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一阶导数同步荧光光谱法同时测定复方舒必利和盐酸美贝维林片中的两种成分,并应用于实际人血浆。

First derivative synchronous fluorescence spectroscopy for the simultaneous determination of sulpiride and mebeverine hydrochloride in their combined tablets and application to real human plasma.

机构信息

Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, 35516, Mansoura, Egypt.

出版信息

J Fluoresc. 2010 Nov;20(6):1275-85. doi: 10.1007/s10895-010-0679-0. Epub 2010 Jul 7.

DOI:10.1007/s10895-010-0679-0
PMID:20607372
Abstract

A rapid, simple and highly sensitive first derivative synchronous fluorometric method has been developed for the simultaneous analysis of binary mixture of sulpiride (SUL) and mebeverine hydrochloride (MEB). The method is based upon measurement of the synchronous fluorescence intensity of these drugs at ∆λ = 100 nm in water. The different experimental parameters affecting the fluorescence of the two drugs were carefully studied and optimized. The fluorescence-concentration plots were rectilinear over the range of 0.05-1 µg/mL and 0.2-3.2 µg/mL for SUL and MEB respectively with lower detection limits (LOD) of 0.006 and 0.01 µg/mL and quantification limits (LOQ) of 0.0.02 and 0.05 µg/mL for SUL and MEB, respectively. The proposed method was successfully applied for the determination of the two compounds in synthetic mixtures and in commercial tablets. The high sensitivity attained by the proposed method allowed the determination of both of SUL and MEB metabolite (veratic acid) in real human plasma samples applying second derivative synchronous fluorometric technique. The mean% recoveries (n = 3) for both MEB metabolite (veratic acid) and SUL were 99.82 ± 2.53 and 98.84 ± 6.20 for spiked human plasma respectively, while for real human plasma, the mean% recoveries (n = 3) were 91.49 ± 4.25 and 91.36 ± 8.46 respectively.

摘要

一种快速、简单且高灵敏度的一阶导数同步荧光法已被开发用于同时分析舒必利(SUL)和盐酸美贝维林(MEB)的二元混合物。该方法基于在水相中测量这两种药物的同步荧光强度,其差值为∆λ=100nm。仔细研究并优化了影响两种药物荧光的不同实验参数。在 0.05-1μg/mL 和 0.2-3.2μg/mL 范围内,SUL 和 MEB 的荧光浓度图均呈线性,SUL 和 MEB 的检测限(LOD)分别为 0.006 和 0.01μg/mL,定量限(LOQ)分别为 0.002 和 0.05μg/mL。该方法成功应用于合成混合物和商业片剂中两种化合物的测定。所提出的方法具有较高的灵敏度,允许采用二阶导数同步荧光技术测定真实人血浆样品中 SUL 和 MEB 的代谢物(维替酸)。MEB 代谢物(维替酸)和 SUL 的平均回收率(n=3)分别为 99.82%±2.53%和 98.84%±6.20%,用于加标人血浆,而真实人血浆的平均回收率(n=3)分别为 91.49%±4.25%和 91.36%±8.46%。

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