simple operation, fast analysis speed, good test reproducibility, no pretreatment of samples, etc., and can effectively determine the irradiation dose of shelled shrimp and shellfish aquatic products. This method helps to improve the quality control and authenticity identification level of irradiated shelled shrimp and shellfish aquatic products, and will further promote the international trade of irradiated shelled shrimp and shellfish aquatic products.
Description
技术领域technical field
本发明涉及的是一种农产品质量与安全的分析方法,尤其涉及的是一种测定虾贝类去壳水产品辐照剂量的技术方法,具体地说是一种基于多光谱成像技术的虾贝类去壳水产品辐照剂量的检测方法。The present invention relates to an analysis method for the quality and safety of agricultural products, in particular to a technical method for measuring the radiation dose of shelled shrimp and shellfish, specifically a method for measuring the radiation dose of shelled shrimp and shellfish based on multi-spectral imaging technology. Test method for radiation dose of shell-like aquatic products.
背景技术Background technique
近年来,辐照技术已广泛应用于食品行业,其主要目的是灭菌、杀虫和抑制植物发芽。由于辐照处理后可降低产品产后损耗、延长产品货架寿命等方面的优势,已被越来越多的国家所认可。一些国际权威机构以及各国相关部门都对食品辐照制定标准,且要求对辐照食品明确标识。然而,目前国内有很多经过辐照处理的水产品未明确标明,并且有部分企业一味的追求利益随意加大辐照剂量,不仅会破坏产品的营养成分,而且可能会影响食用安全性;同时国际上也把辐照技术作为国际贸易壁垒的重要手段。这些问题未能有效的解决,其凸显出当下缺乏简单、系统、可行的产品辐照剂量检测方法,严重影响了辐照食品的国际贸易。In recent years, irradiation technology has been widely used in the food industry, and its main purpose is to sterilize, kill insects and inhibit plant germination. Due to the advantages of reducing post-production loss and prolonging product shelf life after irradiation treatment, it has been recognized by more and more countries. Some international authoritative organizations and relevant departments of various countries have set standards for food irradiation and require clear labeling of irradiated food. However, at present, there are many irradiated aquatic products in China that are not clearly marked, and some enterprises blindly pursue profits and increase the irradiation dose at will, which will not only destroy the nutritional content of the products, but may also affect the food safety; at the same time, the international Radiation technology is also regarded as an important means of international trade barriers. These problems have not been effectively resolved, which highlights the lack of a simple, systematic and feasible product radiation dose detection method, which seriously affects the international trade of irradiated food.
目前辐照剂量常用的一些有效检测方法和手段,主要为热释光分析法、电子自旋共振光谱检测法(ESR)、高效液相色谱法、色质联用法(GC-MS和LC-MS)、DNA裂解产物检测法、激光成像检测法等。但是上述方法耗时,操作复杂,并且不适用于在线快速无损检测。因而,在检测虾贝类去壳水产品辐照剂量的检测中,迫切需要一种快速、准确、简便的方法。而多光谱成像技术具有量化、无损、实时监控的特点,非常适合水产品辐照剂量的快速检测。国内外还未见有关应用多光谱成像技术快速检测虾贝类去壳水产品辐照剂量的相关文章报道。At present, some effective detection methods and means commonly used for radiation dose are mainly thermoluminescence analysis, electron spin resonance spectroscopy (ESR), high performance liquid chromatography, and chromatography-mass spectrometry (GC-MS and LC-MS). ), DNA cleavage product detection method, laser imaging detection method, etc. However, the above methods are time-consuming and complicated to operate, and are not suitable for fast online non-destructive testing. Therefore, there is an urgent need for a fast, accurate and simple method in the detection of radiation dose of shrimp and shellfish peeled aquatic products. The multi-spectral imaging technology has the characteristics of quantification, non-destructive and real-time monitoring, which is very suitable for the rapid detection of the radiation dose of aquatic products. At home and abroad, there are no related articles and reports on the application of multispectral imaging technology to quickly detect the radiation dose of shelled shrimp and shellfish.
