Ovalles José F, Brunetto María Del Rosario, Gallignani Máximo
Analysis and Quality Control Department, Faculty of Pharmacy, University of Los Andes, Venezuela.
J Pharm Biomed Anal. 2005 Sep 1;39(1-2):294-8. doi: 10.1016/j.jpba.2005.02.030.
A simple and sensitive reversed-phase liquid chromatographic method has been developed for the determination of amikacin (AMK) by derivatization. The method is based on the pre-column derivatization of AMK with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC). The derivatization reaction proceeds in aqueous solution at room temperature with a borate buffer of pH 8.0. The formation of the corresponding derivative of AMK is instantaneous and it is stable for more than 36 h. Detection was performed by UV-absorption instead of fluorescence. Several factors influencing the derivatization reaction yields were studied and optimized. The system offered the following analytical parameters: limit of detection (LOD) of 0.068 micro g ml(-1) (3sigma), linear correlation coefficient of 0.9998 and linear range response from 2 to 50 microg ml(-1). The precision of the method was <1%. As a preliminary application, the method has been successfully applied to the amikacin determination in parenteral pharmaceutical formulations.
已开发出一种简单灵敏的反相液相色谱法,用于通过衍生化测定阿米卡星(AMK)。该方法基于AMK与6-氨基喹啉-N-羟基琥珀酰亚胺基氨基甲酸酯(AQC)的柱前衍生化。衍生化反应在室温下于pH 8.0的硼酸盐缓冲水溶液中进行。AMK相应衍生物的形成是瞬时的,并且在超过36小时内稳定。通过紫外吸收而非荧光进行检测。研究并优化了影响衍生化反应产率的几个因素。该系统提供了以下分析参数:检测限(LOD)为0.068μg ml⁻¹(3σ),线性相关系数为0.9998,线性范围响应为2至50μg ml⁻¹。该方法的精密度<1%。作为初步应用,该方法已成功应用于注射用药物制剂中阿米卡星的测定。