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High performance liquid chromatographic determination of proguanil after derivatisation with sodium benzoxazole-2-sulphonate

机译:用苯并恶唑-2-磺酸钠衍生化衍生后Proguanil的高效液相色谱法测定

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A simple, fast and reproducible method for the determination of proguanil using high performance liquid chromatographic with UV/Fluorescence detection is described. Proguanil was derivatised to its corresponding derivative [(N1-(4-chlorophenyl)-N5-(1 -methyl ethyl) imidocarbonimideamide-N-benzoxazole]. The derivatisation reaction was conducted in methanol at 60°C using sodium benzoxazole-2-sulphonate under alkaline conditions. The resulting derivative was extracted with chloroform after which the extract was observed under UV lamp at 254 nm before TLC and HPLC analysis. Similarly, the derivatisation process was adapted for derivatisation of proguanil in urine sample. The reaction proceeded smoothly and rapidly. The extraction process was not cumbersome and eliminated the need for costly extraction and evaporation equipments. The resulting derivative fluorensced intensely under UV lamp. Direct HPLC analysis of the reaction mixture was found possible without interferences from excess reagent and endogeneous compounds like ammonium salts. The derivative eluted in less than seven minutes thus making the method suitable for routine use. The calibration plot was linear over the concentration range. A correlation regression of the order of 0.94 was obtained from the calibration curve which indicated a strong relationship between the instrument response and the concentration of proguanil. The discussion also summarizes the derivatisation chemistry that have not being fully explored to date but may find utility in future development of highly sensitive analytical methods for biquanide drugs.
机译:描述了使用高效液相色谱法测定具有UV /荧光检测的高效液相色谱的简单,快速和可再现的方法。前川以其相应的衍生物[(N1-(4-氯苯基)-N5-(1--甲基乙基)咪偶甲酰胺-N-苯并唑]。使用苯并恶唑-2-磺酸钠在60℃下在甲醇中在甲醇中进行衍生化反应在碱性条件下。用氯仿萃取所得衍生物,之后在TLC和HPLC分析之前在254nm下观察到提取物。类似地,衍生化方法适于尿液样品中Proguanil的衍生化。平稳又快速地进行了衍生物。提取过程不繁琐,消除了昂贵的提取和蒸发设备的需求。所得衍生衍生物在紫外灯下强烈荧光。反应混合物的直接HPLC分析没有来自过量试剂和未成期的铵盐的干扰。该衍生物在不到七分钟内洗脱,因此使该方法适用于常规用途。校准绘图在浓度范围内线性。从校准曲线获得0.94的顺序的相关回归,该校准曲线表示仪器响应与Proguanil的浓度之间的强烈关系。讨论还总结了迄今为止没有完全探索的衍生化学,但可能在未来发展益芳药物的高敏感分析方法的发展中找到效用。

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