发明内容Contents of the invention
本发明的目的在于克服现有技术的不足,提供了一种基于多光谱成像技术的虾贝类去壳水产品辐照剂量的检测方法,为虾贝类去壳水产品的辐照剂量测定提供了一种快速无损检测的方法,其结果准确。The purpose of the present invention is to overcome the deficiencies of the prior art, to provide a method for detecting the radiation dose of shelled shrimp and shellfish aquatic products based on multi-spectral imaging technology, and to provide radiation dose measurement for shelled shrimp and shellfish aquatic products. A fast non-destructive testing method was developed with accurate results.
本发明是通过以下技术方案实现的:The present invention is achieved through the following technical solutions:
(1)、原料的选取与预处理(1) Selection and pretreatment of raw materials
取同一批次的虾贝类去壳水产品,进行不同剂量的辐照处理,并将处理后的样品的一部分作为校正集,另一部分作为预测集;Take the same batch of shrimp and shellfish peeled aquatic products, and carry out irradiation treatment with different doses, and use a part of the processed samples as a calibration set, and another part as a prediction set;
(2)、获取光谱图像:利用多光谱成像系统对所有样品进行扫描获的光谱图信息,其扫描光谱范围为400‐1000nm;(2) Obtain spectral images: use the multi-spectral imaging system to scan the spectral information of all samples, and the scanning spectral range is 400-1000nm;
(3)、结合化学计量学方法建立虾贝类去壳水产品辐照剂量定量分析模型;(3) Combining chemometric methods to establish a quantitative analysis model for radiation dose of shelled shrimp and shellfish;
具体为:Specifically:
1)设定校正集样品辐照剂量值为建模实际值;1) Set the calibration set sample irradiation dose value as the actual value of the modeling;
2)校正集样品的光谱波长与其实际值经过数据分析,结合化学计量学方法建立模型;2) The spectral wavelength of the sample in the calibration set and its actual value are analyzed through data analysis, and a model is established in combination with chemometric methods;
3)根据建立的模型,对预测集样品的辐照剂量值进行预测,光谱预测得到样品的辐照剂量值,并分析其与虾贝类去壳水产品辐照剂量实际值的差异,选取预测精度达到要求的虾贝类去壳水产品辐照剂量的模型,利用此模型能够实现对虾贝类去壳水产品辐照剂量快速无损检测。3) According to the established model, predict the radiation dose value of the prediction set samples, obtain the radiation dose value of the sample through spectral prediction, and analyze the difference between it and the actual radiation dose value of shelled shrimp and shellfish aquatic products, select the predicted value The model of irradiation dose of shelled shrimp and shellfish with the required precision can be used to realize rapid and non-destructive detection of radiation dose of shelled shrimp and shellfish.
所述步骤(1)中样品分别经过不同强度辐照电子束辐照。In the step (1), the samples are respectively irradiated with electron beams of different intensities.
所述步骤(2)中,利用Videometer Lab多光谱成像系统对所有样品进行多光谱扫描,具体为:先利用定标板对多光谱成像系统进行校准,再进行多光谱扫描。In the step (2), use the Videometer Lab multispectral imaging system to perform multispectral scanning on all samples, specifically: first use the calibration plate to calibrate the multispectral imaging system, and then perform multispectral scanning.
所述步骤2)中,采用偏最小二乘法,通过计算机建立模型。In said step 2), a partial least square method is used to establish a model by computer.
所述的检测方法可以用于设计、建立一套光谱无损快速检测虾贝类去壳水产品辐照剂量的自动检测和分析装置,并能在此基础上将该装置应用扩展到虾贝类去壳水产品质量安全的分析装置。The detection method described can be used to design and establish a set of automatic detection and analysis device for non-destructive and rapid detection of radiation dose of shrimp and shellfish peeled aquatic products, and on this basis, the application of the device can be extended to shrimp and shellfish. An analysis device for the quality and safety of shellfish products.
