流动注射双安培法测定多巴胺

通过偶合多巴胺在铂电极上的氧化和高锰酸钾在铂电极上的还原,建立了一个不施加电压的条件下的流动注射双安培法直接测定多巴胺的新方法。以0.05 mol/L硫酸为载液,多巴胺的氧化峰电流与其浓度在0.8~160 mg/L范围内呈线性关系,线性回归方程为i(nA)=652.9C-239.2(r=0.9998,n=10),检出限为0.2 mg/L;RSD为2.86%(N=80 mg/L,n=14);进样频率为80次/h。本方法具有很高的选择性和灵敏度,样品处理方法简单快速,适于连续自动测定。用于实际样品的测定,结果满意。     

Determination of Levodopa in Pharmaceuticals Using a Disposable Electrochemically Activated Carbon-Paste Electrode by Linear Sweep Voltammetry

A simple disposable electrochemically activated carbon-paste electrode was developed for the determination of levodopa in pharmaceuticals and the optimal conditions for carbon-paste electrode electrochemical activation were studied. The study of the oxidation process of levodopa on the proposed electrode was performed using cyclic voltammetry and the irreversibility of levodopa with a kinetic-controlled current was established. The determination of levodopa is possible in the concentration range of 5–100?µM. The detection and quantification limits were 0.65 and 0.79?µM, respectively. The proposed procedure was satisfactorily applied in the levodopa determination in pharmaceuticals with relative standard deviation 3.4%.     

Nanostructured Conducting Polymer/Copper Oxide as a Modifier for Fabrication of L‐DOPA and Uric Acid Electrochemical Sensor

A modified electrode was prepared by modification of the carbon paste electrode (CPE) with a nanostructured material. This nanostructure with electrocatalytic activity was synthesized by combination of poly pyrrole and copper oxide nanoparticles (PPy/CuO). The structure and morphology of PPy/CuO was studied. The fabricated modified electrode (CPE‐PPy/CuO) exhibited an excellent electrocatalytic activity toward levodopa (L‐DOPA) and uric acid (UA) oxidation because of high conductivity, low electron transfer resistance and catalytic effect. The CPE‐PPy/CuO had a lower overvoltage and enhanced electrical current with respect to the bare CPE for both L‐DOPA and UA. Also, the modified electrode showed a good resolution for the overlapped anodic peaks of L‐DOPA and UA. This electrode was used for the successful simultaneous determination of L‐DOPA and UA. The electrochemical sensor responded to L‐DOPA and UA in the concentration range of 0.050–1200 μM and 0.040–2000 μM, respectively. The detection limits were obtained by differential pulse voltammetry as 15 nM for L‐DOPA and 20 nM for UA. Finally, the proposed electrode was used for determination of L‐DOPA and UA in real samples using standard addition method.     

羟乙芦丁在玻碳电极上的阳极微分脉冲伏安法测定

本文对羟乙芦丁在玻碳电极上的阳极微分脉冲安行为进行了研究，发现在Ｎａ２ＨＰＯ４溶液中（ｐＨ＝８．９５）于＋０．６４Ｖ（ｖｓ．Ａｇ／ＡｇＣｌ）左右产生一个良好的阳极氧化伏安峰，浓度在５～６０ｍｇ／Ｌ之间与峰电流呈线性关系，不需分离直接测定了片剂中的羟乙芦丁含量。电极反应为扩散速率控制的不可逆可程。     

毛细管电泳法同时测定血清中的左旋多巴和甲基多巴

建立了毛细管电泳-紫外检测同时测定血清中左旋多巴和甲基多巴的方法。以40 mmol/L硼砂（pH 9.5）为分离缓 冲溶液,在3.45 kPa（0.5 psi）压力下进样7 s、分离电压22 kV、检测波长200 nm、温度25 ℃的条件下进行测定,两 种物质获得了较好的分离。甲基多巴和左旋多巴分别为1.0~64.0 mg/L和1.0~71.0 mg/L时与峰面积呈良好的线性关系, 线性相关系数分别为0.9998和0.9994,检出限分别为0.6和0.8 mg/L(以信噪比为3计)。将该法用于血清中甲基多巴和左 旋多巴的测定,回收率为82.8%~88.8%,相对标准偏差为2.10%~2.63%。     

