液相色谱串联质谱用于原料药甲氧苄啶含量测定

Determination of Pharmaceutical Raw Materials of Trimethoprim by LC-MS/MS

目的建立甲氧苄啶原料药的液相色谱串联质谱(LC-MS/MS)检测方法。方法样品经50%的甲醇溶解后进行液质联用分析。色谱柱为C18柱,流动相为甲醇:水(50∶50),流速为0.2mL/min;质谱采用多重反应监测,正离子模式,离子对m/z(291.1→230.1)。结果甲氧苄啶的线性范围为60～252ng/mL,平均含量为93.64%,平均回收率为99.42%。结论利用液相色谱串联质谱技术测定原料药中甲氧苄啶的方法具有高选择性、高灵敏度等特点,具有一定实用性。

Objective This paper explored Establishing a method for determination of pharmaceutical raw materials of trimethoprim by LC-MS/MS.Method Sample dissoluted by 50% methanol was analyzed by LC-MS/MS.Chromatographic column was C18,and mobile phase was methanol： water（50：50）,flow rate was 0.2 mL/min.Multiple reaction monitoring technique（MRM） was adopted.Positive scan mode was used for Pharmaceutical raw materials of trimethoprim（TMP）,and quantitative ion pairs was m/z291.1 m/z230.1.Result For pharmaceutical raw materials of trimethoprim,linear range was 60~252 ng/mL,and average content was 93.64% and the average recovery was 99.42%.Conclusion This was a highly selective,highly sensitive,and rapid detecting method for pharmaceutical raw materials of trimethoprim.It could be applied to detect pharmaceutical raw materials of trimethoprim effectively.