Pagani Ariana P, Cabezón Miguel A, Ibáñez Gabriela A
Departamento de Química Analítica, Facultad de Ciencias Bioquímicas y Farmacéuticas, Universidad Nacional de Rosario and Instituto de Química Rosario, Consejo Nacional de Investigaciones Científicas y Técnicas, Rosario S2002LRK, Argentina.
Anal Sci. 2009 May;25(5):633-8. doi: 10.2116/analsci.25.633.
A simple and sensitive methodology for the simultaneous determination of levodopa and carbidopa in pharmaceutical samples is described. The method combines the advantages of fluorescence with partial least-squares (PLS) analysis, and requires no previous separation steps. The developed method is based on the oxidation of levodopa and carbidopa by cerium(IV) in a sulfuric acid medium and monitoring the fluorescence of the formed Ce(III) at lambda(exc) = 255 nm and lambda(em) = 355 nm. PLS uses differences in the reaction rates as a discriminatory parameter, and regresses the data of fluorescence vs. time onto the concentrations of the standards. Eight validation samples and seven commercial tablets were studied, using a nine-sample aqueous calibration set. The analyte recoveries from pharmaceuticals ranged from 98 to 101% for levodopa and from 100 to 108% for carbidopa. The results obtained by the developed method were statistically comparable to those obtained with high-performance liquid chromatography.
描述了一种用于同时测定药物样品中左旋多巴和卡比多巴的简单且灵敏的方法。该方法结合了荧光与偏最小二乘法(PLS)分析的优点,无需先前的分离步骤。所开发的方法基于在硫酸介质中铈(IV)氧化左旋多巴和卡比多巴,并在λ(exc)= 255 nm和λ(em)= 355 nm处监测形成的Ce(III)的荧光。PLS使用反应速率的差异作为判别参数,并将荧光与时间的数据回归到标准品的浓度上。使用九个样品的水溶液校准集研究了八个验证样品和七种商业片剂。药物中左旋多巴的分析物回收率为98%至101%,卡比多巴为100%至108%。所开发方法获得的结果在统计学上与高效液相色谱法获得的结果相当。