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.     

石墨烯修饰玻碳电极伏安法测定美洛昔康

通过在玻碳电极表面电化学还原氧化石墨烯的方法制备了石墨烯修饰电极,研究了美洛昔康在该修饰电极上的电化学行为。优化了包括支持电解质及pH、修饰剂用量、富集电位及时间等测定条件,据此建立了一种直接测定美洛昔康的电化学分析方法。在0.1 mol/L Britton-Robinson缓冲液(pH 3.0)中,氧化峰电流与美洛昔康浓度在1.0×10-6～8.0×10-5mol/L范围内呈现良好的线性关系,检出限为3.0×10-7mol/L(S/N=3)。方法可用于片剂和尿样中美洛昔康的测定。     

Voltammetric determination of levofloxacin using a glassy carbon electrode modified with poly(o-aminophenol) and graphene quantum dots

A strategy was developed for the voltammetric determination of the antibiotic drug levofloxacin (LV) based on a glassy carbon electrode modified with a composite consisting of poly(o-aminophenol) and graphene quantum dots (PoAP/GQD) that was fabricated by electropolymerization. The PoAP/GQD composite provides a large surface area and sensing interface and strongly promotes the oxidation current of LV. Under optimal conditions, the modified GCE displays an oxidation peak current (best measured at a working voltage of 1.05 V vs. SCE) that is linearly related to the levofloxacin concentration in the range from 0.05 to 100 μM, and the detection limit is 10 nM (at an S/N of 3). The method was applied to the determination of levofloxacin in spiked milk samples where is gave recoveries between 96.0 and 101.0 %.

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Graphical Abstract We describe a one-step electrochemical polymerization method to synthesize a layer of conductive film of poly(o-aminophenol) and graphene quantum dots (PoAP/GQD) onto a glassy carbon electrode (GCE) surface. The composite film exhibited high electro catalytic activity for the quantitative determination of levofloxacin by stripping voltammetry.

     

石墨烯修饰玻碳电极伏安法测定酪氨酸

制备了石墨烯修饰玻碳电极,研究了酪氨酸在修饰电极上的电化学行为.优化了包括支持电解质、溶液pH、修饰剂用量、富集电位及时间等测定条件.在0.1 mol·L-1pH 7.0的磷酸盐缓冲溶液中,峰电流与酪氨酸的浓度在3×10-6～1.2×10-4mol·L-1的范围内呈良好的线性关系,检出限为2 × 10-7 mol·L-...     

Voltammetric determination of 4-nitrophenol at a lithium tetracyanoethylenide (LiTCNE) modified glassy carbon electrode

The reduction of 4-nitrophenol (4-NP) has been carried out on a modified glassy carbon electrode using cyclic and differential pulse voltammetry (DPV). The sensor was prepared by modifying the electrode with lithium tetracyanoethylenide (LiTCNE) and poly-l-lysine (PLL) film. With this modified electrode 4-NP was reduced at −0.7 V versus SCE. The sensor presented better performance in 0.1 mol l⁻¹ acetate buffer at pH 4.0. The other experimental parameters, such as concentration of LiTCNE and PLL, pulse amplitude and scan rate were optimized. Under optimized operational conditions, a linear response range from 27 up to 23200 nmol l⁻¹ was obtained with a sensitivity of 3.057 nA l nmol⁻¹ cm⁻². The detection limit for 4-NP determination was 7.5 nmol l⁻¹. The proposed sensor presented good repeatability, evaluated in term of relative standard deviation (R.S.D.=4.4%) for n=10 and was applied for 4-NP determination in water samples. The average recovery for these samples was 103.0 (± 0.7)%.     

