新型化学修饰电极的构建及在食品分析中的一些应用
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摘要
运用纳米材料,如石墨烯、纳米金、有机聚合膜及其相关的复合材料作为修饰电极的新材料是当前化学修饰电极发展的新方向,对于提高分析方法的灵敏度和选择性具有重要意义。基于这种考虑,本文构建了几种新型的化学修饰电极,并应用于食品中瘦肉精、人工合成抗氧化剂和香料等的分析,具体的内容与结果如下：
1.基于纳米金修饰的玻碳电极(AuNPs/GCE)和化学计量学MVCl,研究和发展了一种同时分析三种p2激动剂-莱克多巴胺、沙丁胺醇和克伦特罗复杂体系的新方法。与裸玻碳电极(GCE)相比,AuNPs/GCE电极对这三种p2激动剂有很好的电催化性能,具体表现为三种物质的峰电流大大增加,峰电位负移。莱克多巴胺、沙丁胺醇和克伦特罗的峰电流随浓度变化呈正比关系,线性范围分别为0.005～0.075μg mL-1,0.010～0.150μg mL-1和0.004～0.064μg mE-1,其检测限分别为2.4ng mL-1,5.8ng mE-1和2.6ng mE-1。由于三种药物的结构相似,它们的微分脉冲伏安曲线存在重叠,对它们进行同时定量分析存在一定困难,而采用化学计量学方法MVCl(如PLS1)建立合适的校正模型,进而对重叠波谱进行解析,获得了满意的定量结果,其相对预报偏差和百分回收率分别为7.0%和97.6%。该方法被用于分析猪肉、猪肝和猪饲料样品中三种β2激动剂,并与HPLC标准方法相比较,结果比较满意。
2.基于纳米金修饰电极(AuNPs/GCE)和一阶导数的校正模型,研究和发展了一种同时分析三种抗氧化剂BHA、BHT和TBHQ的方法。修饰电极通过扫描电子显微镜(SEM)表征,实验结果表明修饰电极对三种抗氧化剂BHA、BHT和TBHQ表现出良好的电化学催化作用,主要表现在峰电流增加、峰电位负移;本研究通过循环伏安法(CV)研究了三种抗氧化剂的电化学反应机理,结果发现BHA和TBHQ的氧化产物是相同的。在最佳实验条件下,BHA和BHT的氧化峰完全分离,但还存在基线干扰,由此本文提出了一种基于一阶导数数据前处理的化学计量学校正模型用于同时分析混合物的BHA、BHT和TBHQ方法,其线性范围分别为0.10～1.50μg mE-1,0.20～2.20μg mL-1和0.20～2.80pgmL-1,检测限分别为0.039μg mL-1,0.080tg mL-1和0.079μg mL-1。该方法被用于分析几个食用油样品中三种抗氧化剂,与标准方法HPLC的结果进行比较,结果满意。
3.基于电聚合一种荧光试剂7-(2,4-二羟基-5-羧基苯偶氮)-8-羟基喹啉-5-磺酸(DHCBAQS)在石墨烯-nafion修饰的玻碳电极上,构建了一种新型的修饰电极；运用扫描电镜(SEM)对修饰的电极进行了微观形貌的表征,利用循环伏安法(CV)和电化学阻抗谱图(EIS)对电极的修饰过程进行了表征。考察了三种硝基苯胺同分异构体在各种电极上的电化学行为,结果表明Poly-DHCBAQS/graphene-nafion/GCE电极对这三种分析物表现出良好的电催化性能。在修饰电极上,邻、间、对硝基苯胺同分异构体的峰电流与其浓度呈良好的线性关系,其线性范围分别为0.05～0.55μg mL-1,0.05-0.60μg mL-1和0.05-0.60μg mL-1,检测限分别为0.025μg mL-1,0.021μg mE-1和0.019μg mL-1。由于三种药物的结构相似,它们的微分脉冲伏安曲线存在重叠,对它们进行同时定量分析存在一定困难,采用化学计量学方法PLS和PCR所建立的校正模型用于混合物的解析,其相对预报偏差分别为9.04%和9.23%,回收率分别为]01.0%和101.7%。此外,新制备的电极被成功用于水样和废水样品中三种硝基苯胺的同时分析。
4.基于电聚合一种荧光分子4,5-二羟基-3-[(2-羟基-5-苯磺酸钠)偶氮]-2,7-萘二磺酸钠(酸性铬蓝K(ACBK))于石墨烯-nafion修饰的玻碳电极上制备了Poly-ACBK/graphene-nafion/GCE电极。运用原子力显微镜(AFM)对修饰的电极进行了微观形貌的表征,利用循环伏安法(CV)和电化学阻抗谱图(EIS)对电极的修饰过程进行了表征。在修饰电极上,八种p受体激动剂(克伦特罗、特步他林、莱克多巴胺、沙丁胺醇、多巴胺、多巴酚丁胺、肾上腺素、异丙肾上腺)的线性扫描伏图的峰电流与其浓度呈正比关系,其线性范围和检测限分别为1-36ng mL-1和0.58-1.44ng mL-1。此外,新制备的电极表现出好的稳定性和重现性,成功地用于猪肉样品中克伦特罗的分析,获得了比较满意的结果。
