技术领域technical field
本发明涉及一种农药多残留检测仪，尤其涉及一种基于阵列式传感器的农药残留检测仪，其融合了生物传感器检测技术和嵌入式系统设计方法，用于方便、迅速、准确的检测农产品中含有何种农药残留及是否超标。属于农产品安全检测技术领域。The invention relates to a pesticide multi-residue detector, in particular to a pesticide residue detector based on an array sensor, which integrates biosensor detection technology and embedded system design method, and is used for convenient, rapid and accurate detection of agricultural products What kind of pesticide residues are contained and whether they exceed the standard. The invention belongs to the technical field of agricultural product safety detection.
背景技术Background technique
现在生产领域中应用的农药种类已经达到100多种，对农业保持丰收增产起到了很大的作用，其已成为重要的一种生产资料。伴随着改革开放的深入进行，在一些常熟地区，农药事业的发展速度变得很快。因农业机械化正在不断推进，农药的大面积使用是不可缺少的。但因农药的不合理的使用，造成了诸多的环境问题，如农田生态系统被破坏等。农药的大量使用，在保证了粮食等农作物大量稳产的同时，也带来了诸多的环境问题。在植物、土壤和水体中残留的农药有两种残存的形式：第一种保持原有的化学结构；第二种以化学转化后的产物或被生物降解产物的形式残存。因此，农药残留问题不容忽视。Now there are more than 100 types of pesticides used in the field of production, which have played a great role in maintaining a bumper harvest and increasing production in agriculture, and have become an important means of production. With the deepening of reform and opening up, in some Changshu areas, the development speed of the pesticide industry has become very fast. Due to the continuous advancement of agricultural mechanization, the large-scale use of pesticides is indispensable. However, due to the unreasonable use of pesticides, many environmental problems have been caused, such as the destruction of the farmland ecosystem. The extensive use of pesticides has not only ensured the stable production of food and other crops, but also brought many environmental problems. Pesticide residues in plants, soil and water have two remaining forms: the first remains in the original chemical structure; the second remains in the form of chemically transformed products or biodegraded products. Therefore, the problem of pesticide residues cannot be ignored.
目前农药残留分析的主要方法是气相色谱仪、液相色谱仪、气质联用仪、液质联用仪等，这些方法虽然分析精度高，定量准确，但其样品的前处理复杂、检测耗时长、成本高、需要技术熟练的操作人员。我国农药残留的速测方法是酶抑制试纸法和酶抑制分光光度法（农残快速检测仪），可以实现有机磷农药及氨基甲酸酯类农药的现场快速检测，具有较好的实用价值。速测卡是通过肉眼观察卡片的颜色变化，因此一般只能用于严重超标的蔬菜样品进行定性测量。酶抑制分光光度法的应用也比较广泛，国内已有多种农药残留速测仪均是基于此原理。分光光法的原理是基于吸光度的变化进行检测的，但蔬菜水果中大量的色素会对分光光度法造成很大的影响，导致检测结果的不准确。并且上述方法存在回收率低、错检、漏检比例较高、重复性差、难以满足低残留和定量检测的要求等缺点。At present, the main methods for the analysis of pesticide residues are gas chromatography, liquid chromatography, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, etc. Although these methods have high analysis precision and accurate quantification, the pretreatment of samples is complicated and the detection time is long , high cost and requires skilled operators. The rapid detection methods of pesticide residues in my country are enzyme inhibition test paper method and enzyme inhibition spectrophotometry (rapid detection instrument for pesticide residues), which can realize rapid on-site detection of organophosphorus pesticides and carbamate pesticides, and has good practical value. The quick test card is to observe the color change of the card with naked eyes, so it can generally only be used for qualitative measurement of vegetable samples that seriously exceed the standard. Enzyme inhibition spectrophotometry is also widely used, and there are many pesticide residue rapid detectors in China based on this principle. The principle of spectrophotometry is based on the change of absorbance for detection, but a large number of pigments in vegetables and fruits will have a great impact on spectrophotometry, resulting in inaccurate detection results. Moreover, the above method has disadvantages such as low recovery rate, high proportion of false detection and missed detection, poor repeatability, and difficulty in meeting the requirements of low residue and quantitative detection.
