Analytical Chemistry Division, D215, Discovery Laboratory, Indian Institute of Chemical Technology, Tarnaka, Hyderabad 500 607, India.
Analytical Chemistry Division, D215, Discovery Laboratory, Indian Institute of Chemical Technology, Tarnaka, Hyderabad 500 607, India.
J Pharm Biomed Anal. 2014 Feb;89:28-33. doi: 10.1016/j.jpba.2013.10.007. Epub 2013 Oct 29.
Darunavir, an anti-HIV drug was subjected to forced degradation under acid, base, thermal and neutral hydrolysis, oxidation and photolysis as prescribed by ICH guidelines. Four major degradation products were formed under acid and base hydrolysis, while stable under neutral and thermal hydrolysis, oxidative and photolysis. The drug and its degradation products were separated on Hiber, LiChrospher® 60, RP-select B, C8 column (250mm×4.6mm i.d., 5μm) using 10mM ammonium acetate: acetonitrile (52:48, v/v) as mobile phase in an isocratic elution mode by LC. The degradation products were characterized by LC-MS/MS and fragmentation pathways were proposed. The proposed structures of degradation products were confirmed by HRMS and the LC method was validated with respect to specificity, linearity, accuracy, recovery, LOD and LOQ.
达芦那韦，一种抗 HIV 药物，根据 ICH 指南的规定，在酸、碱、热和中性水解、氧化和光解条件下进行强制降解。在酸和碱水解条件下形成了四个主要的降解产物，而在中性和热水解、氧化和光解条件下则稳定。药物及其降解产物在 Hiber、LiChrospher® 60、RP-select B、C8 柱（250mm×4.6mm id，5μm）上分离，使用 10mM 乙酸铵：乙腈（52:48，v/v）作为流动相，通过 LC 以等度洗脱模式洗脱。通过 LC-MS/MS 对降解产物进行了表征，并提出了碎片途径。通过 HRMS 确认了降解产物的建议结构，并对 LC 方法进行了专属性、线性、准确性、回收率、LOD 和 LOQ 的验证。
