UFLC-MS/MS法测定氨茶碱制剂中的氨茶碱含量

Content Determination of Aminophylline in Aminophylline Preparation by UFLC-MS/MS

目的:建立测定氨茶碱制剂(片剂和注射液)中氨茶碱含量的方法。方法:采用超快速液相色谱串联质谱(UFLC-MS/MS)法。色谱柱为Shim-packXR-ODS,流动相为乙腈-0.4%甲酸水溶液(54:46),流速为0.40ml/min;通过电喷雾离子化、采用多反应检测方式进行正离子检测,用于定量分析的检测离子为m/z181.0→124.0。结果:在3min内可完成氨茶碱定量分析;氨茶碱检测质量浓度线性范围为0.25～100ng/ml(r=0.9998),最低定量限为0.25ng/ml;平均回收率为99.75%,日内、日间RSD均<2.84%。结论:本方法灵敏、准确、专属性好、定量限低且分析时间短,适用于氨茶碱制剂的含量测定。

OBJECTIVE：To establish the method for the content determination of aminophylline in Aminophylline preparations （tablet and injection）.METHODS：UFLC-MS/MS was adopted.The determination was performed on Shim-pack XR-ODS column with mobile phase consisted of acetonitrile-0.4% formic acid solution（54：46）at the flow rate of 0.40 ml/min;the detection was performed in multiple reaction monitoring mode（MRM）with positive electrospray ionization（ESI）,using the transitions of m/z 181.0→124.0 of aminophylline.RESULTS：Quantity analysis of aminophylline was completed within 3 min.Linear range of aminophylline were 0.25-100 ng/ml（r=0.999 8）with average recovery of 99.75%.The limit of quantification（LOQ）was 0.25 ng/ml,and intra-day and inter-day RSDs were lower than 2.84%.CONCLUSIONS：The method is sensitive,accurate and specific with low LOQ,and it costs short time.It is suitable for the content determination of Aminophylline preparations.