发明的目的在于针对现有技术的不足，设计提供一种基于阵列式传感器的农药残留检测仪，具有携带方便、检测快速准确、操作简单、可实现农药多残留同时检测等特点。The purpose of the invention is to design and provide a pesticide residue detector based on an array sensor, which has the characteristics of easy portability, fast and accurate detection, simple operation, and simultaneous detection of multiple pesticide residues.
所述的一种基于阵列式传感器的农药残留检测仪其检测原理为：利用抗体与农药之间的特异性免疫反应，以抗体作为识别元件，采用固定化技术在工作电极表面固定不同种类的农药抗体，通过模拟多路开关使阵列式传感器中的一个工作电极与共用的参比电极和对电极接通。通过传感器在测试底液中导致的阻抗变化来确定样品中含有何种农药，并根据不同农药产生阻抗变化的标准曲线，确定样品中的农药的含量。The detection principle of the pesticide residue detector based on the array sensor is as follows: using the specific immune reaction between the antibody and the pesticide, using the antibody as the recognition element, and using immobilization technology to immobilize different types of pesticides on the surface of the working electrode Antibody, by simulating a multiplex switch, a working electrode in the array sensor is connected to a common reference electrode and a counter electrode. The pesticide contained in the sample is determined by the impedance change caused by the sensor in the test bottom liquid, and the content of the pesticide in the sample is determined according to the standard curve of impedance change produced by different pesticides.
为了实现上述目的，本发明提供的一种基于阵列式传感器的农药多残留检测仪由检测电路、阵列式传感器、电源、按键、微控制器及显示屏构成。检测电路用来产生激励电压并施加到各免疫传感器上，随后采样激励后的响应信号并进行数字处理，将结果送入微控制器；微控制器及其上面运行的检测程序对输入信号进行再次处理，并对整个系统的运行进行控制和响应；按键用来输入指令和检测参数；显示屏用来量化输出呈现最终的检测结果，是用户与系统的交互界面；电源为整个系统供电。In order to achieve the above object, the present invention provides an array sensor-based pesticide multi-residue detector consisting of a detection circuit, an array sensor, a power supply, buttons, a microcontroller and a display screen. The detection circuit is used to generate the excitation voltage and apply it to each immune sensor, then sample the response signal after excitation and perform digital processing, and send the result to the microcontroller; the microcontroller and the detection program running on it process the input signal again , and control and respond to the operation of the entire system; the buttons are used to input instructions and detection parameters; the display is used to quantify the output and present the final detection results, which is the interactive interface between the user and the system; the power supply supplies power to the entire system.
本发明的一种基于阵列式传感器的农药多残留检测仪具体结构为：农药多残留检测仪由检测电路、阵列式传感器、模拟多路开关、电源、按键、微控制器及显示屏构成，其中：检测电路由供电电路、检测芯片、拨码开关、标定电阻、阵列式传感器、模拟多路开关构成。供电电路与微控制器和检测芯片相连，采用先经变压器降压再经滤波稳压的方法获得的+5V供电；芯片通过拨码开关与标定电阻相连，根据输入测量范围参数，通过拨码开关选择相应标定电阻，以此调整测量灵敏度；在微控制器的控制下，芯片产生激励电压施加到阵列式免疫传感器上并收集响应信号，经过离散型傅立叶变换后得到其实部与虚部，并将其输出到微控制器。微控制器上运行检测程序，将接收到的阻抗实部与虚部通过阻抗的模值与相角计算公式计算出阻抗的模值与相角，再经过校准后得出实际的阻抗值，与设定的反应前的阻抗值进行比较，得到变化率并对比标准曲线得出结论，送至显示屏显示。所述的显示屏与微控制器相连，用于显示数据及作为用户进行交互操作的窗口，显示屏采用LED12864，其功耗能够满足便携式设备的功耗要求。所述的按键与微控制器和检测电路相连，设有启动、开始、复位、停止按键和四个检测范围档位，用于输入相关指令和检测参数。所述电源与供电电路相连。The specific structure of a pesticide multi-residue detector based on an array sensor of the present invention is as follows: the pesticide multi-residue detector is composed of a detection circuit, an array sensor, an analog multi-way switch, a power supply, buttons, a microcontroller and a display screen, wherein : The detection circuit is composed of a power supply circuit, a detection chip, a code switch, a calibration resistor, an array sensor, and an analog multi-way switch. The power supply circuit is connected with the microcontroller and the detection chip, and the +5V power supply is obtained by first stepping down the voltage of the transformer and then filtering and stabilizing the voltage; the chip is connected with the calibration resistor through the dial switch, and