加替沙星纯度标准物质研制

Development of a purity certified reference material of gatifloxacin

研制加替沙星纯度标准物质。采用质量平衡法和氢谱定量核磁法对加替沙星纯度标准物质候选物进行纯度定值,采用卡尔费休法和热重分析法准确测量了影响主成分纯度的水分含量,并考察了水分含量的稳定性。开展了加替沙星纯度定值、均匀性检验、稳定性考察以及不确定度评估。结果表明,加替沙星纯度标准物质的纯度值为93.1%,扩展不确定度为0.6%(k=2),水分含量为6.6%,特性量值均匀性良好,6个月稳定性可靠,被认定为国家二级标准物质,编号为GBW(E) 100476。研制的加替沙星纯度标准物质填补了国内空白,同时也为吸湿性较强的药物纯度标准物质研制过程中水分测定提供了参考与借鉴。

The certified reference material of gatifloxacin was developed.Two independent methods including mass balance and quantitative nuclear magnetic resonance were established and employed to measure the purity of gatifloxacin.In experiment,characterization of purity,homogeneity testing,stability study and uncertainty evaluation were carried out.Water content as the main influence factor on purity was accurately determined by Karl Fischer and thermal gravimetric analysis and stability of water in pure gatifloxacin substance was also investigated.The results demonstrate that the purity of gatifloxacin was assigned to be 93.1%with expanded uncertainty of 0.6%(k=2),water content was 6.6%,the homogeneity and stability for six months at storage condition were satisfied with the requests of a certified reference material,and the gatifloxacin CRM(certified reference material)was approved and numbered as GBW(E)100476.The gatifloxacin CRM was first developed in this study and the results could be a reference for water determination and stability maintenance during the development of certified reference materials of pure substance with strong hygroscopicity.