聚磺胺嘧啶修饰电极伏安法测定对乙酰氨基酚

利用循环伏安法制备了聚磺胺嘧啶修饰电极, 研究了对乙酰氨基酚在该修饰电极上的电化学行为. 该电极对对乙酰氨基酚有较强的电催化作用. 在pH 9.0的PBS缓冲溶液中, 用循环伏安法和差分脉冲伏安法在该电极上测定了对乙酰氨基酚, 其线性范围分别为4.0×10-6～3.0×10-4 mol/L和2.0×10-7～1.0×10-5 mol/L, 检出限分别为9.0×10-7 mol/L和8.0×10-8 mol/L.     

银掺杂聚L-酪氨酸修饰电极的制备及对尿酸的测定

利用循环伏安法将银和L-酪氨酸聚合修饰在玻碳电极表面,制成银掺杂聚L-酪氨酸(Ag-PLT/GCE)修饰电极,研究了尿酸在该电极上的电化学行为,建立了循环伏安法测定尿酸的新方法。在pH=3.0的磷酸盐缓冲溶液中,扫描速率为100mV/s时,尿酸在该修饰电极上产生一氧化峰,Epa=0.637V(vs.Ag/AgCl)。用循环伏安法进行测定时,峰电流与尿酸浓度在8.0×10-7～1.0×10-5mol/L和1.0×10-5～1.0×10-4mol/L范围内呈良好的线性关系,检出限为3.0×10-7mol/L。方法用于尿样中尿酸的测定,结果满意。     

聚对氨基酚修饰电极的制备及其对尿酸的催化氧化作用

采用循环伏安法制备了聚对氨基酚薄膜修饰玻碳电极, 研究了尿酸在该修饰电极上的电化学行为, 建立了循环伏安法测定尿酸的新方法. 研究发现: 在pH 5.6的磷酸盐缓冲溶液中, 以0.1 mol/L KCl作支持电解质, 聚对氨基酚修饰电极对尿酸存在灵敏的氧化作用, 应用循环伏安法对尿酸进行定量分析, 线性范围为1.0×10-6～4.0×10-5 mol/L, 检出限为8×10-7 mol/L. 对2.0×10-5 mol/L尿酸平行测定5次, 相对标准偏差为4.0%.     

尿酸在聚L-苯丙氨酸修饰电极上的伏安测定

采用循环伏安法制备了聚L-苯丙氨酸薄膜修饰玻碳电极,研究了尿酸在该修饰电极上的电化学行为,循环伏安法测定了尿酸. 研究发现,在pH=5.6的磷酸盐缓冲溶液中,尿酸在聚L-苯丙氨酸修饰电极上于0.43 V处产生1灵敏的氧化峰;循环伏安法测定其氧化峰电流与尿酸的浓度在2.0×10-6～3.0×10-4 mol/L呈良好的线性关系,检出限为1×10-6 mol/L. 对1.0×10-5 mol/L尿酸平行测定5次,相对标准偏差为3.0%. 该聚合物修饰电极制作简单,重现性好,可用于尿液中尿酸的测定,结果令人满意.     

黄嘌呤和尿酸在修饰电极上的电化学行为及测定研究

用循环伏安法制备了银掺杂聚L-赖氨酸修饰玻碳电极,并对修饰电极表面进行了表征,研究了黄嘌呤和尿酸在该修饰电极上的电化学行为,建立了循环伏安法和示差脉冲伏安法同时测定黄嘌呤和尿酸的新方法。研究表明,修饰电极对尿酸和黄嘌呤的氧化具有较好的电催化活性,在pH 3.0磷酸盐缓冲溶液中,黄嘌呤和尿酸在银掺杂聚L-赖氨酸修饰电极上的氧化峰电位分别为0.980和0.600 V,两者的峰电位差达0.380 V。在最优实验条件下,用差分脉冲伏安法同时测定黄嘌呤和尿酸的线性范围为1.0×10-6~2.5×10-4mol/L,检出限为5.0×10-7mol/L。用于人尿样中黄嘌呤和尿酸的测定,获得满意结果。     