5.基于电沉积硫酸铜和氯金酸的混合溶液制备了铜掺杂纳米金修饰电极(cu@AuNPs/GCE),研究了丁香酚在该修饰电极上的电化学行为,结果表明该电极对丁香酚有良好的电催化作用,而为了证实邻甲氧基苯酚这类物质电化学反应机理,还考察了邻苯二酚、愈创木酚和香草醛的电化学行为,从而推断出这类物质在Cu@AuNPs/GCE电极上电化学反应机理。在该修饰电极上,丁香酚线性扫描伏安图的峰电流与其浓度呈线性关系,其线性范围为0.05～0.80μg mL-1,检测限为0.042μg mL-1。此外,该修饰电极被用于食品中丁香酚的测定,结果满意。
This paper is to apply nano-materials, such as graphene, gold nanoparticles, organic polymeric membranes and their composite materials to the construction of electrode, which is a new direction for chemically modified electrodes and has an important significance to improve the sensitivity and selectivity of analysis. Based on this, different novel chemically modified electrodes were constructed and applied to some food analysis (β-agonists, synthetic antioxidants and spice). The main contents and conclusions are as follows:
1. An electrochemical method involving a gold nanoparticle modified glassy carbon electrode (AuNPs/GCE), was researched and developed for the simultaneous analysis of three (32-agonists, ractopamine (RAC), salbutamol (SAL) and clenbuterol (CLB). The three analytes were electrocatalytically oxidized at the AuNP/GCE, which enhanced the oxidation peak current and influenced the shift of the oxidation potentials to lower values in comparison with the analysis involving only the GCE. The peak currents associated with RAC, SAL and CLB measurements were linear as a function of their concentrations (ranges within0.005～0.075μg mL-1,0.010～0.150μg mL-1and0.004～0.064μg mL-1for RAC, SAL and CLB, respectively); the detection limits for RAC, SAL and CLB were2.4,5.8and2.6ng￣mL-1, respectively. The differential pulse stripping voltammetry (DPSV)voltammograms from the drug mixture produced complex, overlapping profiles, and chemometrics methods were applied for calibration modeling. It was shown that satisfactory quantitative results were obtained with the use of the MVC1package of chemometrics methods e.g the PLS1calibration model produced a relative prediction error (PRET) of7.0%and an average recovery of97.6%. The above AuNP/GCE was successfully employed for the simultaneous analysis of RAC, SAL and CLB in pork meat, liver and pig feed samples.
