Aboshabana Rasha, Zeid Abdallah M, Ibrahim Fawzia A
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt.
Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura 35516, Egypt; Department of Chemistry, University of Michigan, Ann Arbor, 48109, MI, United States.
Spectrochim Acta A Mol Biomol Spectrosc. 2023 Jul 5;295:122626. doi: 10.1016/j.saa.2023.122626. Epub 2023 Mar 15.
In this work, a label-free, rapid, and sensitive synchronous spectrofluorometric method was implemented to assay atenolol (ATL) and ivabradine hydrochloride (IVB) in pharmaceutical and biological matrices. Simultaneous determination of ATL and IVB by conventional spectrofluorometry cannot be implemented because of the clear overlap of the emmision spectra of ATL and IVB. To overcome this problem, synchronous fluorescence measurements at a constant wavelength difference (Δλ) combined with mathematical derivatization of the zero order spectra were perforemed. The results indicated a good resolution between emission spectra of the studied drugs when the first-order derivative of the synchronous fluorescence scans at Δλ = 40 nm was conducted using ethanol as the optimum solvent which is less hazardous than other organic solvents such as methanol and acetonitrile, keeping the method safe and green. The amplitudes of the first derivative synchronous fluorescent scans of ATL and IVB in ethanol were monitored at 286 and 270 nm to simultaneously estimate ATL and IVB, respectively. Method optimisation was conducted by assessing different solvents, buffer pHs, and surfactants. The optimum results were obtained when ethanol was utilized as a solvent without using any other additives. The developed method was linear over concentration ranges of 10.0-250.0 ng mL for IVB and 100.0-800.0 ng mL for ATL with detection limits of 3.07 and 26.49 ng mL for IVB and ATL, respectively. The method was utilized to assay the studied drugs in their dosages and in human urine samples with acceptable % recoveries and RSD values. The greenness of the method was implemented by three approaches involving the recently reported metric (AGREE) which ensured the eco-freindship and safety of the method.
在本研究中，我们采用了一种无标记、快速且灵敏的同步荧光光谱法来测定药物和生物基质中的阿替洛尔（ATL）和盐酸伊伐布雷定（IVB）。由于ATL和IVB发射光谱明显重叠，无法采用传统荧光光谱法同时测定ATL和IVB。为解决这一问题，我们进行了固定波长差（Δλ）的同步荧光测量，并结合零阶光谱的数学导数处理。结果表明，以乙醇作为最佳溶剂（比甲醇和乙腈等其他有机溶剂危害小，使方法安全且绿色），在Δλ = 40 nm下进行同步荧光扫描的一阶导数测量时，所研究药物的发射光谱之间具有良好的分辨率。在乙醇中，分别于286和270 nm监测ATL和IVB的一阶导数同步荧光扫描幅度，以同时估算ATL和IVB。通过评估不同溶剂、缓冲液pH值和表面活性剂进行方法优化。当仅使用乙醇作为溶剂而不添加任何其他添加剂时，获得了最佳结果。所建立的方法在IVB浓度范围为10.0 - 250.0 ng/mL和ATL浓度范围为100.0 - 800.0 ng/mL内呈线性，IVB和ATL的检测限分别为3.07和26.49 ng/mL。该方法用于测定所研究药物的制剂及人尿样中的含量，回收率和相对标准偏差（RSD）值均可接受。该方法的绿色性通过三种方法实现，包括最近报道的指标（AGREE），确保了该方法的环境友好性和安全性。