according to the input measurement range parameters, through the dial switch Select the corresponding calibration resistance to adjust the measurement sensitivity; under the control of the microcontroller, the chip generates an excitation voltage that is applied to the array immunosensor and collects the response signal. After discrete Fourier transform, the real part and the imaginary part are obtained, and the its output to the microcontroller. The detection program is run on the microcontroller, and the real part and imaginary part of the received impedance are calculated through the impedance modulus value and phase angle calculation formula to calculate the impedance modulus value and phase angle, and then the actual impedance value is obtained after calibration. Compare the impedance value before the set reaction, get the rate of change and compare it with the standard curve to draw a conclusion, and send it to the display screen for display. The display screen is connected with the microcontroller and is used for displaying data and as a window for users to perform interactive operations. The display screen adopts LED12864, and its power consumption can meet the power consumption requirements of portable devices. The buttons are connected with the micro-controller and the detection circuit, and are provided with start, start, reset, stop buttons and four detection range gears for inputting relevant instructions and detection parameters. The power supply is connected with the power supply circuit.
本发明的一种基于阵列式传感器的农药多残留检测仪，检测使用时，首先通过拨码开关选定标定电阻保证测量灵敏度，将阵列式传感器放入待检测溶液中，在微控制器的控制下，芯片产生激励电压施加到阵列式传感器上并收集响应信号，经过离散型傅立叶变换后得到其实部与虚部，并将其输出到微控制器，经微控制器及其检测程序进行信号再处理，并与反应前阻抗值做比较，计算得出变化率。由于在阵列式传感器的工作电极上固定不同种类的农药抗体，因此根据各传感器阻抗变化率的大小即表明了检测的样品中含有何种农药及农药残留的浓度。A kind of pesticide multi-residue detector based on the array sensor of the present invention, when detecting and using, first select the calibration resistance through the dial switch to ensure the measurement sensitivity, put the array sensor into the solution to be detected, and control it under the control of the microcontroller Next, the chip generates an excitation voltage and applies it to the array sensor and collects the response signal. After the discrete Fourier transform, the real part and the imaginary part are obtained and output to the microcontroller. The signal is reconstructed by the microcontroller and its detection program. Processing, and compared with the impedance value before the reaction, the rate of change is calculated. Since different kinds of pesticide antibodies are immobilized on the working electrodes of the array sensor, the impedance change rate of each sensor indicates which pesticide and the concentration of pesticide residues are contained in the detected sample.
为达到以上目的，阵列式传感器采取以下技术方案实现：由一个圆形的电极盘组成，中心位置有对电极和参比电极，外围是工作电极，以确保对电极、参比电极与各工作电极的距离相等，使各个工作电极与对电极之间的有相等的阻抗值。在工作电极与参比电极之间加300毫伏的工作电压，测试液中测定的是工作电极与对电极之间的阻抗值。使用模拟多路开关确定哪一路工作电极接通。In order to achieve the above goals, the array sensor adopts the following technical solutions: it is composed of a circular electrode plate, with a counter electrode and a reference electrode in the center, and a working electrode on the periphery, so as to ensure that the counter electrode, reference electrode and each working electrode The distances are equal, so that there are equal impedance values between each working electrode and the counter electrode. A working voltage of 300 millivolts is applied between the working electrode and the reference electrode, and the impedance value between the working electrode and the counter electrode is measured in the test solution. Use an analog multiplexer to determine which working electrode is on.
