Department of Pharmaceutical Analysis, National Institute of Pharmaceutical Education and Research, Sector 67, SAS Nagar 160 062, Punjab, India.
J Pharm Biomed Anal. 2011 Nov 1;56(3):538-45. doi: 10.1016/j.jpba.2011.06.012. Epub 2011 Jun 23.
Lornoxicam was subjected to forced degradation studies under hydrolytic (acidic, basic and neutral), oxidative, photolytic and thermal stress conditions, as defined under ICH guideline Q1A (R2). The drug degraded significantly in hydrolytic, oxidative and photoneutral conditions, leading to the formation of eight degradation products in total. It was stable on exposure to light and dry heat in the solid state. The stressed samples in which degradation was observed were mixed together and used to develop a stability-indicating HPLC method wherein degradation products were separated from the drug and also from each other. To characterize the degradation products, a complete mass fragmentation pathway of the drug was first established with the help of MS/TOF, MS(n) and H/D exchange mass studies. The same was followed by LC-MS/TOF and on-line H/D exchange experiments on the degradation products. The degradation pathway of the drug was outlined, justified by the mechanisms of formation of the degradation products.
氯诺昔康在酸、碱和中性水解条件，氧化、光解和热应力条件下，按照 ICH 指南 Q1A（R2）进行强制降解研究。药物在水解、氧化和光稳定条件下显著降解，导致总共形成了 8 个降解产物。它在固态暴露于光和干热下稳定。在观察到降解的应激样品中，将它们混合在一起，用于开发一种稳定性指示 HPLC 方法，其中降解产物与药物本身以及彼此分离。为了表征降解产物，首先借助 MS/TOF、MS(n) 和 H/D 交换质量研究，建立了药物的完整质谱裂解途径。随后，对降解产物进行 LC-MS/TOF 和在线 H/D 交换实验。通过降解产物的形成机制，阐述了药物的降解途径。
