Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy (Girls), Al-Azhar University, Cairo 11754, Egypt.
J Chromatogr Sci. 2021 Oct 29;59(10):909-922. doi: 10.1093/chromsci/bmaa143.
In this study, a green stability indicating chromatographic methods were developed and validated for the quantitative determination of tenofovir alafenamide in the presence of its degradation products in bulk powder as well as in dosage forms. The first method was micellar UPLC in which separation was achieved on kinetex ® 1.7 μm HILIC 100A, LC column using an ecofriendly micellar mobile phase consisting (0.05 M sodium dodecyl sulphate and 0.05 M sodium dihydrogen phosphate, (pH 5.5) and 10% 1-propanol (70:30) at a flow rate of 1 mL min-1 with a UV detection at 210 nm. The second method depended on HPTLC method performed on HPTLC plates pre-coated with silica gel 60 F254 using a mobile phase consisting of n-butanol-acetic acid (7:3, v/v) and detection at 260 nm. Tenofovir alafenamide was subjected to stress conditions including alkaline and acidic degradation. Beer' law was obeyed over the concentration range of 1-18 μg mL-1 and 0.1-4 μg/spot for micellar UPLC and HPTLC methods, respectively. Both methods are successfully applied to the analysis of the drug in its tablets and validated according to ICH guidelines. In addition, their greenness was assessed using three different tools indicating their least hazardous effect on the environment.
在这项研究中，开发并验证了一种绿色稳定的色谱方法，用于定量测定大量粉末中泰诺福韦艾拉酚胺及其降解产物，以及制剂中的泰诺福韦艾拉酚胺。第一种方法是胶束 UPLC，分离在 kinetex ® 1.7μm HILIC 100A，LC 柱上进行，采用环保型胶束流动相，由 0.05 M 十二烷基硫酸钠和 0.05 M 磷酸二氢钠（pH 5.5）和 10% 1-丙醇（70:30）组成，流速为 1mL/min，在 210nm 处进行紫外检测。第二种方法依赖于 HPTLC 法，在预先涂有硅胶 60 F254 的 HPTLC 板上进行，流动相由正丁醇-乙酸（7:3，v/v）组成，在 260nm 处检测。泰诺福韦艾拉酚胺在碱性和酸性降解条件下进行了应力试验。胶束 UPLC 和 HPTLC 方法的浓度范围分别为 1-18μg/mL 和 0.1-4μg/斑点，均服从比尔定律。两种方法均成功应用于片剂中药物的分析，并根据 ICH 指南进行了验证。此外，使用三种不同的工具评估了它们的绿色性，表明它们对环境的危害最小。
