反相液相色谱法测定索磷布韦起始物料中的对映异构体
Determination of Enantiomers in Sofobuvir Starting Material by RP-HPLC
赵珊 1兰公剑 1郑礼康 1赵翠1
作者信息
- 1. 南京正大天晴制药有限公司,江苏南京 210046
- 折叠
摘要
目的:建立索磷布韦起始物料[(2R)-2-脱氧-2-氟-2-甲基-D-赤式戊糖酸γ-内酯3,5-二苯甲酸酯]对映异构体检测方法.方法:采用CHIRALCEL OJ-RH(4.6mm×150mm,5μm)为色谱柱;流动相为三氟乙酸-乙腈-水(0.25∶680∶320),等度洗脱;检测波长为230nm,流速为1.0mL/min.结果:专属性良好,对映异构体在限度浓度的20％～200％范围内线性关系良好,r=0.9999;回收率在97.7％～104.0％范围内,RSD小于10.0％(n=9);进样精密度RSD小于2.0％,中间精密度和重复性RSD值均小于10.0％;耐用性良好.结论:方法精密度好且准确度高,可用于索磷布韦的对映异构体检测.
Abstract
Objective:To establish a method for the determination of the enantiomers of Sophobuvir starting material[(2R)-2-deoxy-2-fluoro-2-methyl-D-carboxylic acid γ-Lactone 3,5-Dibenzoate]. Methods:Daicel CHIRALPAK OJ-RH (4.6 mm×150 mm,5 μm) was used as chromatographic column. trifluoroacetic acid-acetonitrile-water(0.25∶680∶320) as mobile phase,and elute equally. The detection wavelength was 230 nm and the flow rate was 1.0 mL/min. Results:The specificity was good,and the linear relationship between enantiomers was good in the limit concentration range of 20％～200％,r ≥ 0.9999. The recovery was in the range of 97.7％～104.0％,RSD was less than 10.0％ (n=9),and preci-sion and repeatability RSD are less than 10.0％,good durability. Conclusion:This method has good precision and high accuracy,and can be used for the determination of enantiomers of this product.
关键词
索磷布韦/对映异构体/高效液相色谱仪法(HPLC)Key words
Sophobuvir/enantiomer/high performance liquid chromatography (HPLC)引用本文复制引用
出版年
2024
NETL
NSTL
万方数据