UFLC-MS/MS法测定替加氟制剂中替加氟含量___

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0.40 mL•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10 μL，用于定量分析的检测离子为m/z 198.9→42.0(FT)和m/z 128.8→42.1(5-FU)，在3 min内完成FT定量分析。结果：线性范围为5~3000 ng•mL-1，最低检测限为5 ng•mL-1。FT 3个浓度（550，700，1000 ng•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.

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