Venkatesan S, Kannappan N, Mannemala Sai Sandeep
Department of Pharmacy, Annamalai University, Chidambaram, Tamil Nadu 608002, India.
Int Sch Res Notices. 2014 Oct 29;2014:849149. doi: 10.1155/2014/849149. eCollection 2014.
A simple, accurate, rapid, and stability-indicating RP-HPLC method for a combination of tenofovir disoproxil fumarate, emtricitabine, and rilpivirine has been developed and subsequently validated in commercial tablets. The proposed HPLC method utilizes Phenomenex Gemini C18 column (150 mm × 4.6 mm i.d., 5 µm) and mobile phase consisting of MeCN, potassium dihydrogen phosphate buffer (20 mM, pH 3.3), and triethylamine 58.72 : 41.23 : 0.05 (v/v) at a flow rate of 1.7 mL/min. Quantitation was achieved with UV detection at 270 nm. The method was validated in terms of accuracy, precision, linearity, limits of detection, limits of quantitation, and robustness. This optimized method has been successively applied to pharmaceutical formulation and no interference from the tablet excipients was found. TDF, EMT, and RPV and their combination drug product were subjected to acid, base, neutral hydrolysis, oxidation, dry heat, and photolytic stress conditions and the stressed samples were analyzed by the proposed method. As the proposed LC method could effectively separate the drugs from its degradation products, it can be employed as stability-indicating method for the determination of instability of these drugs in bulk and commercial tablets.
已开发出一种用于测定富马酸替诺福韦二吡呋酯、恩曲他滨和利匹韦林组合的简单、准确、快速且具有稳定性指示功能的反相高效液相色谱（RP-HPLC）方法，并随后在市售片剂中进行了验证。所提出的HPLC方法使用菲罗门Gemini C18柱（150 mm×4.6 mm内径，5 µm），流动相由乙腈、磷酸二氢钾缓冲液（20 mM，pH 3.3）和三乙胺按58.72∶41.23∶0.05（v/v）组成，流速为1.7 mL/min。通过在270 nm处进行紫外检测实现定量。该方法在准确性、精密度、线性、检测限、定量限和稳健性方面进行了验证。这种优化后的方法已成功应用于药物制剂，未发现片剂辅料产生干扰。对替诺福韦（TDF）、恩曲他滨（EMT）、利匹韦林（RPV）及其组合药物产品进行了酸、碱、中性水解、氧化、干热和光解应激条件处理，并采用所提出的方法对应激样品进行了分析。由于所提出的液相色谱方法能够有效地将药物与其降解产物分离，因此可作为一种稳定性指示方法，用于测定这些药物原料药和市售片剂中的不稳定性。