本发明提供的一种基于阵列式传感器的农药多残留检测仪应用到农产品中的农药残留快速检测领域，可以为检测人员带来极大的便利，能够充分满足农药残留现场快速检测的要求。相对于以往的检测工作必须把各种待测样品运输到检测中心，由专业工作人员在大型的工作站设备进行而言，本发明的检测仪具有携带方便、检测快速准确、操作简单、实用性强等突出特点。The multi-residue pesticide detection instrument based on the array sensor provided by the present invention is applied to the field of rapid detection of pesticide residues in agricultural products, which can bring great convenience to detection personnel and can fully meet the requirements of rapid detection of pesticide residues on site. Compared with the previous detection work, which must transport various samples to be tested to the detection center, and is carried out by professional staff in large-scale workstation equipment, the detector of the present invention has the advantages of easy portability, fast and accurate detection, simple operation, and strong practicability and other outstanding features.
附图说明Description of drawings
图1是本发明的一种基于阵列式传感器的农药多残留检测仪的结构框图，Fig. 1 is a structural block diagram of a pesticide multi-residue detector based on an array sensor of the present invention,
图2为本发明中供电电路原理图，Fig. 2 is a schematic diagram of the power supply circuit in the present invention,
图3为本发明中检测电路原理图。Fig. 3 is a schematic diagram of the detection circuit in the present invention.
具体实施方式Detailed ways
下面结合附图和实施例对本发明的技术方案作详细说明。图1为本发明的一种基于阵列式传感器的农药多残留检测仪的结构框图，本发明由检测电路、阵列式免疫传感器、模拟多路开关、电源、按键、微控制器及显示屏构成。其中检测电路由供电电路、检测芯片、拨码开关、标定电阻、阵列式免疫传感器连接构成。检测电路用来产生激励电压并施加到免疫传感器上，随后采样激励后的响应信号并进行数字处理，将结果送入微控制器；微控制器及其上面运行的检测程序对输入信号进行再次处理，并对整个系统的运行进行控制和响应；按键用来输入指令和检测参数；显示屏用来量化输出呈现最终的检测结果，是用户与系统的交互界面；电源为整个系统供电。The technical solution of the present invention will be described in detail below in conjunction with the accompanying drawings and embodiments. Fig. 1 is a structural block diagram of a pesticide multi-residue detector based on an array sensor of the present invention. The present invention is composed of a detection circuit, an array type immune sensor, an analog multi-way switch, a power supply, buttons, a microcontroller and a display screen. The detection circuit is composed of a power supply circuit, a detection chip, a dial switch, a calibration resistor, and an array immune sensor connection. The detection circuit is used to generate the excitation voltage and apply it to the immune sensor, then sample the excited response signal and perform digital processing, and send the result to the microcontroller; the microcontroller and the detection program running on it process the input signal again, And control and respond to the operation of the entire system; the buttons are used to input instructions and detection parameters; the display is used to quantify the output and present the final detection results, which is the interactive interface between the user and the system; the power supply supplies power to the entire system.
所述的阵列式传感器由一个圆形的电极盘组成，中心位置有对电极和参比电极，外围是工作电极，以确保对电极、参比电极与各工作电极的距离相等，使各个工作电极与对电极之间的有相等的阻抗值。在工作电极与参比电极之间加300毫伏的工作电压，测试液中测定的是工作电极与对电极之间的阻抗值。使用模拟多路开关确定哪一路工作电极接通。The array sensor is composed of a circular electrode plate, with a counter electrode and a reference electrode at the center, and a working electrode at the periphery, so as to ensure that the distance between the counter electrode, the reference electrode and each working electrode is equal, so that each working electrode It has the same impedance value as that between the counter electrodes. A working voltage of 300 millivolts is applied between the working electrode and the reference electrode, and the impedance value between the working electrode and the counter electrode is measured in the test solution. Use an analog multiplexer to determine which working electrode is on.
