咖啡因离子选择性电极的研制及其用于测定可乐饮料中咖啡因

研制了以咖啡因-磷钼酸缔合物为电活性物质的离子选择性电极。试验表明:该离子选择性电极对咖啡因具有良好的选择性和电位响应特性。在pH 2.54磷酸盐缓冲溶液中,电极电位呈现能斯特响应,线性范围为5.0×10~(-6)～1.0×10~(-2)mol·L~(-1),斜率为51.4mV·pc~(-1)。将该电极用于测定可乐饮料中咖啡因的含量,测得方法的回收率在98.4%～102.4%之间。     

磷钼酸修饰的铂电极对二甲醚氧化的电催化作用

利用循环伏安扫描法制备了磷钼酸(H3PMo12O40)修饰的铂电极.在制备修饰电极时,随着扫描次数的增加,磷钼酸的氧化还原峰电流增大,但最终获得稳定的重现性好的磷钼酸修饰的铂电极.通过循环伏安法研究了该修饰电极对二甲醚氧化的电催化反应.结果表明,与未修饰的铂电极相比,磷钼酸修饰的铂电极电催化氧化二甲醚的起始氧化电位负移50 mV,氧化峰电位负移35 mV,氧化峰电流密度提高了1.86倍,这表明修饰电极的电催化活性有了很大的提高.同时,电位负扫时,二甲醚在425 mV(vsSCE)处出现氧化峰,表明二甲醚在修饰电极上的电氧化机理可能发生了改变.实验还发现,制备修饰电极时,降低扫速会提高还原物质杂多蓝的吸附量,但过多的修饰物质会降低铂的活性位数目,反而降低了对二甲醚氧化的电催化作用.     

氧氟沙星选择性电极的制备及其性能研究

氧氟沙星是一种新型广谱抗菌素类药物 ,其含量测定的标准方法是高效液相色谱法 ,用离子选择性电极测定氧氟沙星的方法尚未见报道 .以氧氟沙星与四苯硼酸根形成的缔合物为电活性物质首次研制了一种氧氟沙星PVC膜涂层玻璃电极 ,用于氧氟沙星制剂的测定 .实验表明 ,该电极的Nernst响应范围为 5 .0× 10 -5～ 5 .0× 10 -3mol/L ;斜率为 5 1.8mV/pC ;该电极制作方法简单 ,响应迅速 ,重现性好 ,用于氧氟沙星注射液和口服胶囊的测定 ,所得结果与高效液相色谱法一致     

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。     

左氧氟沙星选择性电极的制备及其性能研究

以左氧氟沙星与四苯硼酸根形成的缔合物为电活性物质,研制了一种左氧氟沙星PVC膜涂层玻璃电极,并对其响应性能进行了系统研究.实验表明,该电极的Nernst响应范围为5.0×10-3～2.0×10-5 moL/L,斜率为51.7 mV/pC,适用pH范围为3.0～4.5.该电极制作方法简单,响应迅速,重现性好,用于左氧氟沙星注射液和片剂的测定.     

固体石蜡碳糊—磷钼酸根电极的研制与应用

研究了以固体石蜡作粘和剂的碳糊电极,在磷钼酸溶液中活化一定时间后,该电极对1.0×10~(-6)～5.0×10~(-4)mol·L~(-1)的磷钼酸有能斯特响应,斜率约为30mV,检出限为3.2×10~(-7)mol·L~(-1).电极的稳定性和选择性较好,已用于矿石、水样中磷的测定,结果满意.     

乙基紫—高氯酸根缔合物体系的界面电荷转移性质的研究

用油/水界面电化学方法研究离子选择性电极的响应机理,已取得了一定的进展。考虑到以乙基紫-高氯酸根缔合物为电活性物质的高氯酸根离子选择性电极,具有良好的电极行为,故拟对此体系的界面电荷转移行为进行研究,从理论上探讨该电极系统的电极响应行为。     

咪唑四氟硼酸盐离子液体中磷钼酸掺杂聚吡咯薄膜修饰电极的制备及其电催化活性

以1-丁基-3-甲基咪唑四氟硼酸盐(BMIMBF4)离子液体作为介质,利用电化学方法在铂电极表面制备了磷钼酸掺杂聚吡咯薄膜;采用扫描电子显微镜观察了所制备的薄膜的形貌,利用热重分析评价了其热稳定性,利用循环伏安法测定了其电化学活性和对甲醇的电催化氧化活性.结果表明,与传统的硫酸溶液相比,以BMI-MBF4离子液体作为反应介质制备的修饰电极的表面形貌更均匀,电化学活性和对甲醇的电催化氧化活性更强.     

