Indirect Electrochemical Determination of Ribavirin Using Boronic Acid-Diol Recognition on a 3-Aminophenylboronic Acid-Electrochemically Reduced Graphene Oxide Modified Glassy Carbon Electrode (APBA/ERGO/GCE)

A novel method for the indirect electrochemical determination of ribavirin based on boronic acid-diol recognition was developed using the platform as the sensing element. The device was constructed using a 3-aminophenylboronic acid (APBA)-electrochemically reduced graphene oxide (ERGO) modified electrode. When the electrode was immersed in a solution of ribavirin, complexation of boronic acid groups of APBA with ribavirin occurred at the surface of the electrode and simultaneously caused steric hindrance, resulting in a current decrease because the ferricyanide redox probe was unable access the surface. Under the optimized conditions, a linear relationship was obtained between the relative change in current (%Δi) of [Fe(CN)₆]^3?/4?and the concentration of ribavirin at levels from 10.0 to 7.50?×?10²?ng mL^?1. The proposed electrochemical sensor performed with acceptable sensitivity and reproducibility and was successfully used to determine the content of ribavirin in an injection with satisfactory results.     

基于羧基化多壁碳纳米管修饰玻碳电极快速检测氨基脲的研究

基于羧基化多壁碳纳米管修饰的玻碳电极(CMWCNTs/GCE),构建了一种灵敏检测氨基脲(SEM)的电化学传感器.采用傅里叶变换红外光谱、透射电子显微镜、电化学阻抗谱对修饰材料进行表征.结果表明,羧基化的多壁碳纳米管出现羧基碳氧双键的红外特征峰,管径明显减小,长度变短,电化学阻抗值显著减小.在1 mol/L HAc-NaAc缓冲液中,利用循环伏安法和时间-电流曲线研究了SEM在CMWCNTs修饰电极上的电化学行为.SEM在修饰电极上呈现不可逆的氧化峰.与裸电极相比,氧化峰电流明显增大.在最佳实验条件(pH 7.0,扫描速度为0.1 V/s)下,测得SEM在5.00×10-6~1.09×10-3mol/L浓度范围内与氧化峰电流呈线性关系,线性方程为IP(μA)=-0.472+0.0599C(μmol/L),相关系数r=0.997,检出限为1.88×10-7 mol/L(S/N=3).在实际猪肝样品检测中加标回收率为92.8%~98.0%.     

聚苯基荧光酮修饰玻碳电极吸附溶出伏安法测定痕量汞

研究利用聚苯基荧光酮修饰玻碳电极测定痕量汞的溶出伏安法,在0.1 mol.L-1氨水-NH4Cl缓冲溶液中(pH 9.5),开路搅拌,Hg(Ⅱ)富集于修饰电极表面,通过介质交换至0.1mol.L-1盐酸溶液中,于-0.40 V还原后阳极化线性扫描,在0 V左右处获得一灵敏汞的溶出峰。其氧化峰电流与Hg(Ⅱ)浓度在9.0×10-8~8.0×10-7mol.L-1范围内呈线性关系,开路富集5 min,检出限达2.0×10-8mol.L-1。应用此方法于尿液中汞的测定,所得平均RSD值小于4.02%,回收率试验结果在98.4%~103.2%间。     

Determination of Chlorpromazine Hydrochloride with a Layered Double Hydroxide Modified Glassy Carbon Electrode as a Nanocatalyst

We report a simple and sensitive voltammetric sensor for the determination of chlorpromazine (CPZ) based on Ni?Al layered double hydroxide (NiAlLDH) modified glassy carbon electrode (GCE). NiAlLDH was simply electrodeposited on GCE surface in a very short time. The response linear range was 1×10^?3–1×10^?9 mol L^?1, with a detection limit of 1×10^?9 mol L^?1. The NiAlLDH film showed well defined and well separate peaks for dopamine, ascorbic acid, uric acid and CPZ in the same solution. The proposed electrode was used to measure the active pharmaceutical ingredient of CPZ tablet as a real sample.     

吡哌酸在玻碳电极上的伏安测定

本文应用线性扫描伏安法，微分脉冲伏安法，循环伏安法对吡哌酸在ＧＣＥ上的伏安行为进行了研究，发现在磷酸盐缓冲溶液中＋１．２Ｖ左右有一氧化峰，ＰＰＡ的浓度２－１００μｇ／ｍｌ与峰电流呈良好的线性关系。测定了胶囊和片剂中ＰＰＡ的含量，ＲＳＤ２．１％，回收率在９７％－１０４％之间，方法操作简单快速。ＰＰＡ在ＧＣＥ上的电极反应属于不可逆过程。     

