首页> 外文期刊>Acta Chimica Slovenica >The Possibility of Simultaneous Voltammetric Determination of Desloratadine and 3-Hydroxydesloratadine
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The Possibility of Simultaneous Voltammetric Determination of Desloratadine and 3-Hydroxydesloratadine

机译:同时伏安法测定地氯雷他定和3-羟基地氯雷他定的可能性

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摘要

The electrochemical behaviour of desloratadine (DLOR) and its derivative 3-hydroxydesloratadine (3OH-DLOR) was investigated by direct current (DCP) polarography, cyclic (CV), differential pulse (DPV) and square-wave (SWV) vol-tammetry in Britton-Robinson (BR) buffer solutions (pH 4-11). Both compounds are reduced at mercury electrode in irreversible two electron reduction of the C=N bond of the pyridine ring in their molecules. The difference in their electrochemical behaviour was investigated, and the most pronounced distinction is observed at pH > 9, as a consequence of the deprotonation of the phenolic moiety in 3OH-DLOR molecule, yielding significant change in their reduction potentials (E_(p DLOR ) = -1.48 V, and E_(p 3OH-DLOR) = -1.6 V). The observed results correlate with calculated LUMO energy levels and Hammet substituent constants (σ). Based on the difference in the reduction potential for DLOR and 30H-DLOR, conditions for simultaneous determination these two molecules in alkaline medium were established. The best selectivity was achieved using SWV method at pH 10. The linearity of the calibration graphs were achieved in the concentration range from 1.5 x 10~(-6)M - 1 x 10~(-5)M for DLOR and 7.5 x 10~(-6) M - 5 x 10~(-5) M for 30H-DLOR with detection limits of 2.29 x 10~(-7) M and 2.08 x 10~(-6) M, and determination limits of 7.64 x 10~(-7) M and 6.94 x 10~(-6) M, for DLOR and 30H-DL0R, respectively. The method was checked in human plasma sample. Good response was obtained with LOD and LOQ values of 4.63 x 10~(-7)M and 1.54 x 10~(-6)M, for DLOR and 2.39 x 10~(-6)M and 7.97 x 10~(-6)M, 3OH-DLOR, respectively.
机译:通过直流(DCP)极谱法,循环(CV),微分脉冲(DPV)和方波(SWV)伏安法研究了去氯雷他定(DLOR)及其衍生物3-羟基去氯雷他定(3OH-DLOR)的电化学行为。 Britton-Robinson(BR)缓冲溶液(pH 4-11)。两种化合物在汞电极上均以不可逆的两个电子还原,其分子中的吡啶环的C = N键被还原。研究了它们的电化学行为的差异,并且由于3OH-DLOR分子中酚类部分的去质子化,在pH> 9时观察到了最明显的区别,从而使它们的还原电位发生了显着变化(E_(p DLOR) = -1.48 V,并且E_(p 3OH-DLOR)= -1.6 V)。观察到的结果与计算的LUMO能级和Hammet取代基常数(σ)相关。根据DLOR和30H-DLOR还原电位的差异,建立了同时测定碱性介质中这两个分子的条件。使用SWV方法在pH 10时可获得最佳选择性。在DLOR和7.5 x 10的浓度范围为1.5 x 10〜(-6)M-1 x 10〜(-5)M范围内,可实现校准图的线性30H-DLOR的〜(-6)M-5 x 10〜(-5)M,检测极限为2.29 x 10〜(-7)M和2.08 x 10〜(-6)M,测定极限为7.64 x DLOR和30H-DL0R分别为10〜(-7)M和6.94 x 10〜(-6)M.在人血浆样本中检查了该方法。对于DLOR,2.39 x 10〜(-6)M和7.97 x 10〜(-6),LOD和LOQ值分别为4.63 x 10〜(-7)M和1.54 x 10〜(-6)M时获得了良好的响应。 M,3OH-DLOR。

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