2. The electrochemical behaviors of three antioxidants:butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT) and butylated hydroquinone (TBHQ) at a gold nanoparticles modified glassy carbon electrode (AuNPs/GCE) were investigated. The modified electrode was characterized by scanning electron microscope (SEM). The experimental results indicated that the modified electrode exhibited an excellent electrocatalytic activity towards the redox reactions of BHA, BHT and TBHQ, testified by the increased redox peak currents and shifted potentials, and in addition, the oxidation products of BHA and TBHQ were found to be the same. The experimental conditions were optimized and the oxidation peaks of BHA and BHT were clearly separated. Based on this, an electrochemical method was proposed to simultaneously determine the BHA, BHT and TBHQ in mixtures by first derivative voltammetry, with linear concentration ranges of0.10-1.50μg mLL1,0.20～2.20μg mL-1and0.20～2.80jig mL-1, and detection limits of0.039,0.080and0.079μg mL-1, for BHA, BHT and TBHQ, respectively. The proposed method was successfully used for the analysis of the three analytes in edible oil samples.
3. A novel modified electrode was constructed by the electro-polymerization of7-[(2,4-dihydroxy-5-carboxybenzene)azo]-8-hydroxyquinoline-5-sulfonic acid (DHCBAQS) at a graphene-nafion modified glassy carbon electrode (GCE). The construction process was performed stepwise and at each step the electrochemical characteristics were investigated particularly with respect to the oxidation of the three noxious analytes,2-nitroaniline (2-NA),3-nitroaniline (3-NA),4-nitroaniline (4-NA); the electrode treated with the fluorescence reagent DHCBAQS perfomed best. At this electrode, the differential pulse voltammetry peak currents of the three isomers-2-NA,3-NA and4-NA increased linearly with their concentrations in the range of0.05～0.55μg mL-1,0.05～0.60μg mL-1and0.05～0.60μg mL-1, respectively, and their corresponding limits of detection (LODs) were0.025,0.021and0.019μg mL-1. Furthermore, satisfactory results were obtained when this electrode was applied for the simultaneous quantitative analysis of the nitroaniline isomer mixtures by Principal component regression (PCR) and Partial least squares (PLS) as calibration methods (relative prediction error (PRET)-9.04%and9.23%) and average recoveries (101.0%and101.7%), respectively. The above novel poly-DHCBAQS/graphene-nafion/GCE was successfully employed for the simultaneous analysis of the three noxious nitroaniline isomers in water and sewage samples.
4. A new modified electrode was constructed by the electro-polymerization of4,5-dihydroxy-3-[(2-hydroxy-5-sulfophenyl)azo]-2,7-naphthalenedisulfonic acid trisodium salt (acid chrome blue K (ACBK)) at a graphene-nafion modified glassy carbon electrode (GCE). The electrode was investigated by the electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and atomic force microscope (AFM) techniques, and the results were interpreted and compared at each stage of the electrode construction. At this modified electrode, the linear sweep voltammetry peak currents of the eight β-agonists (clenbuterol, terbutaline. ractopamine, salbutamol, dopamine, dobutamine, adrenaline and isoprenaline) increased linearly with their concentrations in the range of1.0-36.0ng mL-1, respectively, and their corresponding limits of detection (LODs) were0.58-1.46ng mL-1. This electrode showed satisfactory reproducibility and stability, and was used successfully for the quantitative analysis of clenbuterol in pork samples.
5. A new modified electrode was constructed by the electro-deposition of the mixture of CuSO4and HAuCl4at a glassy carbon electrode (GCE). The eugenol was electrocatalytically oxidized at the Cu@AuNP/GCE, which enhanced the oxidation peak current and influenced the shift of the oxidation potentials to lower values in comparison with the analysis involving only the GCE. In order to confirm the electrochemical reaction mechanism for o-methoxy phenol, the electrochemical behavior for catechol, guaiacol and vanillin were studied. Based on this, the electrochemical reaction mechanism for o-methoxy phenols was inferred. At this modified electrode, the linear sweep voltammetry peak current of eugenol increased linearly with its concentration in the range of0.05-0.80μg mL-1, and its corresponding limit of detection (LOD) were0.042μg mL-1. Moreover, The above Cu@AuNP/GCE was successfully employed for the analysis of eugenol in food samples.