聚结晶紫薄膜修饰电极测定尿酸

利用循环伏安法制备了聚结晶紫薄膜修饰电极(PCVE) ,详细研究了该修饰电极对生物分子尿酸 (UA)的电催化作用。结果表明 ,PCVE对UA具有较强的电催化作用 ,并且对抗坏血酸(AA)具有较强的抗干扰作用 ,允许高达1000倍以上AA存在而不干扰痕量UA的测定。将PCVE结合差分脉冲伏安(DPV)技术 ,对UA的检测线性范围为5.0×10 -7～5.0×10 -5mol/L,检出限达7.5×10 -8mol/L。将该法用于尿液中尿酸的测定 ,取得满意结果     

Nafion-离子液体-修饰碳糊电极在抗坏血酸和尿酸存在下选择性测定多巴胺

用Nafion和亲水性离子液体溴化1-辛基-3-甲基咪唑([OMIM]Br)作修饰剂制作了Nafion-离子液体-修饰碳糊电极;在0.1 mol/L磷酸盐缓冲溶液(pH 7.40)中,用循环伏安法(CV)和方波伏安法(SWV)研究了多巴胺在该修饰电极上的电化学行为,建立了抗坏血酸和尿酸存在下选择性测定多巴胺的新方法.研究表明,该修饰电极降低了多巴胺氧化、还原反应的过电位,增大了其氧化、还原反应的峰电流,而抗坏血酸和尿酸在该修饰电极上无响应;在方波伏安曲线上,多巴胺的氧化电流与其浓度在3.0×10-8～2.0×10-6 mol/L范围内呈线性关系,检出限为1.0×10-8 mol/L.该法可用于注射液和模拟生物样品中多巴胺的测定.     

银掺杂聚L-天冬氨酸修饰电极的制备及对多巴胺的测定

利用循环伏安法将银与L-天冬氨酸聚合修饰在玻碳电极表面,制成银掺杂聚L-天冬氨酸修饰电极,研究了多巴胺在此电极上的电化学行为,建立了循环伏安法测定多巴胺的新方法.在磷酸盐缓冲溶液(PBS, pH 7.0)中,扫描速率为50 mV/s时,多巴胺在修饰电极上产生一对氧化还原峰,Epa=0.191 V,Epc=0.161 V.用循环伏安法进行测定时,峰电流与多巴胺浓度分别在3.0×10-7 ～1.0×10-5 mol/L和1.0×10-5 ～5.0×10-4 mol/L内呈良好的线性关系; 检出限为5.0×10-8 mol/L.用于药物和尿样中多巴胺的测定,结果满意.     

聚L-甲硫氨酸修饰电极的制备及对尿酸的测定

在pH9.5的磷酸盐缓冲溶液中,利用循环伏安(CV)法制备了聚L-甲硫氨酸修饰玻碳电极(PLMet/GC/CME)。研究了尿酸(UA)在该电极上的电化学行为,建立了伏安法测定UA的新方法。在pH5.0的磷酸缓冲溶液中,扫描速率为200 mV/s,循环扫描电位在-0.3~1.0 V时,UA在PLMet/GC/CME上产生一个灵敏的氧化峰,峰电位位于0.52 V(vs.Ag/AgCl)。用CV法、线性扫描伏安(LSV)法和示差脉冲伏安(DPV)法对UA进行测定,测定的线性范围分别为2.50×10-6~1.00×10-4mol/L、5.00×10-6~1.00×10-4mol/L和8.00×10-7~1.00×10-4mol/L;检出限分别为8.0×10-7mol/L(CV、LSV法)和5.0×10-7mol/L(DPV法)。用LSV法对尿样中的UA进行测定,结果满意。     

聚L-酪氨酸修饰电极的制备及对多巴胺的测定

用循环伏安法制备了聚L 酪氨酸修饰玻碳电极,研究了多巴胺在聚L 酪氨酸修饰电极上的电化学行为,建立了循环伏安法测定痕量多巴胺的新方法。多巴胺在pH7.0的磷酸盐缓冲溶液中,在聚L 酪氨酸修饰玻碳电极上产生一对灵敏的氧化还原峰,峰电位分别为Epa=189mV,Epc=131mV。循环伏安法测定多巴胺的线性范围为1.0×10-3～1.0×10-8mol/L,检出限:1.0×10-9mol/L。方法可用于药剂中多巴胺的测定。     

Voltammetric determination of salicylic acid in pharmaceuticals formulations of acetylsalicylic acid

The electrochemical oxidation of salicylic acid (SA) has been studied on a glassy carbon electrode using cyclic voltammetry and differential pulse voltammetric (DPV) method. SA gives a single irreversible oxidation wave over the wide pH range studied. The irreversibility of the electrode process was verified by different criteria. The mechanism of oxidation is discussed. Using differential pulse voltammetry, SA yielded a well-defined voltammetric response in Britton-Robinson buffer solution, pH 2.37 at 1.088 V (versus Ag/AgCl). The method was linear over the SA concentration range: 1-60 μg ml⁻¹. The method was successfully applied for the analysis of SA as a hydrolysis product, in solid pharmaceutical formulations containing acetylsalicylic acid (ASA).     

