CN108444946A - A kind of Practice for Pesticide Residue in Agricultural Products detection method and device - Google Patents
A kind of Practice for Pesticide Residue in Agricultural Products detection method and device Download PDFInfo
- Publication number
- CN108444946A CN108444946A CN201810443765.0A CN201810443765A CN108444946A CN 108444946 A CN108444946 A CN 108444946A CN 201810443765 A CN201810443765 A CN 201810443765A CN 108444946 A CN108444946 A CN 108444946A
- Authority
- CN
- China
- Prior art keywords
- pesticide
- agricultural products
- sample
- spectrum
- detection
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
本发明公开了一种农产品农药残留检测方法，包括以下步骤：步骤(1)建立检测模型；(1.1)制备样品：(1.2)采集光谱数据；(1.3)建立检测模型；步骤(2)检测待测农产品光谱：(2.1)制备样品：(2.2)样品处理：取上述制得的溶质溶于75ml酒精溶液中；(2.3)采集光谱数据：获取溶入酒精的溶质液的近红外透射光谱；步骤(3)判断农产品中农药成分及含量；对比步骤(2.3)获取溶入酒精溶质液的近红外透射光谱与步骤(1.3)得到的光谱与农药含量检测模型对比。本发明实现了对农药的种类及其含量的精准检测，更因检测装置的完善使得样品制备得到精细化处理，极大提高了农药分子的选择透过性，进而提高了测量的精度，满足实际使用要求。
The invention discloses a method for detecting pesticide residues in agricultural products, which comprises the following steps: step (1) establishing a detection model; (1.1) preparing a sample: (1.2) collecting spectral data; (1.3) establishing a detection model; Measure the spectrum of agricultural products: (2.1) prepare the sample: (2.2) sample treatment: get the solute prepared above and dissolve it in 75ml alcohol solution; (2.3) collect spectral data: obtain the near-infrared transmission spectrum of the solute liquid dissolved in alcohol; (3) Determine the pesticide composition and content in agricultural products; compare the near-infrared transmission spectrum obtained in step (2.3) with the spectrum obtained in step (1.3) and the pesticide content detection model. The present invention realizes the precise detection of the types and contents of pesticides, and the refinement of sample preparation due to the improvement of the detection device greatly improves the selective permeability of pesticide molecules, thereby improving the accuracy of measurement and meeting the actual requirements. Requirements.
Description
技术领域technical field
本发明涉及一种农产品农药残留检测方法及装置，属于农产品检测技 术领域。The invention relates to a method and device for detecting pesticide residues in agricultural products, belonging to the technical field of agricultural product detection.
背景技术Background technique
目前，农药残留的常规检测方法有：薄层色谱法、气相色谱法、高效 液相色谱法、超临界流体色谱法等等。其中，仪器分析检测法精度最高， 但其检测过程复杂、检测时间长，生化检测技术发展迅速，但前期投入大、 实验条件苛刻，也缺乏一套完整的检测装置。发明专利(微量农药的快速 检测方法)，申请号：200910236834.1，公开了一种基于红外透射光谱的农 药检测方法，具有操作简单、检测速度快的优势，然后这种方式采用滤纸 样品，透过性不好，因此该方法灵敏度差、测量精度不高。为此，需要研 究一种新的技术方案给予解决。At present, the routine detection methods of pesticide residues include: thin layer chromatography, gas chromatography, high performance liquid chromatography, supercritical fluid chromatography and so on. Among them, the instrumental analysis detection method has the highest accuracy, but its detection process is complicated and the detection time is long. The biochemical detection technology has developed rapidly, but the initial investment is large, the experimental conditions are harsh, and a complete detection device is lacking. Invention patent (rapid detection method for trace pesticides), application number: 200910236834.1, which discloses a pesticide detection method based on infrared transmission spectroscopy, which has the advantages of simple operation and fast detection speed. Not good, so the method has poor sensitivity and low measurement accuracy. For this reason, need to study a kind of new technical scheme to give solution.
发明内容Contents of the invention
本发明正是针对现有技术存在的不足，提供一种农产品农药残留检测 方法及装置，实现了对农药的种类及其含量的精准检测，更因检测装置的 完善使得样品制备得到精细化处理，极大提高了农药分子的选择透过性， 进而提高了测量的精度，满足实际使用要求。The present invention is aimed at the deficiencies of the existing technology, and provides a method and device for detecting pesticide residues in agricultural products, which realizes the precise detection of the type and content of pesticides, and the refinement of sample preparation due to the improvement of the detection device. The selective permeability of pesticide molecules is greatly improved, thereby improving the accuracy of measurement and meeting the requirements of actual use.