本发明相比现有技术具有以下优点:本发明提供了一种基于多光谱成像技术的虾贝类去壳水产品辐照剂量的检测方法,该方法是基于多光谱成像技术的虾贝类去壳水产品辐照剂量快速检测方法,为测定虾贝类去壳水产品辐照剂量提供了一种快速、无损、准确的方法。Compared with the prior art, the present invention has the following advantages: the present invention provides a method for detecting the irradiation dose of shelled shrimp and shellfish aquatic products based on multispectral imaging technology. The rapid detection method of radiation dose of shelled aquatic products provides a fast, non-destructive and accurate method for determining the radiation dose of shelled shrimp and shellfish.
附图说明Description of drawings
图1为不同辐照剂量处理去皮虾在波长范围为400‐1000nm的平均反射光谱图;Fig. 1 is the average reflectance spectrum figure of 400-1000nm wavelength range for different irradiation doses of peeled shrimp;
图2为校正集样品实际值和预测值的关系散点图;Figure 2 is a scatter diagram of the relationship between the actual value and the predicted value of the calibration set sample;
图3为预测集样品实际值和预测值的关系散点图。Figure 3 is a scatter diagram of the relationship between the actual value and the predicted value of the samples in the prediction set.
具体实施方式Detailed ways
下面对本发明的实施例作详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。The embodiments of the present invention are described in detail below. This embodiment is implemented on the premise of the technical solution of the present invention, and detailed implementation methods and specific operating procedures are provided, but the protection scope of the present invention is not limited to the following implementation example.
实施例1Example 1
本实施例提供了一种基于多光谱成像技术的虾贝类去壳水产品辐射剂量的检测方法,包括以下步骤:This embodiment provides a method for detecting the radiation dose of shelled shrimp and shellfish aquatic products based on multispectral imaging technology, including the following steps:
(1)原料的选取与预处理(1) Selection and pretreatment of raw materials
取同一批次的冷冻去皮虾5袋,每袋2.5kg;选取的样品分别经过0、1、4、10和20kGy辐照电子束辐照(通常出口美国的辐照强度为3.5~4.5kGy,公认的安全辐照强度最高为20kGy);处理过的样品随机划分校正集和预测集,本实施例中,选取校正集样品数量为50只,预测集样品数量为50只。Take 5 bags of frozen peeled shrimp from the same batch, each bag is 2.5kg; the selected samples are irradiated by electron beams at 0, 1, 4, 10 and 20kGy (usually the irradiation intensity for export to the United States is 3.5-4.5kGy) , the highest recognized safe radiation intensity is 20kGy); the processed samples are randomly divided into a calibration set and a prediction set. In this embodiment, the number of samples in the calibration set is 50, and the number of samples in the prediction set is 50.
(2)获取光谱图像(2) Obtain spectral image
光谱测定采用Videometer Lab多光谱成像系统(Videometer A/S,丹麦),其光谱范围为405‐970nm。具体为:先利用定标板(白板、黑板和几何点板)对多光谱成像系统进行校准,再对步骤(1)解冻后的校正集和预测集去皮虾进行多光谱扫描,获得原始光谱图像;The spectra were measured using the Videometer Lab multispectral imaging system (Videometer A/S, Denmark), its spectral range is 405‐970nm. The details are as follows: firstly use the calibration board (whiteboard, blackboard and geometric point board) to calibrate the multispectral imaging system, and then perform multispectral scanning on the calibration set and prediction set after step (1) thawed to obtain the original spectrum image;
(3)采用偏最小二乘法PLS建立虾贝类去壳水产品辐照剂量定量分析模型(3) Using the partial least squares method PLS to establish a quantitative analysis model for the radiation dose of shelled shrimp and shellfish
1)设定样品辐照剂量值为建模实际值;1) Set the sample irradiation dose value as the actual modeled value;
2)对校正集样品的光谱波长与样品建模实际值进行偏最小二乘PLS回归,建立分析模型,具体为:2) Partial least squares PLS regression is performed on the spectral wavelength of the calibration set sample and the actual value of the sample modeling, and the analysis model is established, specifically:
步骤一:将处理后光谱图像的光谱矩阵X和浓度矩阵Y进行分解,其模型为:Step 1: Decompose the spectral matrix X and concentration matrix Y of the processed spectral image, and its model is:
X=TP+EX=TP+E
Y=UQ+FY=UQ+F
上式中:U和T分别为Y和X的得分矩阵,Q和P分别为Y和X的载荷阵,F和E分别为PLS模型拟合Y和X时带入的误差。In the above formula: U and T are the scoring matrices of Y and X, respectively, Q and P are the load matrices of Y and X, respectively, and F and E are the errors brought in when the PLS model fits Y and X, respectively.