1.基于纳米金修饰的玻碳电极(AuNPs/GCE)和化学计量学MVCl,研究和发展了一种同时分析三种p2激动剂-莱克多巴胺、沙丁胺醇和克伦特罗复杂体系的新方法。与裸玻碳电极(GCE)相比,AuNPs/GCE电极对这三种p2激动剂有很好的电催化性能,具体表现为三种物质的峰电流大大增加,峰电位负移。莱克多巴胺、沙丁胺醇和克伦特罗的峰电流随浓度变化呈正比关系,线性范围分别为0.005～0.075μg mL-1,0.010～0.150μg mL-1和0.004～0.064μg mE-1,其检测限分别为2.4ng mL-1,5.8ng mE-1和2.6ng mE-1。由于三种药物的结构相似,它们的微分脉冲伏安曲线存在重叠,对它们进行同时定量分析存在一定困难,而采用化学计量学方法MVCl(如PLS1)建立合适的校正模型,进而对重叠波谱进行解析,获得了满意的定量结果,其相对预报偏差和百分回收率分别为7.0%和97.6%。该方法被用于分析猪肉、猪肝和猪饲料样品中三种β2激动剂,并与HPLC标准方法相比较,结果比较满意。
2.基于纳米金修饰电极(AuNPs/GCE)和一阶导数的校正模型,研究和发展了一种同时分析三种抗氧化剂BHA、BHT和TBHQ的方法。修饰电极通过扫描电子显微镜(SEM)表征,实验结果表明修饰电极对三种抗氧化剂BHA、BHT和TBHQ表现出良好的电化学催化作用,主要表现在峰电流增加、峰电位负移;本研究通过循环伏安法(CV)研究了三种抗氧化剂的电化学反应机理,结果发现BHA和TBHQ的氧化产物是相同的。在最佳实验条件下,BHA和BHT的氧化峰完全分离,但还存在基线干扰,由此本文提出了一种基于一阶导数数据前处理的化学计量学校正模型用于同时分析混合物的BHA、BHT和TBHQ方法,其线性范围分别为0.10～1.50μg mE-1,0.20～2.20μg mL-1和0.20～2.80pgmL-1,检测限分别为0.039μg mL-1,0.080tg mL-1和0.079μg mL-1。该方法被用于分析几个食用油样品中三种抗氧化剂,与标准方法HPLC的结果进行比较,结果满意。
3.基于电聚合一种荧光试剂7-(2,4-二羟基-5-羧基苯偶氮)-8-羟基喹啉-5-磺酸(DHCBAQS)在石墨烯-nafion修饰的玻碳电极上,构建了一种新型的修饰电极；运用扫描电镜(SEM)对修饰的电极进行了微观形貌的表征,利用循环伏安法(CV)和电化学阻抗谱图(EIS)对电极的修饰过程进行了表征。考察了三种硝基苯胺同分异构体在各种电极上的电化学行为,结果表明Poly-DHCBAQS/graphene-nafion/GCE电极对这三种分析物表现出良好的电催化性能。在修饰电极上,邻、间、对硝基苯胺同分异构体的峰电流与其浓度呈良好的线性关系,其线性范围分别为0.05～0.55μg mL-1,0.05-0.60μg mL-1和0.05-0.60μg mL-1,检测限分别为0.025μg mL-1,0.021μg mE-1和0.019μg mL-1。由于三种药物的结构相似,它们的微分脉冲伏安曲线存在重叠,对它们进行同时定量分析存在一定困难,采用化学计量学方法PLS和PCR所建立的校正模型用于混合物的解析,其相对预报偏差分别为9.04%和9.23%,回收率分别为]01.0%和101.7%。此外,新制备的电极被成功用于水样和废水样品中三种硝基苯胺的同时分析。
4.基于电聚合一种荧光分子4,5-二羟基-3-[(2-羟基-5-苯磺酸钠)偶氮]-2,7-萘二磺酸钠(酸性铬蓝K(ACBK))于石墨烯-nafion修饰的玻碳电极上制备了Poly-ACBK/graphene-nafion/GCE电极。运用原子力显微镜(AFM)对修饰的电极进行了微观形貌的表征,利用循环伏安法(CV)和电化学阻抗谱图(EIS)对电极的修饰过程进行了表征。在修饰电极上,八种p受体激动剂(克伦特罗、特步他林、莱克多巴胺、沙丁胺醇、多巴胺、多巴酚丁胺、肾上腺素、异丙肾上腺)的线性扫描伏图的峰电流与其浓度呈正比关系,其线性范围和检测限分别为1-36ng mL-1和0.58-1.44ng mL-1。此外,新制备的电极表现出好的稳定性和重现性,成功地用于猪肉样品中克伦特罗的分析,获得了比较满意的结果。
5.基于电沉积硫酸铜和氯金酸的混合溶液制备了铜掺杂纳米金修饰电极(cu@AuNPs/GCE),研究了丁香酚在该修饰电极上的电化学行为,结果表明该电极对丁香酚有良好的电催化作用,而为了证实邻甲氧基苯酚这类物质电化学反应机理,还考察了邻苯二酚、愈创木酚和香草醛的电化学行为,从而推断出这类物质在Cu@AuNPs/GCE电极上电化学反应机理。在该修饰电极上,丁香酚线性扫描伏安图的峰电流与其浓度呈线性关系,其线性范围为0.05～0.80μg mL-1,检测限为0.042μg mL-1。此外,该修饰电极被用于食品中丁香酚的测定,结果满意。