为解决上述问题，本发明所采取的技术方案如下：In order to solve the above problems, the technical scheme adopted in the present invention is as follows:
一种农产品农药残留检测方法，包括以下步骤：A method for detecting pesticide residues in agricultural products, comprising the following steps:
步骤(1)建立检测模型Step (1) Build a detection model
(1.1)制备样品：将能够溶于蒸馏水的农药与蒸馏水进行混合，农药 与蒸馏水的质量比选择成等差数列的多个比例关系；(1.1) Sample preparation: mix the pesticides that can be dissolved in distilled water with distilled water, and the mass ratio of pesticides and distilled water is selected as a plurality of proportional relationships of arithmetic progression;
(1.2)采集光谱数据：获取农药水溶液近红外透射光谱；(1.2) Collect spectral data: obtain the near-infrared transmission spectrum of the pesticide aqueous solution;
(1.3)建立检测模型：根据农药与蒸馏水的比例，以及所对应的农药 水溶液近红外透射光谱，在二维坐标系中建立光谱与农药含量检测模型；(1.3) Establish a detection model: according to the ratio of pesticide and distilled water, and the corresponding pesticide aqueous solution near-infrared transmission spectrum, set up a spectrum and pesticide content detection model in a two-dimensional coordinate system;
步骤(2)检测待测农产品光谱Step (2) detect the spectrum of the agricultural product to be tested
(2.1)制备样品：(2.1) Preparation of samples:
将待测农产品清洗干净，然后置于检测装置的真空室内，通过真空泵 实现气压差对待测农产品进行压缩液获取，再通过调节管一、二内装有的 无水硫酸钠、有机溶剂乙酸乙酯及活性炭，对压缩液进行调节、过滤；Clean the agricultural products to be tested, and then place them in the vacuum chamber of the detection device. The compressed liquid of the agricultural products to be tested is obtained through the vacuum pump to realize the air pressure difference, and then through the anhydrous sodium sulfate, organic solvent ethyl acetate and Activated carbon, to adjust and filter the compressed liquid;
(2.2)电极诱导：将上述压缩滤液置入等离子体装置的下电极介质上， 电压2.2kV，电流1.2mA、间隙3.2mm的操作条件下照射3-5秒；(2.2) Electrode induction: put the above-mentioned compressed filtrate on the lower electrode medium of the plasma device, and irradiate for 3-5 seconds under the operating conditions of voltage 2.2kV, current 1.2mA, and gap 3.2mm;
(2.3)浓缩：将上述压缩滤液置于温度为65-75度的盐浴池中加热， 待压缩滤液中的溶剂蒸发干净，留下溶质；(2.3) Concentration: the above-mentioned compressed filtrate is placed in a salt bath with a temperature of 65-75 degrees and heated, and the solvent in the compressed filtrate is evaporated to leave the solute;
(2.4)样品处理：取上述制得的溶质溶于75ml酒精溶液中，振荡均匀；(2.4) Sample treatment: Take the above-mentioned solute and dissolve it in 75ml alcohol solution, shake evenly;
(2.5)采集光谱数据：获取溶入酒精的溶质液的近红外透射光谱；(2.5) Collect spectral data: obtain the near-infrared transmission spectrum of the solute solution dissolved in alcohol;
步骤(3)、判断农产品中农药成分及含量Step (3), judging the composition and content of pesticides in agricultural products
对比步骤(2.5)获取溶入酒精的溶质液的近红外透射光谱与步骤(1.3) 得到的光谱与农药含量检测模型，获取农产品农药成分及含量。Compare the near-infrared transmission spectrum obtained in step (2.5) of the solute solution dissolved in alcohol with the spectrum obtained in step (1.3) and the detection model of pesticide content to obtain the pesticide composition and content of agricultural products.
作为上述技术方案的改进，所述光谱与所述农药含量检测模型为二维 曲线形式，不同的农药绘制不同的二维曲线。As an improvement of the above technical solution, the spectrum and the pesticide content detection model are in the form of two-dimensional curves, and different pesticides draw different two-dimensional curves.
作为上述技术方案的改进，所述二维曲线中相邻的两点为线性连接， 所述二维曲线通过多阶函数拟合方法获得。As an improvement of the above technical solution, two adjacent points in the two-dimensional curve are linearly connected, and the two-dimensional curve is obtained by a multi-order function fitting method.
作为上述技术方案的改进，所述机构本体顶部设有隔层，所述隔层下 方设有真空室，所述隔层内设有配合真空室使用的真空泵，所述真空室下 方设有样品调节池，所述机构本体两侧设有配合样品调节池使用的调节管 一和调节管二，所述样品调节池下方设有电极诱导装置、储样试管及盐浴 池，所述储样试管设置在电极诱导装置上，所述储样试管底部设置在盐浴 池内；所述农产品农药残留检测装置还包括对储样试管内溶入酒精的溶质 液进行检测的光谱农药残留检测仪，所述机构本体外层设有配合光谱农药 残留检测仪使用的对比分析机构。As an improvement of the above technical solution, a partition is provided on the top of the mechanism body, a vacuum chamber is provided below the partition, a vacuum pump used in conjunction with the vacuum chamber is provided inside the partition, and a sample adjustment chamber is provided below the vacuum chamber. pool, both sides of the body of the mechanism are provided with adjustment tube 1 and tube 2 for use with the sample adjustment pool, and an electrode induction device, a storage test tube and a salt bath are arranged below the sample adjustment pool, and the storage test tube is set at On the electrode induction device, the bottom of the sample storage test tube is set in a salt bath; the agricultural product pesticide residue detection device also includes a spectral pesticide residue detector for detecting the solute solution dissolved in alcohol in the sample storage test tube, and the mechanism body The outer layer is equipped with a comparative analysis mechanism used in conjunction with the spectral pesticide residue detector.
