Warner Anne, Piraner Irina, Weimer Heather, White Kevin
Lilly Research Laboratories, Eli Lilly and Company, Indianapolis, IN 46285, United States.
Lilly Research Laboratories, Eli Lilly and Company, Indianapolis, IN 46285, United States.
J Pharm Biomed Anal. 2015 Feb;105:46-54. doi: 10.1016/j.jpba.2014.11.032. Epub 2014 Nov 24.
Stability-indicating reversed phase HPLC methods have been developed and validated for the determination of 13 potential process and degradation impurities in pemetrexed disodium drug substance (DS) and pemetrexed for injection drug product (DP). This paper describes the development of HPLC-UV impurity methods for drug substance and drug product. Relative response factors (RRF) have been determined using HPLC-UV in tandem with CAD or by NMR detection. Conditions for the generation of system suitability solutions are described and assure adequate chromatographic resolution and peak identification without the need for impurity reference standards. The methods were fully validated and demonstrated to have acceptable specificity, linearity, accuracy, repeatability, intermediate precision, detection/quantitation limit, and robustness.
已开发并验证了稳定性指示反相高效液相色谱法,用于测定培美曲塞二钠原料药(DS)和注射用培美曲塞制剂(DP)中13种潜在的工艺杂质和降解杂质。本文描述了原料药和制剂的高效液相色谱-紫外杂质检测方法的开发过程。相对响应因子(RRF)已通过高效液相色谱-紫外联用蒸发光散射检测器(CAD)或核磁共振(NMR)检测来确定。文中描述了系统适用性溶液的配制条件,确保了无需杂质对照品即可获得足够的色谱分离度和峰识别能力。这些方法经过了全面验证,证明具有可接受的专属性、线性、准确度、重复性、中间精密度、检测/定量限和稳健性。