This paper is to apply nano-materials, such as graphene, gold nanoparticles, organic polymeric membranes and their composite materials to the construction of electrode, which is a new direction for chemically modified electrodes and has an important significance to improve the sensitivity and selectivity of analysis. Based on this, different novel chemically modified electrodes were constructed and applied to some food analysis (β-agonists, synthetic antioxidants and spice). The main contents and conclusions are as follows:
1. An electrochemical method involving a gold nanoparticle modified glassy carbon electrode (AuNPs/GCE), was researched and developed for the simultaneous analysis of three (32-agonists, ractopamine (RAC), salbutamol (SAL) and clenbuterol (CLB). The three analytes were electrocatalytically oxidized at the AuNP/GCE, which enhanced the oxidation peak current and influenced the shift of the oxidation potentials to lower values in comparison with the analysis involving only the GCE. The peak currents associated with RAC, SAL and CLB measurements were linear as a function of their concentrations (ranges within0.005～0.075μg mL-1,0.010～0.150μg mL-1and0.004～0.064μg mL-1for RAC, SAL and CLB, respectively); the detection limits for RAC, SAL and CLB were2.4,5.8and2.6ng￣mL-1, respectively. The differential pulse stripping voltammetry (DPSV)voltammograms from the drug mixture produced complex, overlapping profiles, and chemometrics methods were applied for calibration modeling. It was shown that satisfactory quantitative results were obtained with the use of the MVC1package of chemometrics methods e.g the PLS1calibration model produced a relative prediction error (PRET) of7.0%and an average recovery of97.6%. The above AuNP/GCE was successfully employed for the simultaneous analysis of RAC, SAL and CLB in pork meat, liver and pig feed samples.