作为上述技术方案的改进，所述真空室顶部设有阀门和排气阀，所述 真空室内设有配合使用的夹持机构，所述真空室底部设有倒液口，所述倒 液口上设有倒液载体，所述倒液载体为互相叠加的滤纸和纤维素膜。As an improvement of the above technical solution, a valve and an exhaust valve are provided on the top of the vacuum chamber, a clamping mechanism is provided in the vacuum chamber, a liquid pouring port is provided at the bottom of the vacuum chamber, and a liquid pouring port is provided on the liquid pouring port. There is a liquid pouring carrier, which is filter paper and cellulose membrane stacked on top of each other.
作为上述技术方案的改进，所述调节管一和调节管二上均设有与样品 调节池相连通的导管，所述导管上设有调节阀，所述样品调节池底部设有 过滤层和配合所述储样试管使用的导向管。As an improvement of the above-mentioned technical scheme, both the regulating pipe 1 and the regulating pipe 2 are provided with conduits communicating with the sample regulating pool, the conduits are provided with regulating valves, and the bottom of the sample regulating pond is provided with a filter layer and a matching The guide tube used in the sample storage tube.
作为上述技术方案的改进，所述电极诱导装置包括等离子体装置的下 电极介质，所述等离子体装置的下电极介质的为电压2.2kV，电流为1.2mA、 间隙为3.2mm。As an improvement of the above technical solution, the electrode induction device includes a lower electrode medium of the plasma device, the voltage of the lower electrode medium of the plasma device is 2.2kV, the current is 1.2mA, and the gap is 3.2mm.
本发明与现有技术相比较，本发明的实施效果如下：The present invention compares with prior art, and implementation effect of the present invention is as follows:
本发明所述农产品农药残留检测方法，首先建立检测模型，然后通过 检测装置对待检测样品的精细化处理、改善待检测样品的分子选择透过性， 进而提高了对待检测样品进行光谱检测的精准度及精确的判断出农产品中 农药成分及含量(不仅可以通过光谱检测出农药的种类，还可以根据吸收 的强弱判断农药的含量)，即通过与检测模型的对比得到其含量，检测效果 好、效率高，满足实际检测需求。The method for detecting pesticide residues in agricultural products of the present invention firstly establishes a detection model, and then refines the sample to be detected through the detection device to improve the molecular selective permeability of the sample to be detected, thereby improving the accuracy of spectral detection of the sample to be detected And accurately determine the pesticide composition and content in agricultural products (not only the type of pesticide can be detected by spectrum, but also the content of pesticide can be judged according to the strength of absorption), that is, its content can be obtained by comparing with the detection model, and the detection effect is good. High efficiency, to meet the actual detection needs.
此外，检测装置的结构设计合理、操作简单、易行，方便对待测农产 品的的精细化处理，极大改善待检测样品的分子选择透过性，方便了对农 产品农药残留量的检测，其中，电极诱导处后的分子具有选择透过性极强 的特性，灵敏度好、进一步提高了检测精度。In addition, the detection device has a reasonable structural design, simple operation, and is easy to operate, which is convenient for the refined treatment of the agricultural products to be tested, greatly improves the molecular selective permeability of the samples to be tested, and facilitates the detection of pesticide residues in agricultural products. Among them, The molecules behind the electrode induction have the characteristics of strong selective permeability, good sensitivity, and further improve the detection accuracy.
附图说明Description of drawings
图1为本发明所述检测装置结构示意图。Fig. 1 is a schematic structural diagram of the detection device of the present invention.
具体实施方式Detailed ways
下面将结合具体的实施例来说明本发明的内容。The content of the present invention will be described below in conjunction with specific embodiments.
实施例1Example 1
一种农产品农药残留检测方法，包括以下步骤：A method for detecting pesticide residues in agricultural products, comprising the following steps:
步骤(1)建立检测模型Step (1) Build a detection model
(1.1)制备样品：将能够溶于蒸馏水的农药与蒸馏水进行混合，农药 与蒸馏水的质量比选择成等差数列的多个比例关系；(1.1) Sample preparation: mix the pesticides that can be dissolved in distilled water with distilled water, and the mass ratio of pesticides and distilled water is selected as a plurality of proportional relationships of arithmetic progression;
(1.2)采集光谱数据：获取农药水溶液近红外透射光谱；(1.2) Collect spectral data: obtain the near-infrared transmission spectrum of the pesticide aqueous solution;
(1.3)建立检测模型：根据农药与蒸馏水的比例，以及所对应的农药 水溶液近红外透射光谱，在二维坐标系中建立光谱与农药含量检测模型；(1.3) Establish a detection model: according to the ratio of pesticide and distilled water, and the corresponding pesticide aqueous solution near-infrared transmission spectrum, set up a spectrum and pesticide content detection model in a two-dimensional coordinate system;
步骤(2)检测待测农产品光谱Step (2) detect the spectrum of the agricultural product to be tested
(2.1)制备样品：(2.1) Preparation of samples:
