Annapurna M Mathrusri, Mohapatro Chitaranjan, Narendra A
Department of Pharmaceutical Analysis & Quality Assurance, GITAM Institute of Pharmacy, GITAM University, Visakhapatnam 530045, India.
Department of Pharmaceutical Analysis & Quality Assurance, Roland Institute of Pharmaceutical Sciences, Berhampur, Orissa 760010, India.
J Pharm Anal. 2012 Aug;2(4):298-305. doi: 10.1016/j.jpha.2012.01.010. Epub 2012 Feb 3.
A stability-indicating high-performance liquid chromatographic method was developed and validated for the determination of Letrozole in tablet dosage forms. Reversed-phase chromatography was performed on Shimadzu Model LC-Class-Vp with Lichrocart/Lichrosphere 100 C-18 (250 mm×4.6 mm, 5 μm particle size) column with methanol: tetra butyl ammonium hydrogen sulfate (80:20V/V) as mobile phase at a flow rate of 1 mL/min with UV detection at 240 nm. Linearity was observed in the concentration range of 0.5-150 μg/mL (=0.9998) with regression equation =102582+43185. The limit of quantitation (LOQ) and limit of detection (LOD) were found to be 0.043 and 0.012 μg/mL respectively. The forced degradation studies were performed by using HCl, NaOH, HO, thermal and UV radiation. Letrozole is more sensitive towards alkaline conditions and very much resistant towards acidic, oxidative and photolytic degradations. The method was validated as per ICH guidelines. The RSD for intra-day (0.78-0.97) and inter-day (0.86-0.96) precision were found to be lesser than 1%. The percentage recovery was in good agreement with the labeled amount in the pharmaceutical formulations and the method is simple, specific, precise and accurate for the determination of Letrozole in pharmaceutical formulations.
建立了一种用于测定片剂剂型中来曲唑的稳定性指示高效液相色谱法并进行了验证。采用岛津LC-Class-Vp型号的仪器，使用Lichrocart/Lichrosphere 100 C-18（250mm×4.6mm，粒径5μm）色谱柱进行反相色谱分析，以甲醇：硫酸氢四丁铵（80:20V/V）为流动相，流速为1mL/min，在240nm波长处进行紫外检测。在0.5 - 150μg/mL的浓度范围内观察到线性关系（=0.9998），回归方程为=102582 + 43185。定量限（LOQ）和检测限（LOD）分别为0.043和0.012μg/mL。通过使用盐酸、氢氧化钠、过氧化氢、热和紫外辐射进行强制降解研究。来曲唑对碱性条件更敏感，对酸性、氧化和光解降解具有很强的抗性。该方法按照国际协调会议（ICH）指南进行了验证。日内精密度（0.78 - 0.97）和日间精密度（0.86 - 0.96）的相对标准偏差（RSD）均小于1%。回收率百分比与药物制剂中的标示量吻合良好，该方法对于药物制剂中来曲唑的测定简单、特异、精密且准确。
