基于碳纳米管材料的磺胺电化学传感器研究
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摘要
纳米功能材料在电化学催化和分析中的应用已成为当前电化学传感器领域的一个研究热点。相较于宏观颗粒,纳米材料由于表面与界面效应、量子尺寸效应、宏观量子隧道效应和小尺寸效应而被赋予独特的物理、化学性质。纳米材料应用于电化学传感器的研究具有广阔前景。
目前,抗菌药残留超标已成为食品生产领域的一大公害。动物源性食品中磺胺类抗菌药阳性几率大。常用的磺胺类抗菌药残留检测主要采用气质联用(GC-MASS)、高效液相色谱(HPLC)等精密仪器分析技术。尽管检测灵敏度很高,但存在仪器设备昂贵、分析程序繁琐、维护困难、分析成本高、分析周期长等弊端。随着社会对食品安全问题的关注,研究一种简便、成本较低、分析速度快、灵敏度高、适合现场分析的磺胺类抗菌药残留检测的方法是社会的迫切需求。电化学传感器具有选择性好、灵敏度高、易于小型化和批量生产、非常适合用于现场分析等优点。
本文研究了磺胺抗菌药在碳纳米管(MWCNTs)修饰电极上电化学行为,讨论了MWCNTs对磺胺抗菌药的电催化氧化机理和电流增敏机理,利用MWCNTs和OPPF6离子液体、全氟磺酸酯阳离子交换树脂Nafion、大环金属配合物钴酞菁(CoⅡPc)等功能材料的协同作用,构建用于磺胺类抗菌药检测的电化学传感器,解决了传感器在实际应用中所面临的选择性不好、灵敏度不足、使用寿命短、基体干扰等问题。并成功地将传感器用于磺胺类药物、人尿液中磺胺类抗菌药残留的检测。本论文的主要研究内容及结果如下：
1)首次以MWCNTs为电极修饰材料,制备电化学传感器,用于磺胺药物的电化学检测,显著降低了磺胺药物的电化学氧化电位,明显提高了磺胺药物的阳极电流响应,为实现磺胺类药物的高灵敏电化学检测提供科学依据。
2)分别以Pt、GC电极为基础,制备了MWCNTs修饰电极,研究了磺胺在修饰电极的电化学行为,对磺胺在修饰电极上的电极反应机理进行了探讨；对磺胺在MWCNTs修饰电极上的定量分析特性进行了探索,其线性响应范围、检测限、重现性、稳定性等指标均令人满意。
3)以OPPF6室温离子液体为MWCNTs的分散剂和固定剂,制备MWCNTs/OPPF6-GC修饰电极；MWCNTs/OPPF6-GC修饰电极有效降低了电化学测试时的背景电流,并解决了修饰电极上MWCNTs脱落的问题；基于MWCNTs电催化作用和OPPF6的溶解能力,MWCNTs/OPPF6-GC修饰电极不仅降低了抗菌药磺胺嘧啶的阳极过电位,而且使其阳极电流响应显著增强；建立了对磺胺嘧啶的计时安培电流检测方法(i-t),其检测限达到0.21μmol/L的水平；有效地消除干扰物质对检测的干扰,并成功地应用于市售药物磺胺嘧啶混悬液的含量检测,获得了令人满意的效果。
4)以Nafion为分散剂,制备MWCNTs/Nafion-GC修饰电极,并通过电化学聚合的方式将钴酞菁固定于电极表面,得到poly-CoⅡTAPc/MWCNTs/Nafion-GC修饰电极；新修饰电极制备方法解决了电极表面碳纳米管泄漏、电极使用寿命不足的问题；借助于Nafion膜的离子交换作用,对磺胺嘧啶阳离子交换富集、对阴离子还原剂(抗坏血酸、尿酸、草酸等)选择性排斥,提升了新电极对磺胺抗菌药的选择性；在多种功能材料的协同作用下,新修饰电极对磺胺嘧啶的氧化过电位得到降低,安培电流响应的灵敏度明显提升；新电极应用于磺胺嘧啶的安培电流检测,其阳极电流随系统中磺胺嘧啶浓度的增加线性增大,线性范围为0.5-43.5μmol/L,检测限达到0.17μmoVL,并成功地应用于尿液中微量磺胺嘧啶的检测。
Functional nano materials have now been extremely used for preparation of electrochemical sensors and analytical purpose. Due to their surface and interface effect, the quantum size effect, the macroscopic quantum tunnel effect and the small size effect, functional nano materials possess much fantastic physical and chemical advantages. It will be a promising avenue for application of nano materials in electrochemical sensor research.