First Report for Electrochemical Determination of Levodopa and Cabergoline: Application for Determination of Levodopa and Cabergoline in Human Serum,Urine and Pharmaceutical Formulations

The electrochemical oxidation of levodopa on the surface of a carbon paste electrode modified with graphene nanosheets, 1‐(4‐bromobenzyl)‐4‐ferrocenyl‐1H‐[1,2,3]‐triazole (1,4‐BBFT) and hydrophilic ionic liquid (n‐hexyl‐3‐methylimidazolium hexafluoro phosphate) as a binder is studied. It has been found that the oxidation of levodopa at the surface of a modified electrode occurs at a potential of about 210 mV less positive than that of an unmodified carbon paste electrode (CPE). The prepared modified electrode exhibits a very good resolution of the voltammetric peaks of levodopa and cabergoline. The electrode has been applied successfully for the determination of levodopa and cabergoline in some real samples.     

差分脉冲伏安法测定卡托普利

本文基于金电极表面对巯基化合物的吸附作用,提出了一种简便灵敏的测定抗高血压药物卡托普利的新方法.研究了卡托普利在金电极上的伏安响应,优化了差分脉冲伏安法测定卡托普利的实验条件.研究结果表明:在0.217～3.04 mg/L的范围内,卡托普利的氧化峰电流与其浓度呈良好的线性关系,检出限为0.152 mg/L.测定药物中卡...     

碳糊电极阳极吸附伏安法测定卡托普利

在0.40 mol/L的HAc-NaAc(pH=4.8)缓冲溶液中,卡托普利(Captopril,CPT)在碳糊电极(CPE)上有一灵敏的吸附氧化峰,峰电位为0.23 V(vs.SCE)。该氧化峰的二阶导数峰电流与卡托普利的浓度在2.0×10-8～1.0×10-6mol/L(富集90 s)范围内呈良好的线性关系,相关系数为0.9966,检出限为8.0×10-9mol/L,并成功应用于卡托普利片含量的测定。探讨了卡托普利在碳糊电极上的伏安性质和电极反应机理。     

纳米二氧化钛膜光催化分解-电化学法联用测定水体中的总磷

利用电化学方法制备了磷钼酸修饰电极,该修饰电极对溶液中的PO43-有很好的电流响应,继而提出了一种用纳米TiO2-K2S2O7共存体系光催化氧化有机磷生成正磷,然后以磷钼酸修饰电极进行测定的新方法。实验中以有机膦酸为标准物质,研究了测定机理,优化了测定条件。实验表明,本方法操作简单、快速、准确。PO43-在0.04~16 mg/L浓度范围内,与修饰电极上的电流响应呈线性关系,检出限为0.02 mg/L。用本方法测定实际水样与标准分析方法所得结果相近。     

β-环糊精修饰碳糊电极测定盐酸青藤碱

研究盐酸青藤碱在β-环糊精(β-CD)修饰碳糊电极上的电化学行为,在此基础上建立了测定盐酸青藤碱的电化学新方法。盐酸青藤碱在β-CD修饰碳糊电极上是受吸附控制的电化学反应过程,在p H 6.6的柠檬酸–柠檬酸钠底液中,盐酸青藤碱在β-CD修饰碳糊电极上产生一对良好的氧化还原峰,峰电位分别为0.458 V和0.086 V。氧化峰电流与盐酸青藤碱的质量浓度在3.658 5~91.462 5 mg/L范围内呈良好线性关系,线性相关系数为0.995 4,检出限为1.229 3 mg/L。该方法应用于正清风痛宁片中盐酸青藤碱含量的测定,测定结果的相对标准偏差为5.82%(n=7),回收率在95.7%~107.4%之间。该方法简便、快速,结果准确,可用于盐酸青藤碱的测定。     

