Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Cairo, Egypt.
Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Cairo, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2018 Jan 5;188:619-625. doi: 10.1016/j.saa.2017.07.052. Epub 2017 Jul 29.
Simple, smart and sensitive normal fluorescence and stability-indicating derivative synchronous spectrofluorimetric methods have been developed and validated for the determination of gliquidone in the drug substance and drug product. Normal spectrofluorimetric method of gliquidone was established in methanol at λ excitation 225nm and λ emission 400nm in concentration range 0.2-3μg/ml with LOD equal 0.028. The fluorescence quantum yield of gliquidone was calculated using quinine sulfate as a reference and found to be 0.542. Stability-indicating first and third derivative synchronous fluorescence spectroscopy were successfully utilized to overcome the overlapped spectra in normal fluorescence of gliquidone and its alkaline degradation product. Derivative synchronous methods are based on using the synchronous fluorescence of gliquidone and its degradation product in methanol at Δ λ50nm. Peak amplitude in the first derivative of synchronous fluorescence spectra was measured at 309nm where degradation product showed zero-crossing without interference. The peak amplitudes in the third derivative of synchronous fluorescence spectra, peak to trough were measured at 316,329nm where degradation product showed zero-crossing. The different experimental parameters affecting the normal and synchronous fluorescence intensity of gliquidone were studied and optimized. Moreover, the cited methods have been validated as per ICH guidelines. The peak amplitude-concentration plots of the derivative synchronous fluorescence were linear over the concentration range 0.05-2μg/ml for gliquidone. Limits of detection were 0.020 and 0.022 in first and third derivative synchronous spectra, respectively. The adopted methods were successfully applied to commercial tablets and the results demonstrated that the derivative synchronous fluorescence spectroscopy is a powerful stability-indicating method, suitable for routine use with a short analysis time. Statistical comparison between the results obtained by normal fluorescence and derivative synchronous methods and the official one using student's t-test and F-ratio showed no significant difference regarding accuracy and precision.
已经开发并验证了简单、智能和灵敏的普通荧光和稳定指示导数同步荧光光谱法，用于测定药物中的格列喹酮。在甲醇中建立了格列喹酮的普通荧光光谱法，在 λ 激发 225nm 和 λ 发射 400nm 处，浓度范围为 0.2-3μg/ml，LOD 等于 0.028。使用硫酸奎宁作为参比物计算了格列喹酮的荧光量子产率，发现为 0.542。成功地利用稳定指示一阶和三阶导数同步荧光光谱法克服了格列喹酮及其碱性降解产物在普通荧光中的重叠光谱。导数同步方法基于在甲醇中使用格列喹酮及其降解产物的同步荧光，Δ λ 50nm。在一阶导数同步荧光光谱中，在 309nm 处测量降解产物的峰振幅为零交叉，没有干扰。在三阶导数同步荧光光谱中，峰谷处测量的峰振幅在 316、329nm 处，降解产物为零交叉。研究和优化了影响格列喹酮普通和同步荧光强度的不同实验参数。此外，所引用的方法已根据 ICH 指南进行了验证。导数同步荧光的峰振幅-浓度曲线在格列喹酮的浓度范围为 0.05-2μg/ml 时呈线性。一阶和三阶导数同步光谱的检出限分别为 0.020 和 0.022。所采用的方法成功地应用于商业片剂，结果表明，导数同步荧光光谱法是一种强大的稳定指示方法，适合常规使用，分析时间短。使用学生 t 检验和 F 比对普通荧光和导数同步方法与官方方法的结果进行的统计比较表明，在准确性和精密度方面没有显著差异。
