Runja Chinnalalaiah, Kumar Pigili Ravi, Avanapu Srinivasa Rao
Department of Pharmaceutical Chemistry, Joginpally B.R. Pharmacy College, Moinabad, Hyderabad 500 075, Telangana, India
Aizant Drug Research Solutions, Hyderabad 500 014, Telangana, India.
J Chromatogr Sci. 2016 May-Jun;54(5):759-64. doi: 10.1093/chromsci/bmw004. Epub 2016 Feb 9.
A new simple, rapid stability indicating assay method has been developed and validated for the determination of emtricitabine, tenofovir disoproxil fumarate, elvitegravir and cobicistat using reverse-phase high-performance liquid chromatography in their pharmaceutical dosage form. The chromatographic separation was performed on an ODS column (250 × 4.6 mm, 5 µm) using mobile phase A (potassium dihydrogen orthophosphate, pH adjusted to 2.5) and mobile phase B (acetonitrile) in the ratio of 55:45% v/v at a flow rate of 1 mL/min. The analytes were detected at 250 nm. The method was found to be linear in the concentration range of 2-12 µg/mL for EMT, 3-18 µg/mL for TNDF, 1.5-9 µg/mL for ELV and COB, with the coefficient value (R(2)) of >0.9990. The accuracy was measured via recovery studies and found to be acceptable, and the percentage recoveries were found in the range of 99.93-100.08 ± 0.5%. Forced degradation studies were also conducted, and the drugs were subjected to various stress conditions such as acid hydrolysis, base hydrolysis, oxidative, photolytic and thermal degradation. The proposed method was successfully validated and applied for the quantitative estimation of these drugs in both bulk and tablet dosage forms.
已开发并验证了一种新的简单、快速的稳定性指示测定方法，用于采用反相高效液相色谱法测定其药物剂型中的恩曲他滨、替诺福韦酯富马酸盐、埃替格韦和考比司他。色谱分离在ODS柱（250×4.6 mm，5 µm）上进行，使用流动相A（磷酸二氢钾，pH值调至2.5）和流动相B（乙腈），比例为55:45% v/v，流速为1 mL/min。在250 nm处检测分析物。该方法在恩曲他滨（EMT）浓度范围为2 - 12 µg/mL、替诺福韦酯富马酸盐（TNDF）为3 - 18 µg/mL、埃替格韦（ELV）和考比司他（COB）为1.5 - 9 µg/mL时呈线性，系数值（R(2)）>0.9990。通过回收率研究测量准确度，发现其可接受，回收率百分比在99.93 - 100.08 ± 0.5%范围内。还进行了强制降解研究，使药物经受各种应力条件，如酸水解、碱水解、氧化降解、光解降解和热降解。所提出的方法成功得到验证，并应用于原料药和片剂剂型中这些药物的定量测定。