将待测农产品清洗干净，然后置于检测装置的真空室内，通过真空泵 实现气压差对待测农产品进行压缩液获取，再通过调节管一、二内装有的 无水硫酸钠、有机溶剂乙酸乙酯及活性炭，对压缩液进行调节、过滤；Clean the agricultural products to be tested, and then place them in the vacuum chamber of the detection device. The compressed liquid of the agricultural products to be tested is obtained through the vacuum pump to realize the air pressure difference, and then through the anhydrous sodium sulfate, organic solvent ethyl acetate and Activated carbon, to adjust and filter the compressed liquid;
(2.2)电极诱导：将上述压缩滤液置入等离子体装置的下电极介质上， 电压2.2kV，电流1.2mA、间隙3.2mm的操作条件下照射3-5秒；(2.2) Electrode induction: put the above-mentioned compressed filtrate on the lower electrode medium of the plasma device, and irradiate for 3-5 seconds under the operating conditions of voltage 2.2kV, current 1.2mA, and gap 3.2mm;
(2.3)浓缩：将上述压缩滤液置于温度为65-75度的盐浴池中加热， 待压缩滤液中的溶剂蒸发干净，留下溶质；(2.3) Concentration: the above-mentioned compressed filtrate is placed in a salt bath with a temperature of 65-75 degrees and heated, and the solvent in the compressed filtrate is evaporated to leave the solute;
(2.4)样品处理：取上述制得的溶质溶于75ml酒精溶液中，振荡均匀；(2.4) Sample treatment: Take the above-mentioned solute and dissolve it in 75ml alcohol solution, shake evenly;
(2.5)采集光谱数据：获取溶入酒精的溶质液的近红外透射光谱；(2.5) Collect spectral data: obtain the near-infrared transmission spectrum of the solute solution dissolved in alcohol;
步骤(3)、判断农产品中农药成分及含量Step (3), judging the composition and content of pesticides in agricultural products
对比步骤(2.5)获取溶入酒精的溶质液的近红外透射光谱与步骤(1.3) 得到的光谱与农药含量检测模型，获取农产品农药成分及含量。Compare the near-infrared transmission spectrum obtained in step (2.5) of the solute solution dissolved in alcohol with the spectrum obtained in step (1.3) and the detection model of pesticide content to obtain the pesticide composition and content of agricultural products.
具体地，所述光谱与所述农药含量检测模型为二维曲线形式，不同的 农药绘制不同的二维曲线；所述二维曲线中相邻的两点为线性连接，所述 二维曲线通过多阶函数拟合方法获得。Specifically, the spectrum and the pesticide content detection model are in the form of a two-dimensional curve, and different pesticides draw different two-dimensional curves; two adjacent points in the two-dimensional curve are connected linearly, and the two-dimensional curve passes through Obtained by multi-order function fitting method.
其中，所述农产品农药残留检测装置，包括机构本体100，机构本体 100顶部设有隔层10，所述隔层10下方设有真空室20，所述隔层10内设 有配合真空室20使用的真空泵11，所述真空室20下方设有样品调节池30， 所述机构本体100两侧设有配合样品调节池30使用的调节管一41和调节 管二42，所述样品调节池30下方设有电极诱导装置50、储样试管60及盐 浴池70，所述储样试管60设置在电极诱导装置50上，所述储样试管60底 部设置在盐浴池70内；所述农产品农药残留检测装置还包括对储样试管60 内溶入酒精的溶质液进行检测的光谱农药残留检测仪80，所述机构本体100 外层设有配合光谱农药残留检测仪80使用的对比分析机构90。Wherein, the agricultural product pesticide residue detection device includes a mechanism body 100, a partition 10 is provided on the top of the mechanism body 100, a vacuum chamber 20 is provided below the partition 10, and a vacuum chamber 20 is provided in the partition 10 for use with the vacuum chamber 20. A vacuum pump 11, a sample adjustment pool 30 is provided below the vacuum chamber 20, and an adjustment tube 1 41 and an adjustment tube 2 42 used in conjunction with the sample adjustment pool 30 are provided on both sides of the body 100 of the mechanism. An electrode induction device 50, a storage sample test tube 60 and a salt bath 70 are provided, the storage sample test tube 60 is arranged on the electrode induction device 50, and the bottom of the storage sample test tube 60 is arranged in the salt bath 70; the agricultural product pesticide residue detection The device also includes a spectral pesticide residue detector 80 for detecting the solute dissolved in alcohol in the storage test tube 60 , and the outer layer of the mechanism body 100 is provided with a comparative analysis mechanism 90 used in conjunction with the spectral pesticide residue detector 80 .
进一步改进地，所述真空室20顶部设有阀门21和排气阀22，所述真 空室20内设有配合使用的夹持机构23，真空室20底部设有倒液口24，倒 液口24上设有倒液载体241，倒液载体241为互相叠加的滤纸和纤维素膜。As a further improvement, the top of the vacuum chamber 20 is provided with a valve 21 and an exhaust valve 22, and the inside of the vacuum chamber 20 is provided with a cooperating clamping mechanism 23, and the bottom of the vacuum chamber 20 is provided with a liquid pouring port 24, and the liquid pouring port 24 is provided with a liquid pouring carrier 241, and the liquid pouring carrier 241 is a filter paper and a cellulose membrane superimposed on each other.
进一步改进地，所述调节管一41和调节管二42上均设有与样品调节 池30相连通的导管43，所述导管43上设有调节阀431，所述样品调节池 30底部设有过滤层31和配合储样试管60使用的导向管32。As a further improvement, both the first regulating pipe 41 and the second regulating pipe 42 are provided with a conduit 43 communicating with the sample adjustment tank 30, the conduit 43 is provided with a regulating valve 431, and the bottom of the sample adjustment tank 30 is provided with The filter layer 31 and the guide tube 32 used in conjunction with the sample storage tube 60 .
