液质联用分析测定硝基呫吨酮的方法改进研究

The improvement of analytical method for determination of nitroxanthone by LCMS

对国标方法中的硝基呫吨酮液质联用分析测定方法进行改进,以期提高方法的灵敏度和扩大方法的定量范围。采用液质联用仪、ESI源、MRM正离子扫描模式,流动相为乙腈∶1 mM/L乙酸铵水溶液=50∶50(体积比),流速为1.0 mL/min,对硝基呫吨酮进行定量分析。当硝基呫吨酮质量浓度为0.005~1 mg/L时,其线性相关系数(R^(2))为0.9996,分析方法的相对标准偏差为3.30%,平均回收率为86%~100%。经过分析条件改进,提高了方法的灵敏度,扩大了定量范围,节省了分析时间。改进后的方法适更适合于硝基呫吨酮的定量分析。

The improvement for the national standard of LCMS determination method of nitroxanthone was performed in order to improve the sensitivity and expand the quantitative range of the method.The quantitative analysis of nitroxanthone was carried out by using LCMS with ESI source,MRM positive scanning mode,and acetonitrile-water with 1 mM/L ammonium acetate(50∶50,by vol)at the flow rate of 1.0 mL/min.When the concentration of nitroxanthone was 0.005 to 1 mg/L,the linear correlation coefficient(R^(2))was 0.9996.The variation coefficient of the analytical method was 3.30%,and the mean recovery was 86%~100%.After the improvement of analytical conditions,the method has higher sensitivity,wider quantitative range,more time-saving,and is more suitable for the quantitative analysis of nitroxanthone.