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首页> 外文期刊>Analytica chimica acta >High-performance liquid chromatography with fast-scanning fluorescence detection and multivariate curve resolution for the efficient determination of galantamine and its main metabolites in serum
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High-performance liquid chromatography with fast-scanning fluorescence detection and multivariate curve resolution for the efficient determination of galantamine and its main metabolites in serum

机译:高效液相色谱仪,具有快速扫描荧光检测和多变量曲线分辨率,可有效测定血清中的加兰他敏及其主要代谢产物

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摘要

Based on green analytical chemistry principles, an efficient approach was applied for the simultaneous determination of galantamine, a widely used cholinesterase inhibitor for the treatment of Alzheimer's disease, and its major metabolites in serum samples. After a simple serum deproteinization step, second-order data were rapidly obtained (less than 6min) with a chromatographic system operating in the isocratic regime using ammonium acetate/acetonitrile (94:6) as mobile phase. Detection was made with a fast-scanning spectrofluorimeter, which allowed the efficient collection of data to obtain matrices of fluorescence intensity as a function of retention time and emission wavelength/Successful resolution was achieved in the presence of matrix interferences in serum samples using multivariate curve resolution-alternating least-squares (MCR-ALS). The developed approach allows the quantification of the analytes at levels found in treated patients, without the need of applying either preconcentration or extraction steps. Limits of detection in the range between 8 and 11 ngmL~(-1), relative prediction errors from 7 to 12% and coefficients of variation from 4 to 1% were achieved.
机译:基于绿色分析化学原理,一种有效的方法被用于同时测定加兰他敏,加兰他敏是一种广泛使用的胆碱酯酶抑制剂,用于治疗阿尔茨海默氏病及其在血清样品中的主要代谢产物。经过简单的血清脱蛋白步骤后,使用乙酸铵/乙腈(94:6)作为流动相,通过等度色谱操作的色谱系统,快速获得了二级数据(不到6分钟)。使用快速扫描荧光分光光度计进行检测,该荧光分光光度计可以有效收集数据,以获得荧光强度的矩阵,该矩阵是保留时间和发射波长的函数/使用多变量曲线分辨率可在血清样品中存在基质干扰的情况下实现成功的分离度-交替最小二乘(MCR-ALS)。所开发的方法允许以治疗患者中发现的水平对分析物进行定量,而无需应用预浓缩或提取步骤。检出限在8〜11 ngmL〜(-1)之间,相对预测误差为7〜12%,变异系数为4〜1%。

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