具体地，所述电极诱导装置50包括等离子体装置的下电极介质51，等 离子体装置的下电极介质51的电压为2.2kV，电流为1.2mA、间隙为3.2mm。Specifically, the electrode induction device 50 includes a lower electrode medium 51 of the plasma device, the voltage of the lower electrode medium 51 of the plasma device is 2.2kV, the current is 1.2mA, and the gap is 3.2mm.
本发明所述农产品农药残留检测方法，首先建立检测模型，然后通过 检测装置对待检测样品的精细化处理、改善待检测样品的分子选择透过性， 进而提高了对待检测样品进行光谱检测的精准度及精确的判断出农产品中 农药成分及含量(不仅可以通过光谱检测出农药的种类，还可以根据吸收 的强弱判断农药的含量)，即通过与检测模型的对比得到其含量，检测效果 好、效率高，满足实际检测需求。The method for detecting pesticide residues in agricultural products of the present invention firstly establishes a detection model, and then refines the sample to be detected through the detection device to improve the molecular selective permeability of the sample to be detected, thereby improving the accuracy of spectral detection of the sample to be detected And accurately determine the pesticide composition and content in agricultural products (not only the type of pesticide can be detected by spectrum, but also the content of pesticide can be judged according to the strength of absorption), that is, its content can be obtained by comparing with the detection model, and the detection effect is good. High efficiency, to meet the actual detection needs.
此外，检测装置的结构设计合理、操作简单、易行，方便对待测农产 品的的精细化处理，极大改善待检测样品的分子选择透过性，方便了对农 产品农药残留量的检测，其中，电极诱导处后的分子具有选择透过性极强 的特性，灵敏度好、进一步提高了检测精度In addition, the detection device has a reasonable structural design, simple operation, and is easy to operate, which is convenient for the refined treatment of the agricultural products to be tested, greatly improves the molecular selective permeability of the samples to be tested, and facilitates the detection of pesticide residues in agricultural products. Among them, The molecules behind the electrode induction have the characteristics of strong selective permeability, good sensitivity, and further improve the detection accuracy
附注：本发明的检测方法配合检测装置的检测精度达99.3％。Note: The detection accuracy of the detection method of the present invention combined with the detection device reaches 99.3%.
实施例2Example 2
一种农产品农药残留检测方法，包括以下步骤：A method for detecting pesticide residues in agricultural products, comprising the following steps:
步骤(1)、建立检测模型Step (1), building a detection model
(1.1)制备样品：将能够溶于蒸馏水的农药与蒸馏水进行混合，农药 与蒸馏水的质量比选择成等差数列的多个比例关系；(1.1) Sample preparation: mix the pesticides that can be dissolved in distilled water with distilled water, and the mass ratio of pesticides and distilled water is selected as a plurality of proportional relationships of arithmetic progression;
(1.2)采集光谱数据：获取农药水溶液近红外透射光谱；(1.2) Collect spectral data: obtain the near-infrared transmission spectrum of the pesticide aqueous solution;
(1.3)建立检测模型：根据农药与蒸馏水的比例，以及所对应的农药 水溶液近红外透射光谱，在二维坐标系中建立光谱与有机磷农药含量检测 模型；(1.3) Establish detection model: according to the ratio of pesticide and distilled water, and the near-infrared transmission spectrum of corresponding pesticide aqueous solution, set up spectrum and organophosphorus pesticide content detection model in two-dimensional coordinate system;
步骤(2)、检测待测农产品Step (2), detecting the agricultural product to be tested
(2.1)制备样品：(2.1) Preparation of samples:
(2.11)萃取：将农产品切碎、研磨，称取12g于离心管中，加入10g 无水硫酸钠和18ml的有机溶剂乙酸乙酯，萃取4min，然后将萃取液转移到 另一支离心管中；(2.11) Extraction: chop and grind the agricultural products, weigh 12g in a centrifuge tube, add 10g of anhydrous sodium sulfate and 18ml of organic solvent ethyl acetate, extract for 4min, and then transfer the extract to another centrifuge tube ;
(2.13)电极诱导：将上述萃取液置入等离子体装置的下电极介质上， 电压2.2kV，电流1.2mA、间隙3.2mm的操作条件下照射4秒；(2.13) Electrode induction: place the above extract on the lower electrode medium of the plasma device, and irradiate for 4 seconds under the operating conditions of voltage 2.2kV, current 1.2mA, and gap 3.2mm;
(2.14)浓缩：将装有滤液的试管置于温度为65度的盐浴中蒸发，至 留下溶质；(2.14) Concentration: place the test tube containing the filtrate in a salt bath with a temperature of 65 degrees to evaporate until the solute is left;
(2.2)样品处理：取上述制得的溶质溶于75ml酒精溶液中，振荡均匀；(2.2) Sample treatment: Take the above-mentioned solute and dissolve it in 75ml alcohol solution, shake evenly;
(2.3)采集光谱数据：获取溶入酒精的溶质液的近红外透射光谱；(2.3) Collect spectral data: obtain the near-infrared transmission spectrum of the solute solution dissolved in alcohol;
步骤(3)、判断农产品中农药成分及含量Step (3), judging the composition and content of pesticides in agricultural products
对比步骤(2.3)获取溶入酒精的溶质液的近红外透射光谱与步骤(1.3) 得到的光谱与农药含量检测模型，获取农药成分及含量。Compare the near-infrared transmission spectrum obtained in step (2.3) of the solute solution dissolved in alcohol with the spectrum obtained in step (1.3) and the detection model of pesticide content to obtain the pesticide composition and content.