壳聚糖碳纳米管修饰电极测定痕量铜

建立了用自制的碳纳米管壳聚糖修饰电极测定Cu^2＋离子的电分析方法,在0．10mol／L的CH,COOH—CH3 COONa（pH4．2）缓冲溶液中,以此修饰电极作为工作电极,以-0．60V为富集电位,搅拌富集6min后,用差分脉冲伏安法测定-0．10V处的峰电流。结果发明,该电极对铜离子吸附的灵敏度较高,当铜离子浓度为1．0×10^-6～4．6×10^-5mol／L时,线性关系良好,相关系数为0．9997,对含铜血清样本进行测定,取得了满意的结果,加标回收率在98％～102％之间。     

Electrochemical Behavior of Caffeic Acid Assayed with Gold Nanoparticles/Graphene Nanosheets Modified Glassy Carbon Electrode

A gold nanoparticle (AuNP) and graphene nanosheet (GN) modified glassy carbon electrode (GCE) is proposed as voltammetric sensor for caffeic acid assay. The sensor exhibits a surface‐confined and reversible process for oxidation of caffeic acid revealed by cyclic voltammetry. The results show more favorable electron transfer kinetics than the bare GCE. The linear response of the sensor is from 5×10^?7 to 5×10^?5 M with a detection limit of 5×10^?8 M (S/N=3). The AuNP/GN nanocomposite shows more favorable electrochemical activity and should be a kind of more robust and advanced functional material, which provides a promising platform for electrochemical sensors and biosensors. The method was successfully applied to detect caffeic acid in pharmaceutical tablets with satisfactory results.     

Electrochemical Behavior and Determination of L‐Tyrosine at Single‐walled Carbon Nanotubes Modified Glassy Carbon Electrode

Based on single‐walled carbon nanotubes (SWCNTs) modified glassy carbon electrode (GCE/SWCNTs), a novel method was presented for the determination of L ‐tyrosine. The GCE/SWCNTs exhibited remarkable catalytic and enhanced effects on the oxidation of L ‐tyrosine. In 0.10 mol/L citric acid‐sodium citrate buffer solution, the oxidation potential of L ‐tyrosine shifted negatively from +1.23 V at bare GCE to +0.76 V at GCE/SWCNTs. Under the optimized experimental conditions, the linear range of the modified electrode to the concentration of L ‐tyrosine was 5.0×10^?6–2.0×10^?5 mol/L (R₁=0.9952) and 2.7×10^?5–2.6×10^?4 mol/L (R₂=0.9998) with a detection limit of 9.3×10^?8 mol/L. The kinetic parameters such as α (charge transfer coefficient) and D (diffusion coefficient) were evaluated to be 0.66, 9.82×10^?5 cm² s^?1, respectively. And the electrochemical mechanism of L ‐tyrosine was also discussed.     

多壁碳纳米管修饰玻碳电极伏安法测定氯霉素

研究了氯霉素(CAP)在多壁碳纳米管修饰玻碳电极上的电化学行为.发现在pH=2.0的0.1 mol/LKCl-HCl底液中,CAP在该修饰电极上有一灵敏的还原峰(Ep=-0.36 V vs.Ag/AgCl),峰电流与CAP浓度成正比,线性范围为6.0×10-6~2.7×10-4mol/L,检测限达3.0×10-6mol/L.该方法灵敏、准确,用于模拟样品和实际样品的测定,结果满意.     

Use of Mercury Film Glassy Carbon Electrode Modified with Multiwalled Carbon Nanotubes in Electrochemical Analysis of DNA

Mercury film plated on a glassy carbon electrode modified with multiwalled carbon nanotubes (MF/MWNTs/GCE) was used for the analysis of single (ss) and double stranded (ds) DNA, as well as for Jurkat genomic DNAs methylated to different degrees. The results indicated that the DNA molecules adsorbed quite strongly on the MF/MWNTs/GCE surface allowing ex situ adsorption and produce well developed peaks (due to cytosine and adenine) by using adsorptive stripping (Ads, ex situ) square wave voltammetry (SWV). Also, SWV of Jurkat DNA mixtures methylated to different degrees revealed a linear decrease of the peak height with increasing methylation indicating an increase of structural rigidity.     

Optimization of Square Wave Voltammetry (SWV) Parameters by Design of Experiment (DoE) Methodologies for the Determination of Mifepristone at Glassy Carbon Electrode (GCE)

In the present study, an electroanalytical method that permits the optimization of factors affecting SWV for sensitive detection of mifepristone at glassy carbon electrode (GCE) using response surface methodology (RSM) with desirability function (DF) is presented. Factors selected for optimization after screening using full factorial design were frequency (X₁), amplitude (X₂), and pH (X₃). The central composite design as a response surface methodology with desirability function (DF) was applied for obtaining the optimum level. The optimum conditions were obtained as follows: Frequency (X₁=50 Hz), amplitude (X₂=33.4 mV), and pH (X₃=9.4), with an overall desirability function of 0.97. Subsequently, confirmatory experiments were performed in triplicates to validate the optimum conditions. The results obtained were satisfactory and agreed well with less only 11.9 % deviation from the values predicted by the model. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.54 and 1.80 ppm, respectively. The proposed method was applied for a quantitative determination of mifepristone in spiked tap water samples. The recovery tests showed that the detection of mifepristone at GC could be evaluated on environmental samples.     

