Kadioglu Yucel, Atila Alptug, Serdar Gultekin Mehmet, Alcan Alp Nurdan
Iran J Pharm Res. 2013 Fall;12(4):659-69.
The forced degradation study of lidocaine HCl was carried out according to the ICH guideline Q1A (R2). The degradation conditions were assessed to be hydrolysis, oxidation, photolysis and dry heat during 24 h, 48 h and 72 h and then the samples were investigated by GC-FID method and nuclear magnetic resonance (NMR) spectroscopy. According to these results, the degradation products were not observed in all reaction conditions during the 72 h period. Only spectral changes in the 1H and 13C-NMR spectrum were observed in hydrogen peroxide and acid degradation. As a result of this degradation, n-oxide was formed. After acid-induced degradation with HCl, the secondary amine salt was formed. Furthermore, trifluoroacetic acid (TFA) was used as the acidic media, and the decomposition products were observed. A simple and reliable gas chromatography method with flame ionization detection (GC-FID) was developed and validated for the determination of lidocaine HCl in pharmaceutical formulations in the form of a cream and injections. The GC-FID method can be used for a routine analysis of lidocaine HCl in pharmaceutical formulations and the proposed method, together with NMR spectroscopy, can be applied in stability studies.
盐酸利多卡因的强制降解研究按照国际人用药品注册技术协调会（ICH）指南Q1A（R2）进行。在24小时、48小时和72小时期间评估降解条件为水解、氧化、光解和干热，然后通过气相色谱 - 火焰离子化检测（GC - FID）法和核磁共振（NMR）光谱对样品进行研究。根据这些结果，在72小时期间的所有反应条件下均未观察到降解产物。仅在过氧化氢和酸降解过程中观察到1H和13C - NMR光谱的光谱变化。由于这种降解，形成了N - 氧化物。用盐酸进行酸诱导降解后，形成了仲胺盐。此外，使用三氟乙酸（TFA）作为酸性介质时，观察到了分解产物。开发并验证了一种简单可靠的带有火焰离子化检测的气相色谱法（GC - FID），用于测定乳膏和注射剂形式的药物制剂中的盐酸利多卡因。GC - FID法可用于药物制剂中盐酸利多卡因的常规分析，所提出的方法与NMR光谱一起可应用于稳定性研究。
