Ibrahim F A, El-Enany N, El-Shaheny R N, Mikhail I E
Department of Analytical Chemistry, Mansoura University, 35516, Mansoura, Egypt.
Luminescence. 2015 Jun;30(4):485-94. doi: 10.1002/bio.2764. Epub 2014 Sep 10.
A rapid, simple, and sensitive second-derivative synchronous fluorimetric method has been developed and validated for the simultaneous analysis of a binary mixture of desloratadine (DSL) and montelukast sodium (MKT) in their co-formulated tablets. The method is based on measurement of the synchronous fluorescence intensities of the two drugs in McIlvaine's buffer, pH 2.3, in the presence of carboxy methyl cellulose sodium (CMC) as a fluorescence enhancer at a constant wavelength difference (Δλ) of 160 nm. The presence of CMC enhanced the synchronous fluorescence intensity of DSL by 216% and that of MKT by 28%. A linear dependence of the concentration on the amplitude of the second derivative synchronous fluorescence spectra was achieved over the ranges of 0.10-2.00 and 0.20-2.00 µg/mL with limits of detection of 0.02 and 0.03, and limits of quantification of 0.05 and 0.10 µg/mL for DSL and MKT, respectively. The proposed method was successfully applied for the determination of the studied compounds in laboratory-prepared mixtures and tablets. The results were in good agreement with those obtained with the comparison method. The high sensitivity attained by the proposed method allowed the determination of MKT in spiked human plasma with average % recovery of 100.11 ± 2.44 (n = 3).
已开发并验证了一种快速、简单且灵敏的二阶导数同步荧光法,用于同时分析氯雷他定(DSL)和孟鲁司特钠(MKT)复方片剂中的二元混合物。该方法基于在pH 2.3的McIlvaine缓冲液中,在羧甲基纤维素钠(CMC)作为荧光增强剂存在的情况下,以160 nm的恒定波长差(Δλ)测量两种药物的同步荧光强度。CMC的存在使DSL的同步荧光强度提高了216%,使MKT的同步荧光强度提高了28%。在0.10 - 2.00和0.20 - 2.00 μg/mL范围内,二阶导数同步荧光光谱的浓度与振幅呈线性关系,DSL和MKT的检测限分别为0.02和0.03 μg/mL,定量限分别为0.05和0.10 μg/mL。所提出的方法成功应用于实验室制备的混合物和片剂中所研究化合物的测定。结果与比较方法获得的结果高度一致。所提出的方法具有高灵敏度,可用于测定加标人血浆中的MKT,平均回收率为100.11 ± 2.44(n = 3)。