聚溴酚蓝修饰玻碳电极的制备及电化学性质

在含溴酚蓝的磷酸缓冲溶液中,应用循环伏安法于经预处理的玻碳电极上形成聚合物薄膜.结果表明,在-1. 0V~+1. 8V(vs.Ag/AgCl)扫描电位之间形成的薄膜具有较高的电活性和稳定性.该电极对抗坏血酸电化学氧化有催化作用,既使抗坏血酸的氧化电位负移了 270mV,又增大了其氧化峰电流.催化峰电流与抗坏血酸浓度在 2. 5~250μg/mL范围内呈良好的线性关系.     

阿魏酸聚合修饰玻碳电极的制备及其对NADH的催化氧化

研究了阿魏酸修饰电极的制备、性质及对NADH的电催化作用.该电极在0.1mol/L磷酸缓冲溶液(pH=6.60)中,于-0.1～+0.50V(vs.Ag/AgCl)电位范围内呈现一对氧化还原峰,其式量电位E₀为+0.188V(vs.Ag/AgCl),且E₀随pH增加而负向移动.电子转移系数为0.496,表观电极反应速率常数(ks)为6.6s^-1.电极反应的电子数为1且有1个质子参与.该修饰电极对NADH氧化具有很好的催化作用.在NADH存在下,电极过程由扩散控制,扩散系数为1.76×10^-6cm²/s.NADH浓度在0.01～5.0mmol/L范围内与峰电流呈现良好的线性关系.通过计时安培法测得催化速率常数为6.82×10³mol^-1·L·s^-1.     

聚阿魏酸修饰电极的电化学特性及电催化性能

研究了阿魏酸在玻碳电极表面电聚合成膜的方法和条件,测量了应用电化学方法制备不同厚度的阿魏酸修饰电极的循环伏安行为及其它电化学性质.对厚度为0.5 μm的阿魏酸膜,测得的电子转移系数为0.49,表观电极反应速率常数(ks)为6.56 s－1.扩散系数DR为7.9×108 cm2•s－1,Do为4.48×108 cm2•s－1.该修饰电极对烟酰胺腺嘌呤二核苷酸（NADH）氧化具有很好的催化作用.NADH浓度在0.01～5.0 mmol•dm－3范围内与峰电流呈现良好的线性关系.     

肌红蛋白在磷脂-月桂酸修饰的玻碳电极上的电化学行为及其分析应用

报道了肌红蛋白(Mb)在磷脂、月桂酸修饰的玻碳电极上的电化学行为 ,在 +0.2～ -0.7V(vs.Ag/AgCl)电位范围内 ,于pH6.0的0.01mol·L-1的KH2PO4、Na2HPO4底液中 ,肌红蛋白产生不可逆的还原电流峰 ;还原峰电流与肌红蛋白浓度在2.25×10-8 ～1.40×10-6 mol·L-1 范围内呈良好线性关系 ;线性回归方程为Ip(μA)=-0.01419 +0.2382cMb(10 -7mol·L -1) ,线性回归系数r(10)为0.998 ,检出限为1.20×10 -8mol·L -1,该电极可作为检测肌红蛋白的新型的高灵敏度电化学生物传感器。     

Study on Cd2+ Determination Using Bud-like Poly-L-Tyrosine/Bi Composite Film Modified Glassy Carbon Electrode Combined with Eliminating of Cu2+ Interference by Electrodeposition

A bud-like poly-L-tyrosine/Bi modified glassy carbon electrode (p-Tyr/Bi/GC) was prepared by CV and in situ Bi plating, whose conductivity and membrane morphology were characterized by CV, EIS and SEM, respectively. The p-Tyr membrane can effectively promote the enrichment of Cd²⁺. The optimal Tyr concentration and scanning number for p-Tyr/GC preparation were 2.0 mmol ⋅ L⁻¹ and 35, while the optimal Bi³⁺ concentration, pH and Cd²⁺ accumulation potential in test medium were 3.0 μmol ⋅ L⁻¹, 6.5 and −1.3 V, respectively. The linear equation of p-Tyr/Bi/GC's response to Cd²⁺ (1.0 nmol ⋅ L⁻¹ to 2.0 μmol ⋅ L⁻¹) was i_p (μA) = −0.6809 + 100.2c (μmol ⋅ L⁻¹) (R² = 0.9985) with a detection limit of 0.11 nmol ⋅ L⁻¹ (3S/N). The elimination of interference caused by Cu²⁺ in sample was studied by electrodeposition. The p-Tyr/Bi/GC electrode was successfully used for detecting Cd in rice samples with good reliability and accuracy. The developed Cd²⁺ sensor exhibits high sensitivity, wide linear range and low detection limit, especially the designed method of eliminating Cu²⁺ interference has the characteristics of high selectivity, simple operation and wide application range.     