具体地，所述光谱与所述农药含量检测模型为二维曲线形式，不同的 农药绘制不同的二维曲线；所述二维曲线中相邻的两点为线性连接，所述 二维曲线通过多阶函数拟合方法获得。Specifically, the spectrum and the pesticide content detection model are in the form of a two-dimensional curve, and different pesticides draw different two-dimensional curves; two adjacent points in the two-dimensional curve are connected linearly, and the two-dimensional curve passes through Obtained by multi-order function fitting method.
本发明所述农产品农药残留检测方法，首先建立检测模型，然后通过 检测装置对待检测样品的精细化处理、改善待检测样品的分子选择透过性， 进而提高了对待检测样品进行光谱检测的精准度及精确的判断出农产品中 农药成分及含量(不仅可以通过光谱检测出农药的种类，还可以根据吸收 的强弱判断农药的含量)，即通过与检测模型的对比得到其含量，检测效果 好、效率高，满足实际检测需求The method for detecting pesticide residues in agricultural products of the present invention firstly establishes a detection model, and then refines the sample to be detected through the detection device to improve the molecular selective permeability of the sample to be detected, thereby improving the accuracy of spectral detection of the sample to be detected And accurately determine the pesticide composition and content in agricultural products (not only the type of pesticide can be detected by spectrum, but also the content of pesticide can be judged according to the strength of absorption), that is, its content can be obtained by comparing with the detection model, and the detection effect is good. High efficiency, to meet the actual testing needs
附注：本实施例仅采用本发明的检测方法，没有采用任何检测装置下 进行检测，检测精度达95.1％)。Remarks: the present embodiment only adopts the detection method of the present invention, does not adopt any detection device to detect, and the detection accuracy reaches 95.1%).
实施例3Example 3
一种农产品农药残留检测方法，包括以下步骤：A method for detecting pesticide residues in agricultural products, comprising the following steps:
步骤(1)、建立检测模型Step (1), building a detection model
(1.1)制备样品：将能够溶于蒸馏水的农药与蒸馏水进行混合，农药 与蒸馏水的质量比选择成等差数列的多个比例关系；(1.1) Sample preparation: mix the pesticides that can be dissolved in distilled water with distilled water, and the mass ratio of pesticides and distilled water is selected as a plurality of proportional relationships of arithmetic progression;
(1.2)采集光谱数据：获取农药水溶液近红外透射光谱；(1.2) Collect spectral data: obtain the near-infrared transmission spectrum of the pesticide aqueous solution;
(1.3)建立检测模型：根据农药与蒸馏水的比例，以及所对应的农药 水溶液近红外透射光谱，在二维坐标系中建立光谱与农药含量检测模型；(1.3) Establish a detection model: according to the ratio of pesticide and distilled water, and the corresponding pesticide aqueous solution near-infrared transmission spectrum, set up a spectrum and pesticide content detection model in a two-dimensional coordinate system;
步骤(2)、检测待测农产品Step (2), detecting the agricultural product to be tested
(2.1)制备样品：(2.1) Preparation of samples:
(2.11)萃取：将农产品切碎、研磨，称12g于离心管中，加入10g无 水硫酸钠和18ml的有机溶剂乙酸乙酯，萃取4min，然后将萃取液转移到另 一支离心管中；(2.11) Extraction: chop and grind the agricultural products, weigh 12g in a centrifuge tube, add 10g of anhydrous sodium sulfate and 18ml of organic solvent ethyl acetate, extract for 4min, then transfer the extract to another centrifuge tube;
(2.12)净化：往装有萃取液的离心管中加入6g的无水硫酸钠和0.18g 的活性炭，振荡2min，静置后吸取上层溶液，过滤去除悬浮于溶液中的活 性炭，将滤液收集于试管中；(2.12) Purification: Add 6 g of anhydrous sodium sulfate and 0.18 g of activated carbon to the centrifuge tube containing the extract, shake for 2 minutes, draw the upper layer solution after standing, filter and remove the activated carbon suspended in the solution, and collect the filtrate in in a test tube;
(2.13)浓缩：将装有滤液的试管置于温度为65度的盐浴中，用氮气 或空气将试管中的溶剂吹扫干净，至留下溶质；(2.13) Concentration: place the test tube containing the filtrate in a salt bath with a temperature of 65 degrees, and use nitrogen or air to clean up the solvent in the test tube until the solute is left;
(2.2)样品处理：取上述制得的溶质溶于75ml酒精溶液中，振荡均匀；(2.2) Sample treatment: Take the above-mentioned solute and dissolve it in 75ml alcohol solution, shake evenly;
(2.3)采集光谱数据：获取溶入酒精的溶质液的近红外透射光谱；(2.3) Collect spectral data: obtain the near-infrared transmission spectrum of the solute solution dissolved in alcohol;
步骤(3)、判断农产品中农药成分及含量Step (3), judging the composition and content of pesticides in agricultural products
对比步骤(2.3)获取溶入酒精的溶质液的近红外透射光谱与步骤(1.3) 得到的光谱与农药含量检测模型，获取农药成分及含量。Compare the near-infrared transmission spectrum obtained in step (2.3) of the solute solution dissolved in alcohol with the spectrum obtained in step (1.3) and the detection model of pesticide content to obtain the pesticide composition and content.
