UFLC-MS/MS法测定替加氟制剂中替加氟含量

UFLC-MS/MS determination of tegafur in tegafur preparation

目的:建立超快速液相色谱-质谱/质谱联用法(UFLC-MS/MS)测定替加氟制剂中替加氟(FT)的含量。方法:样品以甲醇-水(80:20)提取,采用Shim-pack XR-ODS柱分离,以甲醇-水(80:20)为流动相,流速为0.40mL.min-1,通过电喷雾离子化(ESI),采用多反应检测(MRM)方式进行负离子检测,进样量10μL,用于定量分析的检测离子为m/z198.9→42.0(FT)和m/z128.8→42.1(5-FU),在3min内完成FT定量分析。结果:线性范围为5～3000ng.mL-1,最低检测限为5ng.mL-1。FT3个浓度(550,700,1000ng.mL-1)的加标回收率分别为100.4%,100.9%,101.2%。结论:本方法灵敏度高,分析速度快,操作简单,可作为替加氟制剂中FT质量控制方法。

Objective：To develop an UFLC-MS/MS method for determination of tegafur in tegafur preparation.Method：The samples was extracted with methanol-water （80∶20,v/v）.The UFLC separation was performed on an Shim-pack XR-ODS column.The mobile phase consisted of methanol-water （80∶20,v/v） at a flow rate of 0.40 mL/min-1.ESI＋ was performed in multiple reaction monitoring mode（MRM）,using the transitions of m/z 198.9→42.0（tegafur） and m/z 128.8→42.1（5-fluorouracil）.Results：The method was linear in the concentration range of 5-3000 ng/mL-1.The lower limit of quantification （LLOQ） was 5 ng/mL-1.The recoveries at the addition of three levels （550,700,1000 ng/mL-1） were 100.4%,100.9% and 101.2%.Conclusion：The method has good repeatability,high sensitivity and more convenient,and can be successfully applied for the determination of tegafur in tegafur preparation.