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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 establish an ultra-fast liquid chromatography-mass spectrometry / mass spectrometry (UFLC-MS / MS) method for the determination of tegafur (FT) in tegafur. Methods: The samples were extracted with methanol-water (80:20) and separated on a Shim-pack XR-ODS column using methanol-water (80:20) as mobile phase at a flow rate of 0.40 mL · min- (ESI), negative ion detection by multi-reaction detection (MRM) mode, the injection volume of 10μL, for the quantitative analysis of the detection of ions m / z198.9 → 42.0 (FT) and m / z128.8 → 42.1 (5 -FU) to complete the FT quantitative analysis within 3 min. Results: The linear range was 5 ~ 3000ng.mL-1, the lowest detection limit was 5ng.mL-1. The spiked recoveries of three FT3 concentrations (550, 700, 1000 ng.mL-1) were 100.4%, 100.9% and 101.2%, respectively. Conclusion: The method has high sensitivity, fast analysis speed and simple operation, and can be used as FT quality control method in tegafur formulation.