纳米PbO2修饰电极安培检测器流动注射法快速测定化学需氧量

采用以纳米PbO₂修饰电极为工作电极的安培检测器,用流动注射法快速检测水体中的化学需氧量(COD).根据纳米PbO₂修饰电极催化氧化电流的大小测定样品的COD值,在50-1 200 mg/L COD的范围内,电流响应与标准水样中的COD_Cr值呈线性关系,检出限为20 mg/L.该法不需对水样进行预处理,不使用有毒试剂,无二次污染,具有快速、简便、进样量少及工作电极使用寿命长等优点,与COD_Cr国家标准分析法对比具有较好的相关性.     

聚伊文思蓝修饰电极对多巴胺和抗坏血酸的电分离及同时测定

研究多巴胺(DA)和抗坏血酸(AA)在聚伊文思蓝(Evans Blue)修饰电极上的伏安行为,建立差示脉冲伏安测定法.在pH4.5磷酸盐缓冲液中,聚伊文思蓝修饰电极对DA和AA有显著的增敏和电分离作用.DA和AA氧化峰电流与浓度分别在1.0×10-6~3.0×10-5mol/L和5.0×10-6~1.05×10-4mol/L范围内呈良好的线性关系,检测限分别为2.5×10-7mol/L和3.0×10-7mol/L.当DA与AA共存时,由该修饰电极检测的二者氧化峰电位差达184 mV,故可同时测定DA和AA,并有效消除其它组分对DA测定的干扰,已用于实际样品中DA和AA含量的测定,结果令人满意.     

聚1,8-萘二胺修饰玻碳电极溶出伏安法测定银的研究

采用电化学聚合的方法制备了聚1,8-萘二胺修饰玻碳电极,建立了开路富集-阳极溶出测定痕量Ag~+的方法.优化了各种实验参数(如富集底液的pH,富集时间等),并考察了其它离子的干扰影响.在最佳实验条件下,银在0.0008～0.1 mg·L~(-1)浓度范围内与溶出峰电流成良好的线性关系,检出限为0.0005 mg·L~(-1).该法用于实际水样中痕量银的测定,效果良好.     

Determination of Iodide and Idoxuridine at a Glutaraldehyde‐Cross‐Linked Poly‐L‐Lysine Modified Glassy Carbon Electrode

The detection limit (about 0.017 μg mL^?1) for voltammetric determination of iodide (peak at +0.87 V vs. Ag/AgCl at pH 2) at a glutaraldehyde‐cross‐linked poly‐L ‐lysine modified glassy carbon electrode involving oxidation to iodine was found to be several orders of magnitude lower than that for the voltammetric determination on a bare glassy carbon electrode. This method was applied successfully to the determination of iodide in two medicinal formulations. Idoxuridine was determined indirectly at the same electrode by accumulating it first at ?0.8 V vs. Ag/AgCl. At this potential the C? I bond in the adsorbed idoxuridine is reduced giving iodide, which is then determined at the modified electrode. The method was successfully applied to the determination of idoxuridine in a urine sample.     

A Laser Reduced Graphene Oxide Grid Electrode for the Voltammetric Determination of Carbaryl

Laser-reduced graphene oxide (LRGO) on a polyethylene terephthalate (PET) substrate was prepared in one step to obtain the LRGO grid electrode for sensitive carbaryl determination. The grid form results in a grid distribution of different electrochemically active zones affecting the electroactive substance diffusion towards the electrode surface and increasing the electrochemical sensitivity for carbaryl determination. Carbaryl is electrochemically irreversibly oxidized at the secondary amine moiety of the molecule with the loss of one proton and one electron in the pH range from 5 to 7 by linear scan voltammetry (LSV) on the LRGO grid electrode with a scan rate of 300 mV/s. Some interference of the juice matrix molecules does not significantly affect the LSV oxidation current of carbaryl on the LRGO grid electrode after adsorptive accumulation without applied potential. The LRGO grid electrode can be used for LSV determination of carbaryl in fruit juices in the concentration range from 0.25 to 128 mg/L with LOD of 0.1 mg/L. The fabrication of the LRGO grid electrode opens up possibilities for further inexpensive monitoring of carbaryl in other fruit juices and fruits     