纳米氧化铜修饰的苯巴比妥分子印迹传感器的制备及其电化学性能

为了改善分子印迹传感器的灵敏度, 在四丁基高氯酸铵的支持电解质溶液中, 以甲基丙烯酸为功能单体, 马来松香丙烯酸乙二醇酯为交联剂在纳米氧化铜修饰过的玻碳电极上电聚合了一种苯巴比妥(PB)识别性能的分子印迹传感膜. 采用循环伏安(CV)法、差分脉冲伏安(DPV)法及交流阻抗(EIS)法对这种纳米氧化铜修饰过的印迹及非印迹电极的电化学性能进行了研究, 结果显示纳米氧化铜修饰过的印迹及非印迹电极的电化学性能完全不同. X射线衍射(XRD)证实纳米粒子为氧化铜. 采用扫描电镜(SEM)对纳米氧化铜修饰过的印迹传感器的形貌进行分析, 发现纳米氧化铜分散在电极表面, 改善了修饰印迹传感器的识别点. 差分脉冲伏安法(DPV)表明苯巴比妥的浓度在1.0×10^-8-1.8×10^-4 mol·L^-1 范围内呈现良好的线性关系(线性相关系数R=0.9994); 检出限2.3×10^-9 mol·L^-1 (信噪比(S/N)=3). 研究结果表明纳米氧化铜修饰过的印迹传感器具有较高灵敏度及选择性. 此印迹传感器能用于实际样品中苯巴比妥的检测, 加标回收率在95.0%-102.5%.     

纳米氧化铜修饰的苯巴比妥分子印迹传感器的制备及其电化学性能

为了改善分子印迹传感器的灵敏度,在四丁基高氯酸铵的支持电解质溶液中,以甲基丙烯酸为功能单体,马来松香丙烯酸乙二醇酯为交联剂在纳米氧化铜修饰过的玻碳电极上电聚合了一种苯巴比妥(PB)识别性能的分子印迹传感膜.采用循环伏安(CV)法、差分脉冲伏安(DPV)法及交流阻抗(EIS)法对这种纳米氧化铜修饰过的印迹及非印迹电极的电化学性能进行了研究,结果显示纳米氧化铜修饰过的印迹及非印迹电极的电化学性能完全不同.X射线衍射(XRD)证实纳米粒子为氧化铜.采用扫描电镜(SEM)对纳米氧化铜修饰过的印迹传感器的形貌进行分析,发现纳米氧化铜分散在电极表面,改善了修饰印迹传感器的识别点.差分脉冲伏安法(DPV)表明苯巴比妥的浓度在1.0×10-8-1.8×10-4mol·L-1范围内呈现良好的线性关系(线性相关系数R=0.9994);检出限2.3×10-9mol·L-1(信噪比(S/N)=3).研究结果表明纳米氧化铜修饰过的印迹传感器具有较高灵敏度及选择性.此印迹传感器能用于实际样品中苯巴比妥的检测,加标回收率在95.0%-102.5%.     

基于多孔碳固载离子液体修饰电极的叔丁基对苯二酚的检测研究

制备了多孔碳固载离子液体纳米材料修饰玻碳电极(GCE),用于抗氧化剂叔丁基对苯二酚(TBHQ)的检测研究。不同电极上的交流阻抗结果表明,经过多孔碳固载离子液体修饰后的玻碳电极阻抗显著减小。多孔碳固载离子液体修饰后电极的氧化峰电流为41.93μA,比修饰前增大约5.5倍,说明多孔碳固载离子液体可显著提高电极的导电性,促进电极表面的电子转移,提高检测灵敏度。用时间~电流曲线测得TBHQ的线性范围为1.00~120.00μg/mL,检出限为0.16μg/mL。     

Effect of Zn2+ Ions on Upconversion Emission of Er3+ in Zn/Er:LiNbO3 Crystal

The effect of Zn2+ ions codoped on the upconversion emission of Er3+ ions in Er:LiNbO3 crystal under different excitation wavelength was reported.The upconversion emission spectra of Zn/Er:LiNbO3 follo...