Sultan S M, Abdennabi A M, Almuaibed A M
Chemistry Department, King Fahd University of Petroleum and Minerals, KFUPM Box No. 2026, Dhahran 31261, Saudi Arabia.
Talanta. 1999 Aug 9;49(5):1051-7. doi: 10.1016/s0039-9140(99)00045-4.
An accurate selective flow injection chemiluminescence (CL) method for the assay of perphenazine was explored. In the method 394 ppm permanganate solution was used as a chemiluminogenic reagent in 0.289 mol dm(-3) sulphuric acid media. A photomultiplier tube was used as a detector at a total flow rate of 4.94 ml/min. Perphenazine was determined by a linear calibration plot of the following equation in the range 50-350 ppm: mV=-4.488+0.1162C, with a correlation coefficient of 0.9989 for five measurements and a relative standard deviation less than 2.33. A sampling frequency not less than 110 samples h(-1) was established. Three factors namely, the flow rate, sulphuric acid and permanganate concentrations were found to have an influence on the amount of chemiluminescence intensity produced. Therefore, their interaction effects were thoroughly investigated by employing the 2(3) factorial design chemometrical approach and the results obtained revealed a higher interaction between sulphuric acid and permanganate and a less significant interaction for both reagents with the flow rate. The interaction of variables observed necessitated the conduct of the super modified simplex optimization procedure which has resulted in offering the proper optimum conditions as stated above and led to the quantitative assay of perphenazine. An interference study indicated that the method was suitable for application in pharmaceutical preparations.
探索了一种准确的选择性流动注射化学发光(CL)法测定奋乃静。该方法中,在0.289 mol dm(-3)硫酸介质中,使用394 ppm的高锰酸钾溶液作为化学发光试剂。以光电倍增管作为检测器,总流速为4.94 ml/min。在50 - 350 ppm范围内,通过以下方程的线性校准曲线测定奋乃静:mV = -4.488 + 0.1162C,五次测量的相关系数为0.9989,相对标准偏差小于2.33。确定了采样频率不少于110个样品/h(-1)。发现流速、硫酸和高锰酸钾浓度这三个因素对产生的化学发光强度有影响。因此,采用2(3)析因设计化学计量学方法对它们的相互作用效应进行了深入研究,结果表明硫酸和高锰酸钾之间的相互作用较强,而两种试剂与流速之间的相互作用不太显著。观察到的变量相互作用需要进行超改进单纯形优化程序,该程序已得出上述适当的最佳条件,并实现了奋乃静的定量测定。干扰研究表明该方法适用于药物制剂分析。