Ni电极电化学流通池检测四环素类药品的研究

比较Au、GC和Ni电极对四环素的电化学响应,讨论了纯Ni电极对四环素的电催化氧化特性,提出以纯Ni为工作电极的电化学流通池,优化结构,建立了测定四环素类抗生素的电化学流通池安培检测法.该方法对四环素、土霉素和强力霉素都有较高的响应灵敏度,线性范围0.1～15mg/L.最低检出限分别为35、45和43μg/L.用此方法可以直接测定四环素类药品的含量.     

聚氯乙烯膜修饰碳微电极的研制及应用

采用浸涂流延法制得ＰＶＣ膜修饰碳微电极,用Ｋ３Ｆｅ（ＣＮ）６的循环伏安图考察了电极的电化学性能,并用此电极建立了环境水样中痕量汞的阳极溶出伏安法测定。在０．０６ｍｏｌ／Ｌ ＫＳＣＮ＋０．０１ｍｏｌ／ＬＫＣｌ介质中,富集电位－０．８０Ｖ,搅拌富集时间３００ｓ,扫描电压范围－０．２０～０．４０Ｖ,扫描速率３１４ｍＶ／ｓ,咄峰电流与Ｈｇ＾２＋浓度在０．０１～２．０ｍｇ／Ｌ的范围内有良好的线性关系,本电极     

基于双氨基三唑硫醚为中性载体的汞离子选择性电极的研究

研制了基于双氨基三唑硫醚为中性载体的阳离子选择性电极。实验表明,该电极对Hg2 具有良好的电位响应特性,在pH 2.0硝酸盐缓冲液中,电极电位呈近能斯特响应,线性响应范围为4.0 mg/L~20 g/L,斜率为33.4 mV/dec.(25℃),检出限为1.7 mg/L。该电极响应时间短(<10 s),pH范围较宽(1.3~3.3)。将该电极用于实际水样和二元混合溶液中Hg2 的检测,其结果令人满意。     

溴离子选择电极法测定有机化工产品中四丁基溴化铵的残留

建立了有机化工产品中四丁基溴化铵残留测定的新方法。该法线性范围为0.01~0.10 g/L,检出限为0.4 mg/L,相对标准偏差为2.4%(0.05 g/L,n=11),相关系数为0.998,用于实际样品测定,结果令人满意。     

Novel electrochemical procedure for the determination of metamitron

In this paper, a chronopotentiometric method for the determination of herbicide metamitron (MTM) using a glassy carbon electrode (GCE) and a thin film mercury electrode (TFME) as working electrodes is presented. MTM provided a well-defined reductive peak in the Britton–Robinson buffer on both working electrodes. Instrumental and chemical factors such as pH of the buffer, initial potential and reduction current influencing MTM chronopotentiometric response were optimised with the Box–Behnken experimental design. Under the optimal combination of factors, the analytical signal was linear in the MTM concentration range of 0.8–30 mg/L, with a detection limit of 68.53 µg/L using a TFME, and in the concentration range of 1–30 mg/L, with a detection limit of 92.91 µg/L using a GCE. The precision of the method was estimated as a function of repeatability and reproducibility, with the value of relative standard deviation lower than 2.6%. The applicability of the method was verified by direct analysis of MTM in spiked water samples and commercial pesticide formulations. The obtained results were in good agreement with those obtained using liquid chromatography/tandem mass spectrometry (LC-MS/MS) method, or with those labelled by the manufacturer. By using chronopotentiometry, neither extraction nor preconcentration procedures are necessary, thus making this method simple, cost-effective and more feasible for analytical routine analysis.