Voltammetric determination of disinfectants at multiwalled carbon nanotube modified glassy carbon electrode

The voltammetric method for simultaneous determination of some disinfectants at glassy carbon electrode modified with multiwalled carbon nanotubes is presented. The examined compounds are: 2-phenylphenol, 4-chloro-3-methylphenol, triclosan (5-chloro-2-(2,4-dichlorophenoxy)phenol and 2-mercaptobenzothiazole. The measurements has been performed using cyclic voltammetry and differential pulse voltammetry in Britton-Robinson buffers as supporting electrolytes. The modification of electrode surface with multiwalled carbon nanotubes enhances the peak current. It is possible to measure mixtures of two compounds (2-phenylphenol and 2-mercaptobenzothiazole, 4-chloro-3-methylphenol and 2-mercaptobenzothiazole, triclosan and 2-mercaptobenzothiazole) in the solution of pH 9.9, which provides the best separation of oxidation peaks.     

聚L-丝氨酸修饰电极伏安法测定对乙酰氨基酚

对乙酰氨基粉(扑热息痛)为芳环对位取代的酰氨类药物,有解热、镇痛作用。临床上广泛用于感冒发烧、关节痛、神经痛及偏头痛、癌性痛及手术后止痛[1]。但过多服用对乙酰氨基酚对人体会造成伤害,对消化系统的影响主要表现为恶心、呕吐、压食、出汗、腹痛等症状;对泌尿系统、血液系统、呼吸系统都有影响,还能使对阿司匹灵过敏患者的支气管痉挛加重,严重时会抑制呼吸中枢。因此建立对乙酰氨基酚的灵敏检测方法是非常必要的。当前用于检测对乙酰氨基酚的方法主要有滴定法[2]、分光光度法[3]、高效液相色谱法[4]、毛细管电泳[5]、荧光法[6]以及电…     

Voltammetric determination of niclosamide at a glassy carbon electrode

A very sensitive and selective procedure was developed for the determination of niclosamide based on square-wave voltammetry at a glassy carbon electrode. Cyclic voltammetry was used to investigate the electrochemical reduction of niclosamide at a glassy carbon electrode. Niclosamide was first irreversibly reduced from NO2 to NHOH at -0.659 V in aqueous buffer solution of pH 8.5. Reversible and well defined peaks at -0.164 V and -0.195 V (vs. Ag/AgCl) were obtained that are responsible for two electron peaks between NHOH and NO. Following optimisation of the voltammetric parameters, pH and reproducibility, a linear calibration curve over the range 5 x 10(-8)-1 x 10(-6) mol dm(-3) was achieved. The detection limit was found to be 2.05 x 10(-8) mol dm(-3) niclosamide. For eight successive determinations of 5 x 10(-7) mol dm(-3) niclosamide, a relative standard deviation of 2.4% was obtained. This voltammetric method was applied to the direct determination of niclosamide in tablets. The results of the analysis suggest that the proposed method has promise for the routine determination of niclosamide in the products examined.     

Voltammetric determination of tinidazole using a glassy carbon electrode modified with single-wall carbon nanotubes.

An electrochemical method based on a single-wall carbon nanotubes (SWNTs) film-coated glassy carbon electrode (GCE) was described for the determination of tinidazole. In a 0.1 M Britton-Robinson buffer with a pH of 10.0, tinidazole yields a very sensitive and well-defined reduction peak at -0.78 V (vs. SCE) on a SWNTs-modified GCE. Compared with that on a bare GCE, the reduction peak of tinidazole increases significantly on the modified GCE. Thus, all of the experimental parameters were optimized and a sensitive voltammetric method is proposed for tinidazole determination. It is found that the reduction peak current is proportional to the concentration of tinidazole over the range from 5 x 10(-8) to 4 x 10(-5) M, and that the detection limit is 1 x 10(-8) M at 3 min open-circuit accumulation. This new analysis method was demonstrated with tinidazole drugs.     

