液相-质谱法测定吗啉甲基萘满酮原料药中主药含量

Content Determination of Main Component of 3,4-Dihyro-2-(4-morpholinylmethyl)-1(2H)-naphthalenone by LC-MS

目的:建立测定吗啉甲基萘满酮原料药中主药含量的方法。方法:采用液相-质谱法。色谱柱为Waters SunFire TMC18,流动相为甲醇-醋酸铵缓冲液(5mmo·lL-1)=70∶30,流速为0.2mL·min-1,柱温为20℃,进样量为10μL;质谱电离源为电喷雾电离源,采用正离子方式检测,扫描方式为多反应监测,用于定量的离子对为m/z245.8→m/z100.1,扫描时间为200ms。结果:吗啉甲基萘满酮检测浓度线性范围为100～300μg·mL-1(r=0.9997),平均回收率为99.83%,RSD为0.21%(n=9)。结论:本方法灵敏度高、专属性强、操作简便,适用于该原料药中主药的含量测定。

OBJECTIVE： To establish a method for the content determination of main component of 3,4-dihyro-2-（4-morpholinylmethyl）-1（2H）-naphthalenone （CY）.METHODS： LC-MS method was adopted.The determination was performed on Waters SunFireTM-C18 column with mobile phase consisted of methanol-ammonium acetate buffer （5 mmol·L-1） （70 ∶ 30） at flow rate of 0.2 mL·min-1.The column temperature was 20 ℃ and injection volume was 10 μL.Electrospray ionization source was applied and operated in the positive ion mode under multiple reaction monitoring mode.The ions for quantification were m/z 245.8→m/z 100.1 and scanning time was 200 ms.RESULTS： The linear range of CY was 100～300 μg·mL-1 （r=0.999 7） with an average recovery rate of 99.83%,RSD=0.21% （n=9）.CONCLUSIONS： The method is sensitive,specific and simple in operation,and it is suitable for the content determine of CY.