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 (4.6 mm×150 mm,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230 nm,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。
Objective:To establish a method for the determination of the enantiomers of Sophobuvir starting material[(2R)-2-deoxy-2-fluoro-2-methyl-D-carboxylic acidγ-Lactone 3,5-Dibenzoate].Methods:Daicel CHIRALPAK OJ-RH(4.6 mm×150 mm,5μm)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.
作者
赵珊
兰公剑
郑礼康
赵翠
ZHAO Shan;LAN Gong-jian;ZHENG Li-kang;ZHAO Cui(Nanjing Chia Tai Tianqing Pharmaceutical Co.Ltd.,Nanjing 210046,China)
出处
《安徽化工》
CAS
2024年第4期154-156,160,共4页
Anhui Chemical Industry