十二烷基二甲基苄基溴化铵离子选择电极的制备与性能

以四苯硼钠作为电活性物质,用溶胶-凝胶方法制备的阳离子表面活性剂离子选择电极对十二烷基二甲基苄基溴化铵具有良好的能斯特响应特性,其线性响应范围为1.0×10-3~1.58×10-6mol·L-1,斜率为57.8mV/pc(pc=-logc),适宜的pH范围为4.0~10.0.同时该电极显示了较好的选择性,重现性和稳定性.用该电极对十二烷基二甲基苄基溴化铵进行了回收率试验,效果很好,对其溶液试样进行了分析,结果和标准方法一致.     

双冠醚PVC膜钾电极的研究

Kimura等报道了双冠醚,庚二酸二-[3,4-(1’,4’,7’,10’,13’-五氧杂环十五-2-烯)骈苄酯](简称双冠醚A),并用作钾离子选择性电极的活性物质。朱春生等最近报道了双冠醚B的合成。本文研究了上述两种双冠醚作为电活性物质的PVC膜钾离子选择性电极,并与目前以二叔丁基二苯骈-30-冠-10为电活性物质的PVC商品钾电极作对比,实验结果说明双冠醚钾电极在测量范围,对Na~+,NH_4~+等离子的选择性系数,pH范围等方面均优于商品电极。     

聚氯乙烯膜氧氟沙星和曲马多选择电极的研制与应用

报道了以氧氟沙星碘化物与碘化铋的分子缔合物为电活性物的新型聚氯乙烯膜氧氟沙星选择电极。并以类似的方法报道了曲马多选择电极。氧氟沙星电极的特响应范围为１．０×１０＾－２－２．２×１０＾－５ｍｏｌ／Ｌ，斜率为３０ｍＶ／ＰＣ，检测限为１．６×１０＾－５ｍｏｌ／Ｌ。     

涂碳CdBr42-离子选择电极的研制

R.W.Cattrall等曾研制PVC膜CdCl₄^2-离子选择电极,其线性响应范围10^-1-10^-4M,级差26-28mV。本文报道以三辛基十二烷基碘化铵与镉澳络阴离子形成的缔合物为电活性物的涂碳(PVC膜)CdBr₄^2-离子选择电极的研究结果。     

Ion-selective electrode for the determination of trazodone in tablets

A coated wire trazodone-selective electrode based on incorporation of trazodone-tetraphenylborate ion pair in a poly(vinylchloride) coating membrane was constructed. The influences of membrane composition, temperature, pH of the test solution, and foreign ions on the electrode performance were investigated. The electrode showed a Nernstian response over a trazodone concentration range from 1.41 x 10(-5) to 0.89 x 10(-2) M, at 25 degrees C, and was found to be very selective, precise, and usable within the pH range 2.4-9.0. The standard electrode potentials, E degree, were determined at 20, 25, 30, 35, 40 and 45 degrees C and used to calculate the isothermal temperature coefficient (dE degree/dT) of the electrode. Temperatures higher than 45 degrees C seriously affected the electrode performance. The electrode was successfully used for potentiometric determination of trazodone hydrochloride both in pure solutions and in pharmaceutical preparations.     

Evaluation of a PVC‐Based Thionine‐Zeolite and Zeolite Free Membranes as Sensing Elements in Ion Selective Electrode

The construction and performance characteristics of thionine electrodes based on the ion‐pair complex thionine‐tungstophosphate and thionine‐mordenite zeolite embedded in a polyvinyl chloride (PVC) matrix is described. Thionine electrode based on the ion‐pair is used for the indirect determination of ascorbic acid by standard addition method.     

Development of Nalbuphine‐Selective Membrane Electrode and Its Applications in Pharmaceutical Analysis

Abstract

A nalbuphine ion‐selective PVC membrane electrode based on ion‐pair complex of nalbuphine with tetra phenyl borate was prepared with di‐butyl sebacate as a plasticizer. The electrode exhibits a linear response with a Nernstain slope 59.6 mV decate^?1 at 25°C with the concentration range of 1×10^?6?1×10^?2 M nalbuphine. The electrode response was not sensitive to pH changes from 3.5–7 and not affected by possible interfering species such as common inorganic cations, sugars and amino‐acids. The electrode shows good stability, reproducibility and fast response. These characteristics of the electrode enable it to be used successfully for the determination of nalbuphine hydrochloride in pure form and in pharmaceutical preparations.     

