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目的:建立液相色谱-质谱联用方法测定氟胞嘧啶中痕量基因毒性杂质N,N-二甲基苯胺的含量。方法:采用C_(18)(2.1 mm×100 mm,1.8μm)色谱柱,以水(含0.1%甲酸)-甲醇(含0.1%甲酸)(95∶5)为流动相,流速0.2 m L·min~(-1),电喷雾离子化(ESI),正离子模式下MRM采集。结果:N,N-二甲基苯胺质量浓度在0.4~10 ng·m L~(-1)范围内,与峰面积线性关系良好(r=0.999 5);检测限为0.1 ng·m L~(-1),定量限为0.4 ng·m L~(-1);平均回收率(n=9)为101.3%。3批样品中N,N-二甲基苯胺的含量均小于0.02μg·g~(-1)。结论:本方法可用于氟胞嘧啶中痕量基因毒性杂质N,N-二甲基苯胺含量的检测。
Objective: To establish a liquid chromatography-mass spectrometry method for the determination of trace genotoxic impurities in flucytosine N, N-dimethylaniline. Methods: The mobile phase consisted of C18 (2.1 mm × 100 mm, 1.8 μm) column with water (containing 0.1% formic acid) -methanol (containing 0.1% formic acid) min ~ (-1), electrospray ionization (ESI), positive ion mode MRM acquisition. Results: The concentration of N, N-dimethylaniline was in the range of 0.4 ~ 10 ng · m L -1 with a good linear relationship with the peak area (r = 0.999 5). The detection limit was 0.1 ng · m L ~ (-1). The limit of quantification was 0.4 ng · m L -1. The average recovery (n = 9) was 101.3%. The contents of N, N-dimethylaniline in three batches of samples were less than 0.02 μg · g -1. Conclusion: This method can be used for the detection of trace genotoxic impurities N, N-dimethylaniline in flucytosine.