LC-MS/MS测定头孢替唑钠中特戊酸含量

Determination of Pivalic Acid in Ceftezole by LC-MS/MS

目的:建立头孢替唑钠中特戊酸的含量测定方法。方法:采用液相色谱-串联质谱法(LC-MS/MS),色谱及质谱条件主要参数为:色谱柱为Gemini-NX C18(150 mm×4.6 mm,3μm);柱温30℃;流动相为1‰氨水(甲酸调pH至7.6)-乙腈(20:80);流速0.5 ml·min-1;采用电喷雾离子源(ESI),以多反应监测模式(MRM)进行负离子扫描用于定量分析离子反应为m/z101.1→m/z 57.1。结果:在该色谱条件下,特戊酸专属性好(分离度≥1.5)在0.2006~1.5044μg·ml-1浓度范围内线性关系良好(r=0.9995),回收率为平均回收率为96.2%(RSD=4.69%,n=9)。结论:该分析方法简便、快速,可用于头孢替唑钠中特戊酸含量测定。

Objective:To establish a method for the determination of pivalic acid in ceftezole.Methods:LC-MS/MS was used with a column of Gemini-NX C18(150 mmx4.6 mm,3μm)at the column temperature of 30℃.The mobile phases consisted of 1‰ammonia water adjusting pH to 7.6 with formic acid and acetonitril(20:80)at the flow rate of 0.5 ml·min-1.Multiple-reaction monitoring(MRM)mode was used with negative ion-switching electrospray ionization(ESI)source at m/z 101.1→m/z 57.1.Results:The method had good specificity(R≥1.5)and promising linearity ranging from 0.2006 to 1.5044μg·ml-1(r=0.9995).The average recovery was 96.2%(RSD=4.69%,n=9).Conclusion:A simple and fast method is developed and validated for the quantification of pivalic acid in ceftezole.