所述微控制器选用STC89C52，其上加载检测程序。检测电路中的供电电路构成和原理如图2所示，由变压器T1，桥式整流电路BR1，电解电容C1、C3，普通电容C2、C4，三端稳压器U1构成，其作用是为整个系统提供+5V的电源供电。本设计中电解电容C1、C2的作用是滤波，简单的讲就是电容两端电压升高时，电容充电，电压降低时，电容放电，让电压降低时的坡度变得平缓，从而起到滤波的作用。普通电容C2、C4的作用是防止自激，其可以将高频激信号吸收保持稳定，使电路没有激励信号，从而防止自激。三端稳压器U1的作用是将输出电压稳定在+5V上，U1的输出端和接地端分别接+5V和接地。The microcontroller is STC89C52, on which the detection program is loaded. The composition and principle of the power supply circuit in the detection circuit are shown in Figure 2. It is composed of transformer T1, bridge rectifier circuit BR1, electrolytic capacitors C1, C3, ordinary capacitors C2, C4, and three-terminal voltage regulator U1. The system provides +5V power supply. In this design, the role of electrolytic capacitors C1 and C2 is to filter. Simply put, when the voltage across the capacitor rises, the capacitor is charged, and when the voltage drops, the capacitor is discharged, so that the slope becomes gentle when the voltage drops, thereby playing the role of filtering. effect. The role of ordinary capacitors C2 and C4 is to prevent self-excitation, which can absorb high-frequency excitation signals and keep them stable, so that the circuit has no excitation signals, thereby preventing self-excitation. The function of the three-terminal regulator U1 is to stabilize the output voltage at +5V, and the output terminal and ground terminal of U1 are connected to +5V and ground respectively.
所述的检测电路中核心部分检测电路的构成如图3所示：由检测芯片U3，拨码开关SW3，标定电阻R1、R2、R3、R4、R5，普通电容C7、C8构成，其作用是产生激励电压并施加到免疫传感器上，随后采样激励后的响应信号并进行数字处理，将结果送入微控制器。其中标定电阻R1、R2、R3的作用是作为外接反馈电阻。拨码开关SW3是四位拨码开关，其作用是选择合适的标定的电阻连入检测电路来防止响应信号超过检测芯片的量程并且保证系统的线性特性。标定电阻R4、R5的作用是作为上拉电阻连接在检测芯片的15、16引脚与电源之间。电容C7、C8的作用是用来滤波和起保护作用的，防止电磁干扰。检测芯片U3是一款高精度的阻抗测量芯片，内部集成了带有12位，采样率高达1MSPS的AD转换器的频率发生器。其作用是产生特定频率的激励电压来激励待测元件，得到的响应信号被ADC采样，并通过片上的DSP进行离散的傅立叶变换，傅立叶变换后返回在这个输出频率下得到的实部值和虚部值，并将结果送入微控制器。其15、16引脚通过上拉电阻R4、R5与+5V电源相连，其12、13、14引脚并联接地，其9、10、11引脚并联与+5V电源相连，其4、5引脚之间通过拨码开关与标定电阻相连，其5、6用来接待测元件。The composition of core part detection circuit in the described detection circuit is as shown in Figure 3: by detection chip U3, dial switch SW3, calibration resistance R1, R2, R3, R4, R5, common electric capacity C7, C8 constitute, its effect is The excitation voltage is generated and applied to the immune sensor, then the response signal after excitation is sampled and digitally processed, and the result is sent to the microcontroller. Among them, the calibration resistors R1, R2, and R3 are used as external feedback resistors. The DIP switch SW3 is a four-position DIP switch. Its function is to select an appropriate calibrated resistor to connect to the detection circuit to prevent the response signal from exceeding the range of the detection chip and ensure the linearity of the system. The role of calibration resistors R4 and R5 is to connect between pins 15 and 16 of the detection chip and the power supply as pull-up resistors. Capacitors C7 and C8 are used for filtering and protection against electromagnetic interference. The detection chip U3 is a high-precision impedance measurement chip, which integrates a frequency generator with a 12-bit AD converter with a sampling rate up to 1MSPS. Its function is to generate an excitation voltage of a specific frequency to excite the component under test, and the obtained response signal is sampled by the ADC, and then undergoes discrete Fourier transform through the on-chip DSP, and returns the real part value and imaginary value obtained at this output frequency after Fourier transform. internal value and send the result to the microcontroller. Its pins 15 and 16 are connected to +5V power supply through pull-up resistors R4 and R5; The pins are connected to the calibration resistor through a dial switch, and 5 and 6 are used to receive the tested components.
