用于土壤中氮钾含量快速测定的非接触电导微流控芯片OACSTPCD
Contactless Conductivity Microfluidic Chip for Rapid Determination of Soil Nitrogen and Potassium Content
[目的/意义]土壤中氮、钾元素在作物生长和农业生产过程中具有关键作用.快速定量检测土壤中氮、钾含量对指导精确施肥具有重要意义.因此,建立一种快速可靠的土壤氮、钾含量检测方法十分必要.[方法]本研究建立一种基于聚二甲基硅氧烷(Polydimethylsiloxane,PDMS)微流控芯片电泳和电容耦合非接触电导检测(Capacitively Coupled Contactless Conductivity Detection,C4D)方法,快速定量检测土壤中氮、钾养分离子.通过微流控电泳芯片实现对土壤中多种离子快速分离,利用C4D进行电导率变化的精准测量.基于检测器工作频率输出响应特性,激励电压响应特性和电泳电压,确定最佳分离和检测性能.[结果和讨论]该方法对钾离子(K+)、铵根离子(NH4+)和硝酸根离子(NO3‒)标准溶液的检测限(S/N=3)分别为0.5、0.1和0.4 mg/L.K+、NH4+和NO3‒在0.5~40.0 mg/L范围内具有良好的线性关系,线性相关系数(R2)分别为0.994、0.997和0.990,表明该方法可以对土壤中氮、钾养分离子进行定量分析.同时,采用峰高、峰面积和出峰时间作为评价指标进行可重复性实验,其相对标准偏差(Relative Standard Deviation,RSD)均小于4.4%,说明该方法具有良好的重复性.此外,对土壤样品进行测试,K+和NH4+可实现完全分离以及同步检测,其检测效率明显提高.通过标准加入法进行回收率实验,回收率保持在81.74%~127.76%.[结论]本研究为土壤氮钾养分离子的快速检测提供了一种简便、高效的方法.
[Objective]The content of nitrogen(N)and potassium(K)in the soil directly affects crop yield,making it a crucial indicator in agricul-tural production processes.Insufficient levels of the two nutrients can impede crop growth and reduce yield,while excessive levels can result in environmental pollution.Rapidly quantifying the N and K content in soil is of great importance for agricultural produc-tion and environmental protection. [Methods]A rapid and quantitative method was proposed for detecting N and K nutrient ions in soil based on polydimethylsiloxane(PDMS)microfluidic chip electrophoresis and capacitively coupled contactless conductivity detection(C4D).Microfluidic chip elec-trophoresis enables rapid separation of multiple ions in soil.The electrophoresis microfluidic chips have a cross-shaped channel layout and were fabricated using soft lithography technology.The sample was introduced into the microfluidic chip by applying the appropri-ate injection voltage at both ends of the injection channel.This simple and efficient procedure ensured an accurate sample introduc-tion.Subsequently,an electrophoretic voltage was applied at both ends of the separation channel,creating a capillary zone electropho-resis that enables the rapid separation of different ions.This process offered high separation efficiency,required a short processing time,and had a small sample volume requirement.This enabled the rapid processing and analysis of many samples.C4D enabled pre-cise measurement of changes in conductivity.The sensing electrodes were separated from the microfluidic chips and printed onto a printed circuit board(PCB)using an immersion gold process.The ions separated under the action of an electric field and sequentially reach the sensing electrodes.The detection circuit,connected to the sensing electrodes,received and regulated the conductivity signal to reflect the variance in conductivity between the sample and the buffer solution.The sensing electrodes were isolated from the sam-ple solution to prevent interference from the high-voltage electric field used for electrophoresis. [Results and Discussions]The voltage used for electrophoresis,as well as the operating frequency and excitation voltage of the excita-tion signal in the detection system,had a significant effect on separation and detection performance.Based on the response characteris-tics of the system output,the optimal operating frequency of 1 000 kHz,excitation voltage of 50 V,and electrophoresis voltage of 1.5 kV were determined.A peak overshoot was observed in the electrophoresis spectrum,which was associated with the