Pharmaceutical Chemistry Department, Faculty of Pharmacy, Egyptian Russian University, Badr City, Cairo 11829, Egypt.
Analytical Chemistry Department, Faculty of Pharmacy, Zagazig University, Zagazig 44519, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2021 Jul 5;255:119715. doi: 10.1016/j.saa.2021.119715. Epub 2021 Mar 19.
Dapoxetine hydrochloride (DAP) and sildenafil citrate (SIL) have proven clinically effective in the treatment of comorbid conditions like erectile dysfunction and premature ejaculation. The analysis of DAP and SIL combinations represents a challenge because of the severe overlap of these compounds' spectra. Six newly developed methods were proven effective for resolving such a challenging overlap. They also exhibited the advantage of simplicity as they depend on the zero-order spectrum and only require simple mathematical handling.
We suggested six simple, precise, and sensitive spectrophotometric methods based on mathematical filtration techniques and ratio spectra manipulations to resolve the spectra of DAP and SIL in their bulk and combined pharmaceutical dosage form and estimate the relevant individual concentrations.
The first three methods were based on the zero-order range and involved modest mathematical manipulations. They are the induced dual-wavelength, Fourier self-deconvolution, and absorptivity factor spectrophotometric methods. Three other methods that are based on ratio spectra manipulation were developed: ratio difference, mean centering of the ratio spectra, and derivative ratio spectrum.
We determined the performance of the suggested methods for estimating DAP and SIL in their laboratory mixtures and their combined pharmaceutical dosage form. The linear ranges for DAP and SIL were 1-40 µg/ml and 2-60 µg/ml, respectively. The detection limits were in the 0.18-1.10 µg/ml range for DAP and in the 0.68-1.11 µg/ml range for SIL. The developed methods were validated as per the ICH guidelines for linearity, detection limit, quantitation limit, selectivity, precision, and accuracy. Normal probability, interval, and Tukey's simultaneous significant difference plots were utilized to confirm and better visualize the analysis of variance test results. Statistically, no significant difference was observed to exist between results obtained from the hereby developed and the previously reported methods.
盐酸达泊西汀（DAP）和枸橼酸西地那非（SIL）已被证明在治疗勃起功能障碍和早泄等共病方面具有临床疗效。由于这些化合物的光谱严重重叠，因此分析 DAP 和 SIL 的组合是一项挑战。已经证明，六种新开发的方法对于解决这种具有挑战性的重叠是有效的。它们还具有简单的优点，因为它们依赖于零阶光谱，只需要简单的数学处理。
我们提出了六种基于数学滤波技术和比值光谱操作的简单、精确和灵敏的分光光度法，以解决 DAP 和 SIL 在其原料药和复方制剂中的光谱，并估计相关的单个浓度。
前三种方法基于零阶范围，涉及适度的数学操作。它们是诱导双波长、傅里叶自解卷积和吸光度因子分光光度法。另外三种基于比值光谱操作的方法是：比值差、比值光谱的均值中心化和导数比值光谱。
我们确定了所建议的方法在实验室混合物及其复方制剂中估计 DAP 和 SIL 的性能。DAP 和 SIL 的线性范围分别为 1-40μg/ml 和 2-60μg/ml。DAP 的检测限在 0.18-1.10μg/ml 范围内，SIL 的检测限在 0.68-1.11μg/ml 范围内。所开发的方法符合 ICH 关于线性、检测限、定量限、选择性、精密度和准确度的指南进行了验证。正态概率、区间和 Tukey 同时显著差异图用于确认和更好地可视化方差分析测试结果。统计学上，没有观察到所开发的方法与以前报道的方法之间存在显著差异。