具体地，所述光谱与所述农药含量检测模型为二维曲线形式，不同的 农药绘制不同的二维曲线；所述二维曲线中相邻的两点为线性连接，所述 二维曲线通过多阶函数拟合方法获得。Specifically, the spectrum and the pesticide content detection model are in the form of a two-dimensional curve, and different pesticides draw different two-dimensional curves; two adjacent points in the two-dimensional curve are connected linearly, and the two-dimensional curve passes through Obtained by multi-order function fitting method.
本发明所述农产品农药残留检测方法，首先建立检测模型，然后通过 对待检测样品的精细化处理、改善待检测样品的分子选择透过性，进而提 高了对待检测样品进行光谱检测的精准度及精确的判断出农产品中农药成 分及含量(不仅可以通过光谱检测出农药的种类，还可以根据吸收的强弱 判断农药的含量)，即通过与检测模型的对比得到其含量，检测效果好、效 率高，满足实际检测需求The method for detecting pesticide residues in agricultural products described in the present invention first establishes a detection model, and then improves the molecular selective permeability of the sample to be detected through refined treatment of the sample to be detected, thereby improving the accuracy and accuracy of spectral detection of the sample to be detected. The composition and content of pesticides in agricultural products can be accurately judged (not only the type of pesticide can be detected by spectrum, but also the content of pesticide can be judged according to the strength of absorption), that is, the content can be obtained by comparing with the detection model, and the detection effect is good and the efficiency is high , to meet the actual testing needs
附注：本实施例仅采用本发明的检测方法，对待测样品进行深度精细 化处理，在没有采用任何检测装置下进行检测，检测精度达96.7％)。Remarks: the present embodiment only adopts the detection method of the present invention, and the sample to be tested is subjected to deep refinement treatment, and is detected without any detection device, and the detection accuracy reaches 96.7%).
综上所述：结合3个不同的实施例可以看出，对待测样品检测装置的 设置及对待测样品的精细化管理直接影响检测效率和检测的精准度，尤其 是对待测样品检测装置的设置，直接影响对待测样品检测的精准度。In summary: Combining the three different embodiments, it can be seen that the setting of the detection device for the sample to be tested and the refined management of the sample to be tested directly affect the detection efficiency and detection accuracy, especially the setting of the detection device for the sample to be tested , which directly affects the detection accuracy of the sample to be tested.
以上内容是结合具体的实施例对本发明所作的详细说明，不能认定本 发明具体实施仅限于这些说明。对于本发明所属技术领域的技术人员来说， 在不脱离本发明构思的前提下，还可以做出若干简单推演或替换，都应当视为属于本发明保护的范围。The above content is a detailed description of the present invention in conjunction with specific embodiments, and it cannot be assumed that the specific implementation of the present invention is limited to these descriptions. For those skilled in the technical field of the present invention, without departing from the concept of the present invention, some simple deductions or substitutions can be made, which should be deemed to belong to the protection scope of the present invention.
Claims (7)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810443765.0A CN108444946A (en) | 2018-05-10 | 2018-05-10 | A kind of Practice for Pesticide Residue in Agricultural Products detection method and device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810443765.0A CN108444946A (en) | 2018-05-10 | 2018-05-10 | A kind of Practice for Pesticide Residue in Agricultural Products detection method and device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108444946A true CN108444946A (en) | 2018-08-24 |
Family
ID=63203340
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810443765.0A Pending CN108444946A (en) | 2018-05-10 | 2018-05-10 | A kind of Practice for Pesticide Residue in Agricultural Products detection method and device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108444946A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109197467A (en) * | 2018-11-07 | 2019-01-15 | 江苏省农业科学院 | A kind of control method of radish kind strain disease |
| CN111077092A (en) * | 2019-12-24 | 2020-04-28 | 苏州市美益添生物科技有限公司 | Food ingredient content detection device based on spectral analysis |
| CN111220601A (en) * | 2018-11-27 | 2020-06-02 | 上海尚湾信息技术有限公司 | Rapid detection method for pesticide residues in vegetables and fruits |
| CN111742931A (en) * | 2020-08-06 | 2020-10-09 | 祥霖美丰生物科技(淮安)有限公司 | Pesticide composition containing fosthiazate and cyclobutrifuram and used for preventing and treating root-knot nematodes |
| CN111771893A (en) * | 2020-08-06 | 2020-10-16 | 祥霖美丰生物科技(淮安)有限公司 | Pesticide composition containing tioxazafen and cyclobutrifluram |
| CN113390814A (en) * | 2021-06-10 | 2021-09-14 | 中国工程物理研究院激光聚变研究中心 | Intelligent component analysis system and method based on metamaterial spectrometer chip |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1243967C (en) * | 2004-06-15 | 2006-03-01 | 厦门大学 | Rapid Determination Method of Carbamate Pesticide Residues in Vegetables |
| CN101701909A (en) * | 2009-11-02 | 2010-05-05 | 中国农业大学 | A Rapid Detection Method for Trace Pesticides |
| CN103499530A (en) * | 2013-10-14 | 2014-01-08 | 无锡艾科瑞思产品设计与研究有限公司 | Method for rapidly detecting pesticide residues in fruits and vegetables |
