Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh 11451, Saudi Arabia.
Molecules. 2023 Mar 20;28(6):2808. doi: 10.3390/molecules28062808.
This study describes the development of a one-step microwell spectrofluorimetric assay (MW-SFA) with high sensitivity and throughput for the determination of four statins in their pharmaceutical and formulations (tablets). These statins were pitavastatin (PIT), fluvastatin (FLU), rosuvastatin (ROS) and atorvastatin (ATO). The MW-SFA involves the measurement of the native fluorescence of the statin aqueous solutions. The assay was conducted in white opaque 96-microwell plates, and the fluorescence intensities of the solutions were measured by using a fluorescence microplate reader. The optimum conditions of the assay were established; under which, linear relationships with good correlation coefficients (0.9991-0.9996) were found between the fluorescence intensity and the concentration of the statin drug in a range of 0.2-200 µg mL with limits of detection in a range of 0.1-4.1 µg mL. The proposed MW-SFA showed high precision, as the values of the relative standard deviations did not exceed 2.5%. The accuracy of the assay was proven by recovery studies, as the recovery values were 99.5-101.4% (±1.4-2.1%). The assay was applied to the determination of the investigated statins in their tablets. The results were statistically compared with those obtained by a reference method and the results proved to have comparable accuracy and precision of both methods, as evidenced by the t- and F-tests, respectively. The green and eco-friendly feature of the proposed assay was assessed by four different metric tools, and all the results proved that the assay meets the requirements of green and eco-friendly analytical approaches. In addition, ever-increasing miniaturization as handling of large numbers of micro-volume samples simultaneously in the proposed assay gave it a high-throughput feature. Therefore, the assay is a valuable tool for the rapid routine application in the pharmaceutical quality control units for the determination of statins.
本研究描述了一种一步微槽荧光分光光度法（MW-SFA）的开发，该方法具有高灵敏度和高通量，可用于测定药物制剂（片剂）中的四种他汀类药物。这些他汀类药物分别是匹伐他汀（PIT）、氟伐他汀（FLU）、罗苏伐他汀（ROS）和阿托伐他汀（ATO）。MW-SFA 涉及他汀类药物水溶液的固有荧光测量。该测定在白色不透明的 96 微孔板中进行，通过荧光微孔板读数器测量溶液的荧光强度。建立了测定的最佳条件；在此条件下，在 0.2-200 µg mL 的范围内，他汀类药物浓度与荧光强度之间存在良好相关性的线性关系，相关系数为 0.9991-0.9996，检测限在 0.1-4.1 µg mL 范围内。所提出的 MW-SFA 显示出高精确度，因为相对标准偏差的值不超过 2.5%。通过回收率研究证明了测定的准确性，因为回收率为 99.5-101.4%（±1.4-2.1%）。该测定法用于测定片剂中所研究的他汀类药物。结果与参考方法获得的结果进行了统计学比较，结果表明两种方法的准确性和精密度相当，分别通过 t 和 F 检验得到证明。通过四种不同的度量工具评估了所提出的测定法的绿色和环保特性，所有结果均证明该测定法符合绿色和环保分析方法的要求。此外，所提出的测定法具有不断增加的微型化特性，可以同时处理大量微体积样品，因此具有高通量特性。因此，该测定法是药物质量控制单位快速常规应用于测定他汀类药物的有价值的工具。