In field of food production, residue of antimicrobial has now been a focus of the society. Because of their broad spectrum antimicrobial effect, sulfonamides are wildly added in feed stuff for treatment of animal diseases, which results in more and more animal product samples are sulfonamides residue positive. Modern instruments methods such as GC-MASS, HPLC, HPLC-FL, etc. have been successfully used for evaluation of the drug residues with the advantageous of high sensitive and accuracy. However these methods also have drawbacks of instrument expensive, procedure tedious, skilled laboratory personnel deeding, cost and time tedious. Hence, searching for rapid detection of sulfonamide residues in animal derived food is of particular significance. Electrochemical detection methods have the advantages of simple, low cost, fast response and easy to use.
In this dissertation, we aim at developing an electrochemical sensor based on carbon nanotubes (MWCNTs) functional materials for determination of sulfonamides residues. Electrocatalytic effect and high current reponse of sulfonamides on MWCNTs based electrochemical sensor were thoroughly discussed. Incorporation of MWCNTs, OPPF6ionic liquid, Nafion and cobalt phthalocyanine (CoⅡPc), high performance electrochemical sensors were designed and discussed. Shortcoming such as insufficient of selectivity and sensitivity, short working life and matrix interference were successfully resolved. And the new sensors were successfully used for the determination of sulfadiazine in drug and urine samples. In brief, the major results of the research were listed below.
1. Based on Pt disk electrode, we produced a MWCNTs-Pt modified electrode. Due to the electrocatalytic effect of MWCNTs, the over voltage of sulfanilamide oxidation was negtively shifted dramaticly, but the anode current response was highly sensitive response. And the mechanism of electrochemical reaction of sulfanilamide was also discussed.
2. Based on glassy carbon (GC) disk electrode, a MWCNTs-GC modified electrode was prepared. Due to the electrocatalytic effect of MWCNTs, the over voltage of sulfanilamide oxidation was negtively shifted dramaticly, but the anode current response was highly sensitive response. And pleased performances such as linear range, detection limit, repeatability, stability were obtained by MWCNTs-GC in sulfanilamide determination, wich would be useful for new sensor designing.
3. A MWCNTs/OPPF6-GC modified electrode was produced by using OPPF6ionic liquid as the dispersing and binding agent of MWCNTs. Owing to the performance of OPPF6ionic liquid, troubles of MWCNTs releasing and high noise current were resolved completely. Due to the electrocatalytic effect of MWCNTs and the extractive function, the anodic current of sulfadiazine was highly increased while the anodic potential dropped clearly. Hydrodynamic amperometric method (i-t) was selected for the analysis of sulfadiazine. The aodic currents obtained on MWCNTs/OPPF6-GC modified electrode were linearly responsed against the concentration of sulfadiazine in system in the range of3.3-35.4μmol/L with detection limit of0.21μmol/L. And the interference of matrix was eliminated by background subtraction. A sales sulfadiazine drug was tested by this method.
4. Nation was used as dispersive agent and binder of MWCNTs for producing MWCNTs/Nafion-GC. CoⅡTAPc was electrochemically deposited onto the surface of MWCNTs/Nafion-GC to form poly-CoⅡTAPc/MWCNTs/Nafion-GC. The new modified electrode owns advantages such as preventing MWCNTs releasing, long working life, enrichment of sulfadiazie by cation exchanging, avoiding interference of anions (ascorbic acid, urine acid, oxalic acid, etc.) by electrostatic repulsion, reducing the overvoltage of sulfadiazine. The mechanism of synergistic catalytic effect of MWCNTs, CoⅡTAPc and Nafion was discussed strictly. Hydrodynamic amperometric method (i-t) was selected for the analysis of sulfadiazine. The aodic currents obtained on poly-CoⅡTAPc/MWCNTs/Nafion-GC were linearly responsed against the concentration of sulfadiazine in system in the range of0.5-43.5μmol/L with the detection limit of0.17μmol/L. And the interference of matrix was eliminated by background subtraction. Trace level of sulfadiazine in urine samples was tested successfully by this method.