聚邻氨基对酚磺酸修饰电极测定尿酸

尿酸(UA)是核蛋白和核酸的代谢产物,人体内尿酸的水平与肝脏疾患[1]、肾病[2]以及心血管疾病[3]等有着密切的关系.因此,对人体体液中尿酸的定量分析无论在药物控制方面还是在临床诊断方面都具有重要意义.     

Electroanalytical behaviour of 5-nitroorotic acid

The electroanalytical behaviour of 5-nitroorotic acid has been studied at several pH values, using several techniques (DC and DP polarography and CV). The 5-nitroorotic acid undergoes five irreversible diffusion-controlled reduction waves over entire pH range considered. The optimum conditions for determination of 5-nitroorotic acid-with the above technique are also studied.     

Voltammetric determination of hafnium with calconcarboxylic acid

The interaction of Hf(IV) with calconcarboxylic acid (1-(2-hydroxy-4-sulfo-1-naphtylazo)-3-naphtolic acid) was investigated by cyclic voltammetry varying various factors (pH, ionic strength, contents of ethanol and scan rate). Optimal conditions of Hf(IV) determination in the presence of calconcarboxylic acid were found: acetic buffer solution pH 2.6, scan rate 0.5 Vs⁻¹. The detection limit of Hf(IV) concentration was 2.46 × 10⁻⁷ mol L⁻¹. The influence of foreign ions on the Hf(IV) determination was studied. It was established that some metals like cadmium, nickel, zinc, copper and titanium could be determined with Hf(IV) simultaneously. The method of voltammetric determination of hafnium was tested on model solutions and used in the determination of Hf(IV) in terbium-base alloy.     

Electrochemical sensing of melamine with 3,4-dihydroxyphenylacetic acid as recognition element

A new electrochemical sensor for melamine with 3,4-dihydroxyphenylacetic acid as the recognition element is established. The results of Fourier Transform Infrared (FT-IR) spectra demonstrate that melamine may interact with 3,4-dihydroxyphenylacetic acid to form a complex mainly through the hydrogen-bonding interaction. The electrochemical behavior of 3,4-dihydroxyphenylacetic acid in the presence of melamine was studied. The anodic peak currents of 3,4-dihydroxyphenylacetic acid obtained by differential pulse voltammetry are linear with the logarithm of melamine concentrations in the range from 1.0 × 10⁻⁸ to 5.0 × 10⁻⁶ M with a linear coefficiency of 0.997. The detection limit is 3.0 × 10⁻⁹ M. The proposed method displayed an excellent sensitivity and was successfully applied to the determination of melamine in milk products.     

抗坏血酸在聚对羟基苯甲酸(poly-PHB)修饰玻碳上的电催化

过循环伏安制备了聚对羟基苯甲酸修饰的玻碳电极。考察了该电极对抗坏血酸的电催化性能。结果显示,聚对羟基苯甲酸修饰玻碳电极对抗坏血酸有很好的电催化作用。在修饰后的电极上产生的峰电流比修饰前的电极产生的峰电流大4倍,氧化峰电位负移189 mV。其氧化峰电流与抗坏血酸浓度在2.6×10-5~3.68 ×10-4mol/L范围内呈线性关系,相关性系数为0.9984,检测限为5×10-6 mol/L(S /N = 3)。在AA与UA共存的体系中,能排除多巴胺对抗坏血酸测定的干扰。     

Exploiting micellar environment for simultaneous electrochemical determination of ascorbic acid and dopamine

