Magdy Galal, Belal Fathalla, Abdel-Megied Ahmed M, Abdel Hakiem Ahmed F
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Kafrelsheikh University, P.O. Box 33511, Kafrelsheikh, Egypt.
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Mansoura University, P.O. Box 35516, Mansoura, Egypt.
R Soc Open Sci. 2021 May 26;8(5):210354. doi: 10.1098/rsos.210354.
Two green, simple and sensitive synchronous spectrofluorimetric methods were developed for the first time for the simultaneous estimation of febuxostat (FEB) and ibuprofen (IBU). Method I is constant-wavelength synchronous spectrofluorimetry where FEB and IBU were recorded at 329 and 258 nm, respectively, using Δ of 40 nm. Method II is constant-energy synchronous spectrofluorimetry using a wavenumber interval of -4000 cm. All measurements were carried out in a borate buffer of pH 7 and distilled water for dilution which increased the methods' greenness. The two methods were rectilinear over concentration ranges of 30.0-700.0 ng ml and 0.5-9.0 µg ml in the first method and 20.0-500.0 ng ml and 0.1-8.0 µg ml in the second method for FEB and IBU, respectively. High sensitivity was attained for the two drugs with limits of quantitations (LODs) down to 0.41 and 5.51 ng ml in the first method and 0.25 and 3.32 ng ml in the second method for FEB and IBU, respectively. Recovery percentages were in the range of 97.3-101.9% after extraction from spiked human plasma samples, demonstrating high bioanalytical applicability. The two methods were further applied to tablet dosage forms with good recovery results. The methods' greenness was assessed according to the analytical Eco-Scale and Green Analytical Procedure Index guidelines.
首次开发了两种绿色、简单且灵敏的同步荧光光谱法,用于同时测定非布司他(FEB)和布洛芬(IBU)。方法一是恒波长同步荧光光谱法,其中FEB和IBU分别在329 nm和258 nm处记录,波长差(Δ)为40 nm。方法二是恒能量同步荧光光谱法,波数间隔为 -4000 cm⁻¹。所有测量均在pH 7的硼酸盐缓冲液中进行,并使用蒸馏水稀释,这提高了方法的绿色度。对于FEB和IBU,两种方法在第一种方法中分别在30.0 - 700.0 ng/ml和0.5 - 9.0 μg/ml的浓度范围内呈线性,在第二种方法中分别在20.0 - 500.0 ng/ml和0.1 - 8.0 μg/ml的浓度范围内呈线性。两种药物均具有高灵敏度,第一种方法中FEB和IBU的定量限(LOD)分别低至0.41和5.51 ng/ml,第二种方法中分别低至0.25和3.32 ng/ml。从加标人血浆样品中提取后回收率在97.3 - 101.9%范围内,表明具有高生物分析适用性。这两种方法进一步应用于片剂剂型,回收率良好。根据分析生态尺度和绿色分析程序指数指南评估了方法的绿色度。