反相高效液相色谱法测定雷替曲塞的含量和有关物质

RP-HPLC Determination of Content and Related Substances of Raltitrexed

目的:建立测定雷替曲塞含量及其有关物质的反相高效液相色谱法。方法:采用 Diamonsil C_(18)(150mm×4.6mm,5μm)色谱柱,以缓冲液(0.03mol·L^(-1)磷酸氢二钾,0.03 mol·L^(-1)三乙胺,磷酸调 pH 为7.2)-甲醇(69:31)为流动相,检测波长为342 nm,柱温35℃,流速0.9 mL·min^(-1),按峰面积外标法计算。结果:雷替曲塞在1.0～100.0μg·mL^(-1)范围内呈良好线性,方法回收率为99.94%～102.16%(n=5),日内、日间 RSD<2.22%(n=5),雷替曲塞含量在99.38%～100.45%之间,有关物质<0.58%。结论:本方法简便,快速,结果准确,可靠,重现性好,所测该药含量及有关物质均在合格范围之内。

Objective ：To establish HPLC method for the determination of content and related substance of rahitrexed. Method：A Diamonsil C is （150mm×4.6mm,5μm）column was used. The mobile phase was composed of buffer（0. 03 mol· L^- 1 K2 HPO4 _ 0. 03 mol· L^- 1 （ CH3 CH2 ） 3 N, pH = 7. 2 ） - CH3 OH （ 69 ： 31 ）. Detection wavelength was 342 nm. Flow rate was 0. 9 mL· min^- 1. The temperature of the column was 35℃. Results ：The linearity of the calibration curve was well correlated（ r = 0. 9997）within the range of 1.0 -100. 0μg·mL^-1. The recovery was 99.94% - 102. 16%. The within and between day RSD were less than 2. 22%. The content of related substances were less than 0.58%. Conclusion ： The method is simple, rapid, results are accurate and good reproducible. The content and related substance of rahitrexed are both within acceptable range.