Adawy Hamees A, Hegazy Maha A, Saad Samah S, Boltia Shereen A
Pharmaceutical Analytical Chemistry Department, College of Pharmaceutical Sciences and Drug Manufacturing, Misr University for Science & Technology, 6th of October City, Giza, 16878, Egypt.
Pharmaceutical Chemistry Department, Faculty of Pharmacy, Future University in Egypt, Cairo, 11835, Egypt.
J Fluoresc. 2025 Jan 16. doi: 10.1007/s10895-024-04100-1.
Highly sensitive spectrofluorimetric methods were developed for the quantitative estimation of formoterol fumarate dihydrate (FFD) and fluticasone propionate (FP) in both authentic raw materials and marketed dosage forms using a micellar-enhanced spectrofluorimetric approach. The proposed methods are based on the determination of FP in the presence of FFD using the first derivative emission spectrofluorimetry. The peak amplitude of the emission spectra of the formed micellar fluorescence was measured at 465 nm after excitation at 236 nm (λ max of FP).The second method quantifies FFD in the presence of FP using second derivative emission spectrofluorimetry. This method measures the peak amplitude of the emission spectra of the formed micelle at 283 nm, where there is no interference from FP, following excitation at 214 nm. In these methods, the emission spectra of the target drugs are measured after micellar formation, with excitation wavelengths at 214 nm for FFD and 236 nm for FP. The fluorescence intensity was enhanced using β-cyclodextrin as a micellar system after optimizing parameters affecting native fluorescence, such as diluting solvents, surfactants, and varying concentrations of β-cyclodextrin. A linear relationship was observed between the fluorescence intensity and concentration for FP over the range of 50-100 ng/mL and for FFD over the range of 30-700 ng/mL. The developed methods are simple, sensitive, non-extractive, economical, and suitable for routine analysis of FFD and FP in their raw materials and combined marketed dosage forms. The proposed techniques were carefully validated for linearity, accuracy, precision, and specificity according to the International Council for Harmonization (ICH) guidelines, demonstrating high sensitivity with lower limits of detection and quantitation. Additionally, the analytical greenness of the suggested procedures was assessed using the Analytical Greenness Metric Approach (AGREE), the Red-Green-Blue model, and the Green Procedure Analytical Index (GAPI).
采用胶束增强荧光光谱法，开发了高灵敏度荧光光谱法，用于定量测定富马酸福莫特罗二水合物（FFD）和丙酸氟替卡松（FP）原料药及市售剂型中的含量。所提出的方法基于在FFD存在下使用一阶导数发射荧光光谱法测定FP。在236nm（FP的λmax）激发后，在465nm处测量形成的胶束荧光发射光谱的峰高。第二种方法使用二阶导数发射荧光光谱法在FP存在下定量FFD。该方法在214nm激发后，测量在283nm处形成的胶束发射光谱的峰高，此处不受FP干扰。在这些方法中，在胶束形成后测量目标药物的发射光谱，FFD的激发波长为214nm，FP的激发波长为236nm。在优化影响天然荧光的参数（如稀释溶剂、表面活性剂和不同浓度的β-环糊精）后，使用β-环糊精作为胶束体系增强荧光强度。在50-100ng/mL范围内，FP的荧光强度与浓度呈线性关系；在30-700ng/mL范围内，FFD的荧光强度与浓度呈线性关系。所开发的方法简单、灵敏、非萃取、经济，适用于FFD和FP原料药及其组合市售剂型的常规分析。根据国际协调理事会（ICH）指南，对所提出的技术进行了线性、准确性、精密度和特异性的仔细验证，显示出高灵敏度和较低的检测限与定量限。此外，使用分析绿色度度量方法（AGREE）、红-绿-蓝模型和绿色分析程序指数（GAPI）评估了所建议程序的分析绿色度。