Voltammetric determination of 4-nitrophenol at a sodium montmorillonite-anthraquinone chemically modified glassy carbon electrode

A new method for the determination of 4-nitrophenol(4-NP) by differential pulse voltammetry (DPV) based on adsorptive stripping technique was described. Cyclic voltammetry (CV) and linear scan voltammetry (LSV) were used in a comparative investigation into the electrochemical reduction of 4-NP at a Na-montmorillonite(SWy-2) and anthraquione (AQ) modified glassy carbon electrode. With this chemically modified electrode, 4-NP was first irreversibly reduced from phiNO(2) to phiNHOH at -0.78 V. A couple of well-defined redox peaks at +0.22 V (vs. SCE) were responsible for a two-electron redox peak between phiNHOH and phiNO. Studies on the effect of pH on the peak height and peak potential were carried out over the pH range 2.0-9.0 with the phosphate buffer solution. A pH of 3.4 was chosen as the optimum pH. The other experimental parameters, such as film thickness, accumulation time and potential etc. were optimized. Anodic peak currents were found to be linearly related to concentration of 4-NP over the range 0.3-45 mg l(-1), with a detection limit of 0.02 mg l(-1). The interference of organic and inorganic species on the voltammetric response have been studied. This modified electrode can be used to the determination of 4-NP in water samples.     

活化玻碳电极伏安法测定锰的研究

采用活化玻碳电极(GC)以伏安法对测定锰进行了研究。结果表明:沉积于电极表面的二氧化锰对锰(Ⅱ)的电化学氧化具有自催化作用,活化GC电极可极大地提高测定锰的灵敏度。在0.04mol LNH3 NH4Cl(pH9.0)底液中,锰浓度在6.0×10-8～1.0×10-5mol L范围内成线性关系,检出限为4.0×10-8mol L。用3×10-7mol L锰溶液重复测定9次,RSD为1.6%。     

Electrochemical determination of dopamine using a poly(2-picolinic acid) modified glassy carbon electrode

A poly(2-picolinic acid) chemically modified electrode (CME) for the determination of dopamine (DA) by cyclic voltammetry is described. Compared with a bare glassy carbon electrode, the CME exhibits a 200 mV shift of the oxidation potential of DA in the cathodic direction and a marked enhancement of the current response. In pH 7.0 buffer solution, a linear calibration graph is obtained over the range from 2.5 x 10(-7) to 1.0 x 10(-5) mol dm-3 with a correlation coefficient of 0.998. The detection limit is 3.0 x 10(-8) mol dm-3. The modified electrode eliminated efficiently the interference from ascorbic acid (AA) when present in a 150-fold concentration ratio. It also showed excellent stability and reproducibility.     

Voltammetric oxidation and determination of cinnarizine at glassy carbon electrode modified with multi-walled carbon nanotubes

We discovered a novel method to prepare a protein-based hydrogel, that is, a “Three-Dimensional Nanostructured Protein Hydrogel (3D NPH)”, which is composed of protein–polymer hybrid nanoparticles. In this study, we propose a novel protein microarray whose 3D NPH spots were prepared by dispensing a small volume of the solution of protein–polymer mixture on a substrate. The dispensed solution had a short time for cross-linking before its drying-up and the resulting 3D NPH had loosely cross-linked, thin spongy structure. Therefore, the reaction ratio between ligands and analytes was drastically improved in this system compared with the large volume system for Surface Plasmon Resonance (SPR) protein microarray.     

Highly sensitive electrocatalytic determination of pyrazinamide using a modified poly(glycine) glassy carbon electrode by square-wave voltammetry