Ion Selective Electrode for Potentiometric Determination of Saccharin Using a Thin Film of Silsesquioxane 3-n-Propylpyridinium Chloride Polymer Coated-Graphite Rod

ABSTRACT

A polymer coated graphite rod ion selective electrode for saccharin was constructed and evaluated for the determination of saccharin in artificial table top sweeteners. The polymer consists of a thin film of silsesquioxane 3-n-propylpyridinium chloride. The electrode response was based on the ion pair formed between saccharinate and the 3-n-propylpyridinium cation from the silsequioxane polymer. The electrode exhibits a Nernstian response for saccharin concentrations between 6.9×10^-6 and 5.3×10^-3 mol L^-1 and a detection limit of 5.5×10^-6 mol L^-1. The electrode response for saccharin was fast (10-20 s) and the potential independent of pH in the range of 3 to 7. The selectivity coefficients K _{A, B} ^pot for several anions usually present in commercial table top sweeteners were determined following the IUPAC recommendations. The potentiometric method with the ion selective electrode was validated by the HPLC reference method, through t8543226 determination of saccharin in commercial samples of table top sweeteners. The ion selective electrode is proved suitable for the routine quality control of table top sweeteners by potentiometry.     

二氧化钛溶胶凝胶膜修饰的维生素B6电极

制备了一种以硅钨酸为定域体试剂,用溶胶-凝胶技术制作的新型维生素B6电极,详尽讨论了电极性能的影响因素。电极斜率为58.0 mV/dec,线性范围为1.0×10-2～4.0×10-6mol/L,检测限为2.5×10-6mol/L。该电极易于批量生产和微型化,用于样品分析,结果令人满意。     

Development and Optimization of an Ion‐selective Electrode for Serotonin Detection

Our studies are focused on the development of novel potentiometric sensors for the quantification of the neurotransmitter serotonin. Therefore, ion‐selective electrodes based on plasticized PVC membranes are applied. The electroactive part of the membrane consists of an ion pair complex formed between the protonated analyte and a carborane anion [Co(1,2‐C₂B₉H₁₁)₂]⁻. The analytical performance of the electrode was studied regarding sensitivity, concentration range, limit of detection and potential stability. The ion‐selective electrodes were optimized with respect to the material of the transducing element, as well as the membrane thickness and its composition. Stable, all solid state ISEs could be developed, using the non‐polar plasticizer NPOE and a graphite rod with high surface area as transducing element. We thus achieved a near Nernstian response over three decades of concentration (2.25⋅10^‐5‐1.00⋅10^‐2 M) and a limit of detection in the μ‐molar range for the optimized electrodes. The electrodes could successfully be miniaturized using carbon based screen printed electrodes.     

New Ion‐Pair Based All‐Solid‐State Surfactant Sensitive Sensor for Potentiometric Determination of Cationic Surfactants

Cationic surfactants of different types were determined using a few potentiometric sensors based on ion‐pair complexes (dodecyldimethylbenzylammonium dodecylsulfate, dodecylmethylbenzylammonium dodecylbenzensulfonate, tetrahexadecylammonium dodecylsulfate and Hyamine (benzethonium dodecylsulfate)) as sensing materials. The response of the all‐solid state surfactant sensitive electrode based on a Teflonized graphite conducting substrate, coated with a PVC membrane containing sensing material, was investigated in the solutions of Hyamine and hexadecyltrimethylammonium ion in the concentration range from 1 μM to 10 mM. Potentiometric surfactant cation titration has been performed using sodium dodecylsulfate as titrant and an ion‐pair‐based surfactant sensitive electrode as a potentiometric indicator. Several commercial surfactant products have also been titrated and the results were compared with those obtained with two‐phase standard titration method.     

Diffusion layer based probe-in-tube microdevice for selective analysis of electroactive species

A probe-in-tube microdevice based on the concept of diffusion layer gap electrode pair which we proposed recently was designed to selectively analyze electroactive species in the presence of interferents. In this device, a detecting probe electrode was inserted into a cylindrical tube electrode. The gap distance between both electrodes was in the range of diffusion layer thickness. The effectiveness of the device was confirmed by experiments using model system of the electrooxidation of hydrogen peroxide in solution. In practical performance of the microdevice, parameters influencing the interference-removing efficiency were investigated systematically. Under optimal conditions, selective analysis of hydrogen peroxide could be performed free from interferences.