本发明的一种基于阵列式传感器的农药多残留检测仪，具体使用过程如下：在使用前将阵列式传感器工作电极表面使用多壁碳纳米管等纳米材料进行化学修饰，提高传感器检测的灵敏度，之后在阵列式免疫传感器工作电极表面分别固定不同种类的抗体。然后将阵列式抗体传感器放入冰箱中，4°C下保存备用。使用时打开农药多残留检测仪的电源开关，将阵列式传感器放入测试底液中测量初始阻抗值A1，并保存。将免疫传感器放入事先处理好的样品液中孵化10分钟，再将传感器连接至检测仪进行阻抗测量，获取第二次测量的阻抗值A2，微控制器将其送至显示屏显示。计算出变化率，变化率计算公式如下：A pesticide multi-residue detector based on an array sensor of the present invention, the specific use process is as follows: before use, the surface of the working electrode of the array sensor is chemically modified with nanomaterials such as multi-walled carbon nanotubes to improve the sensitivity of sensor detection, Afterwards, different kinds of antibodies were respectively immobilized on the surface of the working electrode of the array immunosensor. Then put the arrayed antibody sensor into the refrigerator and store it at 4°C for future use. When in use, turn on the power switch of the pesticide multi-residue detector, put the array sensor into the test bottom liquid, measure the initial impedance value A1, and save it. Put the immunosensor into the pre-treated sample solution and incubate for 10 minutes, then connect the sensor to the detector for impedance measurement, obtain the impedance value A2 of the second measurement, and send it to the display screen for display by the microcontroller. The rate of change is calculated, and the formula for calculating the rate of change is as follows:
变化率=|A1-A2|/A1Rate of change=|A1-A2|/A1
如果样品液中含有农药，则含相应农药的工作电极发生特异性免疫反应，导致反应后的相应传感器阻抗值明显增大。A1与A2的差值越大，表明检测溶液中的含有某种农药残留的浓度越高。对比标准曲线得到样品中农药残留的浓度，在显示屏显示。阻抗变化率与农药残留浓度关系标准曲线，可以通过农药残留检测仪对多组不同浓度不同种类的农药加标测定得出。If the sample solution contains pesticides, a specific immune reaction will occur on the working electrode containing the corresponding pesticides, resulting in a significant increase in the impedance of the corresponding sensor after the reaction. The larger the difference between A1 and A2, the higher the concentration of a certain pesticide residue in the detection solution. Compare the standard curve to get the concentration of pesticide residues in the sample, which will be displayed on the display. The standard curve of the relationship between the impedance change rate and the pesticide residue concentration can be obtained through the spiked measurement of multiple groups of different concentrations and different types of pesticides by the pesticide residue detector.
本发明的一种基于阵列式传感器的农药多残留检测仪检测方法操作工艺简单，检测时间较短，可实现农药残留的定性定量测量，具有灵敏度高，稳定性好、重现性好等优点，符合我国农药残留快速检测技术发展和国际化要求。The detection method of a pesticide multi-residue detector based on an array sensor of the present invention has simple operation process, short detection time, can realize qualitative and quantitative measurement of pesticide residues, and has the advantages of high sensitivity, good stability, good reproducibility, etc. It is in line with the development and internationalization requirements of rapid detection technology for pesticide residues in my country.
| Application Number | Priority Date | Filing Date | Title |
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| CN201310577417.XACN103558257B (en) | 2013-11-19 | 2013-11-19 | Pesticide multiresidue detector based on array sensors |
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| CN201310577417.XACN103558257B (en) | 2013-11-19 | 2013-11-19 | Pesticide multiresidue detector based on array sensors |
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