A simple and reliable method for simultaneous electrochemical determination of ascorbic acid (AA) and dopamine (DA) is presented in this work. It was based on the use of the cationic surfactant cetylpyridinium chloride (CPC) that enables the separation of the oxidation peaks potential of AA and DA. Cyclic voltammetry (CV) as well as pulse differential voltammetry (PDV) were used in order to verify the voltammetric behaviour in micellar media. In the cationic surfactant CPC, a remarkable electrostatic interaction is established with negatively charged AA, as a consequence, the oxidation peak potential shifted toward less positive potential and the peak current increased. On the other hand, the positively charged DA is repelled from the electrode surface and the oxidation peak potential shifts toward more positive potential in comparison to the bare electrode. Therefore, the common overlapped oxidation peaks of AA and DA can be circumventing by using CPC. Parameter that affects the E_pa and I_pa such as CPC concentration and pH were studied. Under optimised conditions, the method presented a linear response to AA and DA in the concentration range from 5 to 75 μmol L⁻¹ and 10 to 100 μmol L⁻¹, respectively. The proposed method was successfully applied to the simultaneous determination of AA and DA in dopamine hydrochloride injection (DHI) samples spiked with AA.     

Electrochemical behaviour of a lead electrode in phosphoric acid

 A lead electrode was studied in 6 and 12 M H₃PO₄. Oxidation of a freshly polished electrode occurred in the −0.5 to −0.3 V vs. SCE range, and led to PbHPO₄ growth on the electrode surface. The dissolution of this layer by electrochemical reduction occurred between −0.5 and −0.7 V. The influence of temperature (20 °C and 65 °C) was investigated and showed that the anodic and the cathodic peaks were increasing, and more markedly for the 12 M H₃PO₄. The ratio Q _cathodic/Q _anodic (Q=electrical charge flowing through the electrode) was equal or close to the unity at 20 °C and decreased as the temperature was increased. The influence of Cl⁻, Br⁻ and I⁻ ions was also evaluated. The addition of Cl⁻ and Br⁻ predominantly led to Pb₅(PO₄)₃Cl and Pb₅(PO₄)₃Br, respectively, while I⁻ led to a mixture of PbI₂ and PbHPO₄. Received: 18 July 1999 / Accepted: 2 November 1999     

咖啡酸苯乙酯在玻碳电极上的电化学行为研究

采用循环伏安法和差分脉冲伏安法研究了咖啡酸苯乙酯(CAPE)在玻碳电极表面上的电化学行为。在0.05 mol.dm-3磷酸盐缓冲溶液(PBS,pH=7.6)中,CAPE在0.229 V和0.214 V处呈现一对明显的氧化还原峰。考察了溶液pH值和扫描速率等因素对CAPE电化学行为的影响,结果表明,电化学过程中CAPE的电子转移数为2,参与反应的质子数也为2,且为吸附控制过程。在0.05 mol.dm-3磷酸盐缓冲溶液(PBS,pH=7.6)中,CAPE的氧化峰电流与其浓度在0.34～3.40μmol.dm-3范围内成线性关系,其响应灵敏度为0.88μA/μmol.dm-3,检出限为60 nmol.dm-3(S/N=3)。本研究建立了一种简单、快速、可灵敏测定CAPE的方法。同时对CAPE在玻碳电极上的电化学行为进行了较为详细的研究。     

Fabrication and characterisation of high performance polypyrrole modified microarray sensor for ascorbic acid determination

In this study, gold microelectrode array (Au/MEA) with electrode of 12 μm diameter was fabricated by photolithography technique. Subsequently, polypyrrole (Ppy) modified gold microarrays sensor (Ppy/Au/MEA) was prepared by cyclic voltammetry technique. The deposition potential range and number of cycles were optimised in order to get optimum thickness of Ppy film. Scanning Electron Microscope and Atomic Force Microscope investigations reveal that Ppy coating formed at 3 cycles is porous with thickness of 1.5 μm which exhibiting high catalytic current for ascorbic acid (AA) in square wave technique (SWV). In contrast to earlier sensors designs, these Ppy/Au/MEA sensors exhibits lower detection limit (LOD) of 10 nm towards AA at physiological conditions. It also exhibits enhanced sensitivity (2.5 mA cm⁻² mM⁻¹) and long range of linear detection limit from 10 nm to 2.8 mM. In the same way, polypyrrole modified macro Au (Ppy/Au/MA) biosensor was also fabricated and its electro catalytic property towards AA was compared with that of Ppy/Au/MEA. The Ppy/Au/MA exhibits sensitivity of only 0.27 mA cm⁻² mM⁻¹, LOD of 5 μM and linear range of 10 μM to 2.2 mM. Hence, our investigations indicate that the Ppy/Au/MEA could serve as highly sensitive sensor for AA than any of the earlier designs. So, the Ppy/Au/MEA electrode was utilised for determination AA in a wide variety of real samples.