Department of Pharmaceutical Analysis, GITAM School of Pharmacy, GITAM (Deemed to be University), Gandhi nagar, Rushikonda, Visakhapatnam, Andhra Pradesh 530045, India.
J Chromatogr Sci. 2024 Oct 1;62(8):719-731. doi: 10.1093/chromsci/bmad067.
A simultaneous ultra-performance liquid chromatography photodiode array detection method was developed and validated for Elvitegravir, Tenofovir and Emtricitabine and Cobicistat drugs in tablet dosage forms. Effective liquid chromatographic quantification was achieved using a Luna C18 (100 × 2.6 mm, 1.6 μ) column with an acetonitrile: 0.1% v/v trifluoro acetic acid (80:20% v/v) mobile phase and a photo diode array detector at 260 nm for a shorter run time of 3 min. The respective retention times for Elvitegravir, Tenofovir, Emtricitabine and Cobicistat were 0.311, 0.792, 1.379 and 2.045 min. The range of linearity was 37.50-225.00, 2.50-15.00, 50.00-300.00 and 37.50-225.00 μg/mL for Elvitegravir, Tenofovir, Emtricitabine and Cobicistat, respectively. A mass spectrometer was employed for quantitative analysis using electron spray ionization multiple reaction monitoring in positive mode. The developed method was validated for different parameters to meet the acceptance criteria as per ICH Q2 (R1) guidelines. Using UPLC-ESI-MS, 12 degradants were identified and their mechanisms were studied.
建立并验证了一种用于片剂制剂中艾维雷格、替诺福韦和恩曲他滨和考比司他药物的同时超高效液相色谱-光电二极管阵列检测法。采用 Luna C18（100×2.6mm，1.6μm）柱，以乙腈：0.1%v/v 三氟乙酸（80:20%v/v）为流动相，在 260nm 下用光电二极管阵列检测器，可在更短的 3 分钟内实现有效的液相色谱定量。艾维雷格、替诺福韦、恩曲他滨和考比司他的保留时间分别为 0.311、0.792、1.379 和 2.045 分钟。艾维雷格、替诺福韦、恩曲他滨和考比司他的线性范围分别为 37.50-225.00、2.50-15.00、50.00-300.00 和 37.50-225.00μg/mL。采用电喷雾电离多反应监测正模式的质谱仪进行定量分析。该方法经过不同参数的验证，符合 ICH Q2（R1）指南的验收标准。使用 UPLC-ESI-MS，鉴定了 12 种降解产物，并研究了它们的降解机制。