目前,抗菌药残留超标已成为食品生产领域的一大公害。动物源性食品中磺胺类抗菌药阳性几率大。常用的磺胺类抗菌药残留检测主要采用气质联用(GC-MASS)、高效液相色谱(HPLC)等精密仪器分析技术。尽管检测灵敏度很高,但存在仪器设备昂贵、分析程序繁琐、维护困难、分析成本高、分析周期长等弊端。随着社会对食品安全问题的关注,研究一种简便、成本较低、分析速度快、灵敏度高、适合现场分析的磺胺类抗菌药残留检测的方法是社会的迫切需求。电化学传感器具有选择性好、灵敏度高、易于小型化和批量生产、非常适合用于现场分析等优点。
本文研究了磺胺抗菌药在碳纳米管(MWCNTs)修饰电极上电化学行为,讨论了MWCNTs对磺胺抗菌药的电催化氧化机理和电流增敏机理,利用MWCNTs和OPPF6离子液体、全氟磺酸酯阳离子交换树脂Nafion、大环金属配合物钴酞菁(CoⅡPc)等功能材料的协同作用,构建用于磺胺类抗菌药检测的电化学传感器,解决了传感器在实际应用中所面临的选择性不好、灵敏度不足、使用寿命短、基体干扰等问题。并成功地将传感器用于磺胺类药物、人尿液中磺胺类抗菌药残留的检测。本论文的主要研究内容及结果如下：
1)首次以MWCNTs为电极修饰材料,制备电化学传感器,用于磺胺药物的电化学检测,显著降低了磺胺药物的电化学氧化电位,明显提高了磺胺药物的阳极电流响应,为实现磺胺类药物的高灵敏电化学检测提供科学依据。
2)分别以Pt、GC电极为基础,制备了MWCNTs修饰电极,研究了磺胺在修饰电极的电化学行为,对磺胺在修饰电极上的电极反应机理进行了探讨；对磺胺在MWCNTs修饰电极上的定量分析特性进行了探索,其线性响应范围、检测限、重现性、稳定性等指标均令人满意。
3)以OPPF6室温离子液体为MWCNTs的分散剂和固定剂,制备MWCNTs/OPPF6-GC修饰电极；MWCNTs/OPPF6-GC修饰电极有效降低了电化学测试时的背景电流,并解决了修饰电极上MWCNTs脱落的问题；基于MWCNTs电催化作用和OPPF6的溶解能力,MWCNTs/OPPF6-GC修饰电极不仅降低了抗菌药磺胺嘧啶的阳极过电位,而且使其阳极电流响应显著增强；建立了对磺胺嘧啶的计时安培电流检测方法(i-t),其检测限达到0.21μmol/L的水平；有效地消除干扰物质对检测的干扰,并成功地应用于市售药物磺胺嘧啶混悬液的含量检测,获得了令人满意的效果。
4)以Nafion为分散剂,制备MWCNTs/Nafion-GC修饰电极,并通过电化学聚合的方式将钴酞菁固定于电极表面,得到poly-CoⅡTAPc/MWCNTs/Nafion-GC修饰电极；新修饰电极制备方法解决了电极表面碳纳米管泄漏、电极使用寿命不足的问题；借助于Nafion膜的离子交换作用,对磺胺嘧啶阳离子交换富集、对阴离子还原剂(抗坏血酸、尿酸、草酸等)选择性排斥,提升了新电极对磺胺抗菌药的选择性；在多种功能材料的协同作用下,新修饰电极对磺胺嘧啶的氧化过电位得到降低,安培电流响应的灵敏度明显提升；新电极应用于磺胺嘧啶的安培电流检测,其阳极电流随系统中磺胺嘧啶浓度的增加线性增大,线性范围为0.5-43.5μmol/L,检测限达到0.17μmoVL,并成功地应用于尿液中微量磺胺嘧啶的检测。
Functional nano materials have now been extremely used for preparation of electrochemical sensors and analytical purpose. Due to their surface and interface effect, the quantum size effect, the macroscopic quantum tunnel effect and the small size effect, functional nano materials possess much fantastic physical and chemical advantages. It will be a promising avenue for application of nano materials in electrochemical sensor research.
