目的 建立富马酸替诺福韦二吡呋酯中痕量遗传毒性杂质9-丙烯基腺嘌呤含量测定方法.方法 采用高效液相色谱-串联质谱(LC-MS/MS)技术,以C18柱分离,乙腈-10 mmol/L乙酸铵溶液(35:65,v/v)为流动相,流速为1.0 ml/min.用正离子扫描方式检测,多反应监测(MRM)模式扫描,检测离子通道为m/z:176.1/136.1.结果 9-丙烯基腺嘌呤浓度在0.49～24.50 ng/ml范围内与峰面积呈良好线性关系,相关系数为0.9999;定量限为0.49 ng/ml;平均加样回收率为99.18 ％,RSD为2.78 ％(n=9);对照品溶液连续进样6次,峰面积RSD为1.72 ％.结论 本方法专属性强、灵敏度高、准确度好,可用于富马酸替诺福韦二吡呋酯中9-丙烯基腺嘌呤的含量测定.%Objective To establish a method for the determination of 9-propenyladenine which is a trace genotoxic impurity in tenofovir disoproxil fumarate. Methods 9-Propenyladenine was separated and determined by LC-MS/ MS. It was separated on a C18 column with acetonitrile-10 mmol/L ammonium acetate solution (35:65,v/v) as the mobile phase. The flow rate was 1.0 ml/min. The detection was accomplished by tandem mass spectroscopy in the positive ion multiple reaction monitoring (MRM) mode with ion transitions of m/z 176.1/136.1. Results The standard curve was linear in the range of 0.49-24.50 ng/ml (r=0.9999) for 9-propenyladenine and the limit of quantification was 0.49 ng/ml. The average recovery was 99.18 ％ with RSD of 2.78 ％ (n=9). The RSD of precision(n=6)was 1.72 ％. Conclusion The method can be accurate, sensitive and specific, and can be used for the determination of trace genotoxic impurity 9-propenyladenine in tenofovir disoproxil fumarate.
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