A new voltammetric sensor based on electropolymerization of glycine at glassy carbon electrode (GCE) was developed and applied to determine of pyrazinamide (PZA) by square-wave voltammetry (SWV). The initial cyclic voltammetric studies showed an electrocatalytic activity of poly(Gly)/GCE on redox system of pyrazinamide in 0.1 mol L^?1 phosphate buffer solution pH 7.5, with E _Pc and E _Pa in ?0.85 and ?0.8 V (versus E _Ag/AgCl), respectively. Studies at different scan rates suggest that the redox system of pyrazinamide at poly(Gly)/GCE is a process controlled by diffusion in the interval from 10 to 100 mV s^?1. Square-wave voltammetry-optimized conditions showed a linear response of PZA concentrations in the range from 0.47 to 6.15 μmol L^?1 (R?=?0.998) with a limit of detection (LOD) of 0.035 μmol L^?1 and a limit of quantification (LOQ) of 0.12 μmol L^?1. The developed SWV-poly(Gly)/GCE method provided a good intra-day (RSD?=?3.75 %) and inter-day repeatability (RSD?=?4.96 %) at 4.06 μmol L^?1 PZA (n?=?10). No interference of matrix of real samples was observed in the voltammetric response of PZA, and the method was considered to be highly selective for the compound. In the accuracy test, the recovery was found in the range of 98.2 and 104.0 % for human urine samples and pharmaceutical formulation (tablets). The PZA quantification results in pharmaceutical tablets obtained by the proposed SWV-poly(Gly)/GCE method were comparable to those found by official analytical protocols.     

Electrochemical determination of maltol in food products using a poly(L-tryptophan) modified glassy carbon electrode

Herein, a poly(L-tryptophan) modified glassy carbon electrode (Ptry/GCE) for the determination of maltol is fabricated by electrochemical polymerisation. The electrochemical behaviour of maltol at the Ptry/GCE is studied by cyclic voltammetry (CV). The modified electrode shows excellent electrocatalytic activity towards the oxidation of maltol and the oxidation is a one-proton-one-electron process. In pH 8.0 phosphate buffer solution (PBS), the oxidation peak current of maltol shows a linear relationship with its concentration in the range from 9.00 × 10^?5 to 3.75 × 10^?3 mol L^?1 with a correlation coefficient of 0.9972. The limit of detection is estimated to be 8.00 × 10^?6 mol L^?1. The novel method shows good selectivity, recovery, reproducibility and great convenience and has been satisfactorily demonstrated in real food sample analysis.     

Voltammetric determination of bisphenol A in food package by a glassy carbon electrode modified with carboxylated multi-walled carbon nanotubes

A highly sensitive and mercury-free method for determination of bisphenol A (BPA) was established using a glassy carbon electrode that was modified with carboxylated multi-walled carbon nanotubes. A sensitive oxidation peak is found at 550?mV in linear sweep voltammograms at pH?7. Based on this finding, trace levels of bisphenol A can be determined over a concentration range that is linear from 10?nM to 10⁴?nM, the correlation coefficient being 0.9983, and the detection limit (S/N?=?3) being 5.0?nM. The method was successfully applied to the determination of BPA in food package.

Simultaneous determination of dopamine and ascorbic acid on poly (3,4-ethylenedioxythiophene) modified glassy carbon electrode

Detection of dopamine (DA) in the presence of excess of ascorbic acid (AA) has been demonstrated using a conducting polymer matrix, poly (3,4-ethylenedioxythiophene) (PEDOT) film in neutral buffer (PBS 7.4) solution. The PEDOT film was deposited on a glassy carbon electrode by electropolymerization of EDOT from acetonitrile solution. Atomic force microscopy studies revealed that the electrodeposited film was found to be approximately 100 nm thick with a roughness factor of 2.6 nm. Voltammetric studies have shown catalytic oxidation of DA and AA on PEDOT modified electrode and can afford a peak potential separation of ∼0.2 V. It is speculated that the cationic PEDOT film interacts with the negatively charged ascorbate anion through favorable electrostatic interaction, which results in pre-concentration at a less anodic value. The positively charged DA tends to interact with the hydrophobic regions of PEDOT film through hydrophobic–hydrophobic interaction thus resulting in favorable adsorption on the polymer matrix. Further enhancement in sensitivity to micro molar level oxidation current for DA/AA oxidation was achieved by square wave voltammetry (SWV) which can detect DA at its low concentration of 1 μM in the presence of 1000 times higher concentration of AA (1 mM). Thus the PEDOT modified electrode exhibited a stable and sensitive response to DA in the presence of AA interference.