In field of food production, residue of antimicrobial has now been a focus of the society. Because of their broad spectrum antimicrobial effect, sulfonamides are wildly added in feed stuff for treatment of animal diseases, which results in more and more animal product samples are sulfonamides residue positive. Modern instruments methods such as GC-MASS, HPLC, HPLC-FL, etc. have been successfully used for evaluation of the drug residues with the advantageous of high sensitive and accuracy. However these methods also have drawbacks of instrument expensive, procedure tedious, skilled laboratory personnel deeding, cost and time tedious. Hence, searching for rapid detection of sulfonamide residues in animal derived food is of particular significance. Electrochemical detection methods have the advantages of simple, low cost, fast response and easy to use.
In this dissertation, we aim at developing an electrochemical sensor based on carbon nanotubes (MWCNTs) functional materials for determination of sulfonamides residues. Electrocatalytic effect and high current reponse of sulfonamides on MWCNTs based electrochemical sensor were thoroughly discussed. Incorporation of MWCNTs, OPPF6ionic liquid, Nafion and cobalt phthalocyanine (CoⅡPc), high performance electrochemical sensors were designed and discussed. Shortcoming such as insufficient of selectivity and sensitivity, short working life and matrix interference were successfully resolved. And the new sensors were successfully used for the determination of sulfadiazine in drug and urine samples. In brief, the major results of the research were listed below.
1. Based on Pt disk electrode, we produced a MWCNTs-Pt modified electrode. Due to the electrocatalytic effect of MWCNTs, the over voltage of sulfanilamide oxidation was negtively shifted dramaticly, but the anode current response was highly sensitive response. And the mechanism of electrochemical reaction of sulfanilamide was also discussed.
2. Based on glassy carbon (GC) disk electrode, a MWCNTs-GC modified electrode was prepared. Due to the electrocatalytic effect of MWCNTs, the over voltage of sulfanilamide oxidation was negtively shifted dramaticly, but the anode current response was highly sensitive response. And pleased performances such as linear range, detection limit, repeatability, stability were obtained by MWCNTs-GC in sulfanilamide determination, wich would be useful for new sensor designing.
3. A MWCNTs/OPPF6-GC modified electrode was produced by using OPPF6ionic liquid as the dispersing and binding agent of MWCNTs. Owing to the performance of OPPF6ionic liquid, troubles of MWCNTs releasing and high noise current were resolved completely. Due to the electrocatalytic effect of MWCNTs and the extractive function, the anodic current of sulfadiazine was highly increased while the anodic potential dropped clearly. Hydrodynamic amperometric method (i-t) was selected for the analysis of sulfadiazine. The aodic currents obtained on MWCNTs/OPPF6-GC modified electrode were linearly responsed against the concentration of sulfadiazine in system in the range of3.3-35.4μmol/L with detection limit of0.21μmol/L. And the interference of matrix was eliminated by background subtraction. A sales sulfadiazine drug was tested by this method.
4. Nation was used as dispersive agent and binder of MWCNTs for producing MWCNTs/Nafion-GC. CoⅡTAPc was electrochemically deposited onto the surface of MWCNTs/Nafion-GC to form poly-CoⅡTAPc/MWCNTs/Nafion-GC. The new modified electrode owns advantages such as preventing MWCNTs releasing, long working life, enrichment of sulfadiazie by cation exchanging, avoiding interference of anions (ascorbic acid, urine acid, oxalic acid, etc.) by electrostatic repulsion, reducing the overvoltage of sulfadiazine. The mechanism of synergistic catalytic effect of MWCNTs, CoⅡTAPc and Nafion was discussed strictly. Hydrodynamic amperometric method (i-t) was selected for the analysis of sulfadiazine. The aodic currents obtained on poly-CoⅡTAPc/MWCNTs/Nafion-GC were linearly responsed against the concentration of sulfadiazine in system in the range of0.5-43.5μmol/L with the detection limit of0.17μmol/L. And the interference of matrix was eliminated by background subtraction. Trace level of sulfadiazine in urine samples was tested successfully by this method.
引文
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