operating fre-quency of the system.The total noise level of the system was approximately 0.091 mV.The detection limit(S/N = 3)for soil nutrient ions was determined by analyzing a series of standard sample solutions with varying concentrations.The detection limited for potassi-um(K+),ammonium(NH4+),and nitrate(NO3‒)standard solutions were 0.5,0.1 and 0.4 mg/L,respectively.For the quantitative deter-mination of soil nutrient ion concentration,the linear relationship between peak area and corresponding concentration was investigat-ed under optimal experimental conditions.K+,NH4+,and NO3‒ exhibit a strong linear relationship in the range of 0.5~40 mg/L,with linear correlation coefficients(R2)of 0.994,0.997,and 0.990,respectively,indicating that this method could accurately quantify N and K ions in soil.At the same time,to evaluate the repeatability of the system,peak height,peak area,and peak time were used as evalua-tion indicators in repeatability experiments.The relative standard deviation(RSD)was less than 4.4%,indicating that the method shows good repeatability.In addition,to assess the ability of the C4D microfluidic system to detect actual soil samples,four collected soil samples were tested using MES/His and PVP/PTAE as running buffers.K+,NH4+,Na+,Chloride(Cl‒),NO3‒,and sulfate(SO43‒)were separated sequentially within 1 min.The detection efficiency was significantly improved.To evaluate the accuracy of this meth-od,spiked recovery experiments were performed on four soil samples.The recovery rates ranged from 81.74%to 127.76%,indicating the good accuracy of the method. [Conclusions]This study provides a simple and effective method for the rapid detection of N and K nutrient ions in soil.The method is highly accurate and reliable,and it can quickly and efficiently detect the contents of N and K nutrient ions in soil.This contactless measurement method reduced costs and improved economic efficiency while extending the service life of the sensing electrodes and reducing the frequency of maintenance and replacement.It provided strong support for long-term,continuous conductivity monitoring.
洪炎;王乐;王儒敬;苏静明;李浩;张家宝;郭红燕;陈翔宇
安徽理工大学 电气与信息工程学院,安徽淮南 232001,中国安徽理工大学 电气与信息工程学院,安徽淮南 232001,中国||中科合肥智慧农业协同创新研究院,农业传感器与智能感知安徽省技术创新中心,安徽合肥 231131,中国中国科学院合肥物质科学研究院,智能机械研究所,安徽省智慧农业工程实验室,安徽合肥 230031,中国||中科合肥智慧农业协同创新研究院,农业传感器与智能感知安徽省技术创新中心,安徽合肥 231131,中国中科合肥智慧农业协同创新研究院,农业传感器与智能感知安徽省技术创新中心,安徽合肥 231131,中国
化学
非接触电导检测微流控芯片土壤养分聚二甲基硅氧烷
contactless conductivity detectionmicrofluidic chipsoil nutrientpolydimethylsiloxane
《智慧农业(中英文)》 2024 (001)
18-27 / 10
国家重点研发计划项目(2021YFD2000204,2023YFD1702104,2023YFD1701800);国家自然科学基金项目(12304236,32301688);安徽省科技重大专项(2020b06050001);安徽省自然科学基金项目(2308085QA19,1908085QE202,1808085MF169);安徽省科技特派团项目(S2022t06010123);安徽省数字农业工程技术研究中心开放课题(AHSZNYGCZXKF021);中国科学院合肥物质科学研究院院长基金(YZJJ2024QN38) National Key Research and Development Program of China(2021YFD2000204,2023YFD1702104,2023YFD1701800);National Natural Science Foundation of China(12304236,32301688);Anhui Province Science and Technology Major Project(2020b06050001);Anhui Provincial Natural Science Foundation(2308085QA19,1908085QE202,1808085MF169);Sci-ence and Technology Mission Program of Anhui Province(S2022t06010123);Open Fund for Anhui Digital Agriculture Engineering Technology Research Center(AHSZNYGCZXKF021);The Dean Foundation of Hefei Institutes of Physical Science,Chinese Acade-my of Sciences(YZJJ2024QN38)
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