摘要
目的:建立超高效液相色谱-质谱联用(UPLC—MS/MS)检测一类新药 F351原料药中催化剂四丁基溴化铵残留量的方法。方法:色谱柱为 Waters Atlantis HILIC Silica(2.1 mm×100 mm,3μm),流动相:乙腈-0.1 mol·L^(-1)甲酸铵溶液(pH=3.5)95:5,流速0.2 mL·min^(-1)。经石油醚和水(1:1)提取出的四丁基溴化铵通过 UPLC—MS/MS 进行检测。结果:本法的线性范围为5～100 ng·mL^(-1)(r=0.9996);最低检测限为2.9×10^(-12)g;回收率为97.1%。结论:本法操作简便,结果准确,可用于新药 F351对催化剂四丁基溴化铵的质量控制。
Objective ：To establish an UPLC -MS/MS method for determination of Tetrabutyl ammonium bromide （TBAB） in F351. Method：A Waters Atlantis HILIC SILICA （2.1mm×100mm,3μm）column was used with acetonitrile -0.1mol·L^-1 ammonium formate （ pH = 3.5 ） （ 95 ： 5 ） as the mobile phase. The flow rate was 0.2 mL·min^-1. TBAB in F351 extracted by Petroleum ether - water（ 1 ： 1 ） was detected by UPLC - MS/MS. Result： The standard curve was linear over the range of 5-100ng· mL^-1 （r =0.9996） , with the detection limit of 2.9×10^-12 g;The average recovery was 97.2%. Conclusion：this mothod is simple, rapid and precise enough to control the remain of TBAB in F351.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2008年第3期443-446,共4页
Chinese Journal of Pharmaceutical Analysis
