HPLC-MS/MS法测定磷酸特地唑胺中基因毒性杂质含量
Determination of Genotoxic Impurities Content in Tedizolid Phosphate by HPLC-MS/MS
黎龙香 1郑康乐 1王学明1
作者信息
- 1. 江西科睿药业有限公司, 江西 赣州 341000
- 折叠
摘要
目的:建立高效液相色谱-串联质谱联用(HPLC-MS/MS)方法测定磷酸特地唑胺中基因毒性的含量.方法:采用Waters Acquity BEH C18(2.1 mm×100 mm,1.7 μm)色谱柱,以20 mmol醋酸铵溶液为流动相A,以乙腈为流动相B,梯度洗脱,采用电喷雾电离源(ESI),正离子模式下选择离子监测(SIM)采集,对m/z 389.1、m/z 310.0 离子进行选择性监测.结果:基因毒性杂质TDZA010、TDZA046 在限度的 30%～150%范围内线性关系良好;检测限均为 1 ng·mL-1,定量限均为 3 ng·mL-1;回收率在 89.8%～105.3%之间,RSD(n=12)分别为 5.3%、4.6%;重复性(n=6)RSD分别为 0.4%、3.3%.结论:本方法操作简便、专属性好、灵敏度高,可用于磷酸特地唑胺中基因毒性杂质TDZA010、TDZA046 含量的检测.
Abstract
Objective:To establish an HPLC-MS/MS analytical method for the determination of genotoxic impurities in tedizolid phosphate.Methods:Chromatographic separation was performed on an Waters Acquity BEH C18(2.1 mm×100 mm,1.7 μm)column using the mobile phase consisting of 20 mmol ammonium acetate(mobile phase A)and acetonitrile(mobile phase B)by gradient elution.The electrospray was operated in an ESI under posive ionization scanning mode with SIM.Selective ion monitors were set at m/z 389.1 for TDZA010,m/z 310.0 for TDZA046.Results:The correlation curves of genotoxic impurities TDZA010,TDZA046 were in good linearity in the range of 30%～150%limit concentration.The detection limits were 1 ng·mL-1 and the quantitation limits were 3 ng·mL-1.The recoveries were between 89.8%to 105.3%and RSD(n=12)were 5.3%,4.6%.The repeatabilities RSD were 0.4%,3.3%.Conclusion:This method is simple,slective,sensitive,and quite suitable for the determination of genotoxic impurities TDZA010,TDZA046 in tedizolid phosphate.
关键词
磷酸特地唑胺/高效液相色谱-串联质谱/基因毒性杂质/TDZA010/TDZA046/含量Key words
tedizolid phosphate/HPLC-MS/MS/genotoxic impurities/TDZA010/TDZA046/content引用本文复制引用
基金项目
赣鄱俊才支持计划-主要学科学术和技术带头人培养项目(20232BCJ22042)
出版年
2024
NETL
NSTL
万方数据