Apostolakis J C, Georgiou C A, Koupparis M A
Department of Chemistry, University of Athens, Greece.
Analyst. 1991 Mar;116(3):233-7. doi: 10.1039/an9911600233.
A flow injection (FI) kinetic potentiometric method for the determination of phenolic (acetaminophen and isoxsuprine) and hydrazino (isoniazid) drugs is described. This work shows the usefulness of ion-selective electrodes as detectors in FI systems, not only for direct ion determination but also in routine kinetic analysis. The method is based on the reaction of 1-fluoro-2,4-dinitrobenzene (FDNB) with the analytes in a weakly alkaline medium, which proceeds through the liberation of fluoride from the reagent. The slow reactions with phenols are catalysed by micelles of cetyltrimethylammonium bromide. The reaction rate is monitored with a fluoride-selective electrode in a wall-jet configuration and is used to construct a calibration graph of antilog(delta E/S)-1 versus c (where E = potential, s = slope of the electrode and c = concentration), using the fixed-time approach. The response time and the long-term stability of the electrode were found to be adequate for such kinetic determinations. The proposed method overcomes problems associated with end-point spectrophotometric methods using FDNB and allows measurements in highly coloured or turbid solutions. The optimized method has a linear concentration range of 1 x 10(-4)-50 x 10(-4) mol dm-3, a measurement throughput of 20 or 40 per hour and the precision ranges from 1.8 to 3.6% relative standard deviation (n = 3). Results obtained for commercial pharmaceutical formulations compare favourably with those given by reference methods.
描述了一种流动注射(FI)动力学电位法,用于测定酚类(对乙酰氨基酚和异舒普林)和肼类(异烟肼)药物。这项工作表明了离子选择性电极作为FI系统检测器的实用性,不仅可用于直接离子测定,还可用于常规动力学分析。该方法基于1-氟-2,4-二硝基苯(FDNB)与分析物在弱碱性介质中的反应,该反应通过试剂中氟化物的释放来进行。与酚类的缓慢反应由十六烷基三甲基溴化铵的胶束催化。用壁流配置的氟离子选择性电极监测反应速率,并使用固定时间法构建反对数(δE/S)-1对c(其中E =电位,s =电极斜率,c =浓度)的校准曲线。发现电极的响应时间和长期稳定性对于这种动力学测定是足够的。所提出的方法克服了使用FDNB的终点分光光度法相关的问题,并允许在高色度或浑浊溶液中进行测量。优化后的方法线性浓度范围为1×10(-4)-50×10(-4)mol dm-3,测量通量为每小时20或40次,精密度范围为相对标准偏差1.8%至3.6%(n = 3)。商业药物制剂获得的结果与参考方法给出的结果相比具有优势。