HPLC法测定达克替尼含量及有关物质

Determination of dacomitinib and related substances by HPLC

目的:建立测定达克替尼含量及有关物质的高效液相色谱法(high performance liquid chromatography,HPLC),以控制达克替尼的质量标准。方法:采用Agilent Eclipse XDB×C18柱(250 mm×4.6 mm,5μm);流动相为乙酸铵水溶液(30 mmol·L-1)-甲醇(20∶80);流速:1.0 mL·min-1;柱温为25℃;检测波长为252 nm;进样体积为20μL。结果:本方法能较好地分离达克替尼和杂质峰,达克替尼浓度在48.40~242.0μg·mL-1浓度范围内,线性关系良好(r=0.999 9);精密度、稳定性、重复性的RSD均<1%;回收率为99.79%,RSD=0.39%(n=9)。结论:该操作方法简便、快捷、重复性好,可用于达克替尼的含量测定。

Objective: To establish a high performance liquid chromatography(HPLC) method for the determination of dacomitinib and related substances for the purpose of quality control of dacomitinib. Methods: The determination was performed on the Agilent Eclipse XDB×C18 column(250 mm×4.6 mm,5 μm) with the mobile phase consisted of ammonium acetate solution(30 mmol·L-1)-methanol(20∶80) at a flow rate of 1.0 mL·min-1. The column temperature was set at 25 ℃, the detection wave length was set at 252 nm, and the injection size was at 20 μL. Results: The calibration curve of dacomitinib was linear in the range of 48.40~242.0 μg·mL-1(r=0.999 9) with RSDs of precision, stability, and reproducibility lower than 1% and the average recovery of dacomitinib of 99.79%,RSD=0.39%(n=9). Conclusion: This method is simple, rapid and reproducible, and can be applied for the content determination of dacomitinib and related substances.