| CN107748141A (en) * | 2017-12-04 | 2018-03-02 | 重庆市合川区农产品质量安全监督检验检测站 | A kind of Practice for Pesticide Residue in Agricultural Products testing agency |
-
2018
- 2018-05-10 CN CN201810443765.0A patent/CN108444946A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1243967C (en) * | 2004-06-15 | 2006-03-01 | 厦门大学 | Rapid Determination Method of Carbamate Pesticide Residues in Vegetables |
| CN101701909A (en) * | 2009-11-02 | 2010-05-05 | 中国农业大学 | A Rapid Detection Method for Trace Pesticides |
| CN103499530A (en) * | 2013-10-14 | 2014-01-08 | 无锡艾科瑞思产品设计与研究有限公司 | Method for rapidly detecting pesticide residues in fruits and vegetables |
| CN107748141A (en) * | 2017-12-04 | 2018-03-02 | 重庆市合川区农产品质量安全监督检验检测站 | A kind of Practice for Pesticide Residue in Agricultural Products testing agency |
Non-Patent Citations (1)
| Title |
|---|
| 沈国华: "负压采汁装置", 《食品机械》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109197467A (en) * | 2018-11-07 | 2019-01-15 | 江苏省农业科学院 | A kind of control method of radish kind strain disease |
| CN111220601A (en) * | 2018-11-27 | 2020-06-02 | 上海尚湾信息技术有限公司 | Rapid detection method for pesticide residues in vegetables and fruits |
| CN111077092A (en) * | 2019-12-24 | 2020-04-28 | 苏州市美益添生物科技有限公司 | Food ingredient content detection device based on spectral analysis |
| CN111742931A (en) * | 2020-08-06 | 2020-10-09 | 祥霖美丰生物科技(淮安)有限公司 | Pesticide composition containing fosthiazate and cyclobutrifuram and used for preventing and treating root-knot nematodes |
| CN111771893A (en) * | 2020-08-06 | 2020-10-16 | 祥霖美丰生物科技(淮安)有限公司 | Pesticide composition containing tioxazafen and cyclobutrifluram |
| CN113390814A (en) * | 2021-06-10 | 2021-09-14 | 中国工程物理研究院激光聚变研究中心 | Intelligent component analysis system and method based on metamaterial spectrometer chip |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108444946A (en) | A kind of Practice for Pesticide Residue in Agricultural Products detection method and device | |
| CN102175606B (en) | A detection method for acute biological toxicity of sewage | |
| AU2020102406A4 (en) | Method for detecting pesticide residues in agricultural products | |
| CN203324075U (en) | Activated carbon filtration purification device | |
| CN103529186B (en) | Device and method for measuring dissolved methane in seawater | |
| CN109521160A (en) | Heavy metal quick screening method in a kind of solid waste Leaching | |
| CN106153770A (en) | A kind of Solid-Phase Extraction liquid chromatography mass detection method of aquatic products glyphosate | |
| CN102928389A (en) | Device for quickly detecting impregnation amount in real time and using method thereof | |
| CN103278539A (en) | Cell impedance sensor apparatus for detecting marine aquatic product diarrheal toxin, and method | |
| CN104390926B (en) | Online rapid detection method of herba andrographis concentrated decolorization process | |
| CN103983703B (en) | A kind of high-efficiency liquid chromatography method for detecting of aquaculture system Methylene Blue | |
| CN104330516B (en) | A kind of method of simultaneously measuring allantoin in dried rhizoma of Dioscorea opposita and adenosine content | |
| CN108414609B (en) | Online mass spectrum detection device for nutrient component change process in traditional Chinese medicine steaming process | |
| CN102565170A (en) | Sensitive capillary electrophoresis methods for detecting melamine in formula milk powder | |
| CN106680403A (en) | Method for detecting dendrophenol in Dendrobium officinale | |
| CN107976469A (en) | A kind of soil nutrient device for fast detecting based on Artificial Olfactory | |
| CN113804799A (en) | A kind of pretreatment method and method for testing NMP content in lithium ion battery pole piece | |
| CN102818782B (en) | Determination method of total 2-(2-phenethyl) chromone compound content | |
| CN102262089B (en) | Rapid Quantitative Detection Method of Cyanopyrethroid Pesticide Residues in Tea | |
| CN102175787A (en) | Method for analyzing relative molecular weights of dissolved organic matters in water by exclusion chromatography | |
| CN102788855B (en) | On-line detection device and detection method for atomizing extraction for volatile organic matters in water | |
| CN103808855A (en) | Method for extracting oestrone from euphausia superba and efficient thin layer chromatography scanning and detecting method | |
| CN107102087A (en) | A kind of method of a variety of organic acid contents in chromatography of ions detection coptis | |
| CN103913535A (en) | Combined detection method for alkaline fermented sludge and nonyl phenol in liquid supernatant of alkaline fermented sludge | |
| CN207571086U (en) | A liquid chromatograph detector switching device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180824 |
|
| RJ01 | Rejection of invention patent application after publication |