步骤二:将T和U作线性回归:Step 2: Perform linear regression on T and U:
U=TBU=TB
B=(TTT)-1TTYB=(T T T) -1 T T Y
步骤三:根据上述步骤一中的分解模型以及获得的P值,计算待测样品的光谱矩阵Xpre的得分Tpre,然后求得浓度预测值Ypre,即为预测样品的辐照剂量值:Step 3: Calculate the score T pre of the spectral matrix X pre of the sample to be tested according to the decomposition model in the above step 1 and the obtained P value, and then obtain the predicted concentration value Y pre , which is the radiation dose value of the predicted sample:
Ypre=TpreBQY pre =T pre BQ
如图2所示,为建立模型的校正集样品实际值和预测值的关系散点图。As shown in Figure 2, it is a scatter diagram of the relationship between the actual value and the predicted value of the calibration set sample for the establishment of the model.
3)根据校正集样品建立的分析模型,计算预测集的辐照剂量值:3) Calculate the radiation dose value of the prediction set according to the analysis model established by the calibration set samples:
利用建立的判别模型,对预测集样品进行预测,获得如下表1所示的实际值与预测值的比较结果和如图3所示的关系散点图:Use the established discriminant model to predict the samples in the prediction set, and obtain the comparison results between the actual value and the predicted value as shown in Table 1 below and the relationship scatter diagram shown in Figure 3:
表1:预测集样品的实际值与预测值的比较结果Table 1: Comparison results of the actual and predicted values of samples in the prediction set
利用相关系数R、均方根误差SEC和预测均方根误差SEP作为评价模型精度的有效指标,其中,R越高,SEC和SEP越小,模型的精度越高:The correlation coefficient R, the root mean square error SEC and the predicted root mean square error SEP are used as effective indicators for evaluating the accuracy of the model. The higher the R, the smaller the SEC and SEP, and the higher the accuracy of the model:
式中,R为相关系数,n表示样品数,yi和分别为样品集中第i个样品的实测值和预测值,包括校正集和预测集;为样品集中第i个样品的实测值的平均值;In the formula, R is the correlation coefficient, n is the number of samples, y i and are the measured value and predicted value of the i-th sample in the sample set, including the calibration set and prediction set; is the average value of the measured values of the i-th sample in the sample set;
式中:yi和分别为样品集中第i个样品的实测值和预测值;N为校正集样品数,n为预测集样品数,P为主成分数;In the formula: y i and are the measured value and predicted value of the i-th sample in the sample set, respectively; N is the number of samples in the calibration set, n is the number of samples in the prediction set, and P is the number of principal components;
通过对50个校正集样品的预测,并与其实际值做比较,结果发现,预测集中,R值为0.9778,SEP为1.7845,说明验证模型的预测效果良好。Through the prediction of 50 calibration set samples and comparing with their actual values, it was found that in the prediction set, the R value was 0.9778 and the SEP was 1.7845, which indicated that the prediction effect of the verification model was good.
(4)待测样品辐照剂量的检测(4) Detection of the irradiation dose of the sample to be tested
取待测样品,解冻后利用Videometer Lab多光谱成像系统进行多光谱扫描,获得原始光谱图像;Take the sample to be tested, and use the Videometer Lab multispectral imaging system to perform multispectral scanning after thawing to obtain the original spectral image;
根据上述建立的模型,计算待测待测样品的光谱矩阵Xpre的得分Tpre,然后求得浓度预测值Ypre,即为待测样品的辐照剂量值。According to the model established above, the score T pre of the spectral matrix X pre of the sample to be tested is calculated, and then the predicted concentration value Y pre is obtained, which is the radiation dose value of the sample to be tested.
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