2. The electrochemical behaviors of three antioxidants:butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT) and butylated hydroquinone (TBHQ) at a gold nanoparticles modified glassy carbon electrode (AuNPs/GCE) were investigated. The modified electrode was characterized by scanning electron microscope (SEM). The experimental results indicated that the modified electrode exhibited an excellent electrocatalytic activity towards the redox reactions of BHA, BHT and TBHQ, testified by the increased redox peak currents and shifted potentials, and in addition, the oxidation products of BHA and TBHQ were found to be the same. The experimental conditions were optimized and the oxidation peaks of BHA and BHT were clearly separated. Based on this, an electrochemical method was proposed to simultaneously determine the BHA, BHT and TBHQ in mixtures by first derivative voltammetry, with linear concentration ranges of0.10-1.50μg mLL1,0.20～2.20μg mL-1and0.20～2.80jig mL-1, and detection limits of0.039,0.080and0.079μg mL-1, for BHA, BHT and TBHQ, respectively. The proposed method was successfully used for the analysis of the three analytes in edible oil samples.
3. A novel modified electrode was constructed by the electro-polymerization of7-[(2,4-dihydroxy-5-carboxybenzene)azo]-8-hydroxyquinoline-5-sulfonic acid (DHCBAQS) at a graphene-nafion modified glassy carbon electrode (GCE). The construction process was performed stepwise and at each step the electrochemical characteristics were investigated particularly with respect to the oxidation of the three noxious analytes,2-nitroaniline (2-NA),3-nitroaniline (3-NA),4-nitroaniline (4-NA); the electrode treated with the fluorescence reagent DHCBAQS perfomed best. At this electrode, the differential pulse voltammetry peak currents of the three isomers-2-NA,3-NA and4-NA increased linearly with their concentrations in the range of0.05～0.55μg mL-1,0.05～0.60μg mL-1and0.05～0.60μg mL-1, respectively, and their corresponding limits of detection (LODs) were0.025,0.021and0.019μg mL-1. Furthermore, satisfactory results were obtained when this electrode was applied for the simultaneous quantitative analysis of the nitroaniline isomer mixtures by Principal component regression (PCR) and Partial least squares (PLS) as calibration methods (relative prediction error (PRET)-9.04%and9.23%) and average recoveries (101.0%and101.7%), respectively. The above novel poly-DHCBAQS/graphene-nafion/GCE was successfully employed for the simultaneous analysis of the three noxious nitroaniline isomers in water and sewage samples.
4. A new modified electrode was constructed by the electro-polymerization of4,5-dihydroxy-3-[(2-hydroxy-5-sulfophenyl)azo]-2,7-naphthalenedisulfonic acid trisodium salt (acid chrome blue K (ACBK)) at a graphene-nafion modified glassy carbon electrode (GCE). The electrode was investigated by the electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and atomic force microscope (AFM) techniques, and the results were interpreted and compared at each stage of the electrode construction. At this modified electrode, the linear sweep voltammetry peak currents of the eight β-agonists (clenbuterol, terbutaline. ractopamine, salbutamol, dopamine, dobutamine, adrenaline and isoprenaline) increased linearly with their concentrations in the range of1.0-36.0ng mL-1, respectively, and their corresponding limits of detection (LODs) were0.58-1.46ng mL-1. This electrode showed satisfactory reproducibility and stability, and was used successfully for the quantitative analysis of clenbuterol in pork samples.
5. A new modified electrode was constructed by the electro-deposition of the mixture of CuSO4and HAuCl4at a glassy carbon electrode (GCE). The eugenol was electrocatalytically oxidized at the Cu@AuNP/GCE, which enhanced the oxidation peak current and influenced the shift of the oxidation potentials to lower values in comparison with the analysis involving only the GCE. In order to confirm the electrochemical reaction mechanism for o-methoxy phenol, the electrochemical behavior for catechol, guaiacol and vanillin were studied. Based on this, the electrochemical reaction mechanism for o-methoxy phenols was inferred. At this modified electrode, the linear sweep voltammetry peak current of eugenol increased linearly with its concentration in the range of0.05-0.80μg mL-1, and its corresponding limit of detection (LOD) were0.042μg mL-1. Moreover, The above Cu@AuNP/GCE was successfully employed for the analysis of eugenol in food samples.
引文
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