HPLC法测定5-氟-1H-吲哚-2,3-二酮中的有关物质

Determination of Related Substances in 5-Fluoro-1H-indole-2,3-dione by HPLC

采用高效液相色谱法建立了5-氟-1H-吲哚-2,3-二酮中有关物质的检测方法。采用YMC-Pack ODS-A(250mm×4.6mm,5μm)色谱柱,以含0.04%辛烷磺酸钠的0.013mol·L^(-1)磷酸氢二钾溶液(用磷酸调节pH=7.1)为流动相A,乙腈为流动相B,梯度洗脱,流速1.2 mL·min^(-1),柱温30℃,检测波长244nm。样品的主峰与相邻杂质的分离良好,在质量浓度0.5~30μg·mL^(-1)范围内线性关系良好,相关系数均大于0.999;定量限为0.53~2.1ng,检测限为0.16~0.61ng,溶液稳定性良好。本方法的精密度好、准确度高,可用于5-氟-1H-吲哚-2,3-二酮中有关物质的检测。

A method for the determination of related substances in the 5-fluoro-1 H-indole-2,3-dione by HPLC was established.YMCPack ODS-A(250 mm×4.6 mm,5μm)was used as column,0.013 mol/L dipotassium hydrogen phosphate solution contained 0.04%sodium octane sulfonate(adjusted pH=7.1 with phosphoric acid)was mobile phase A,acetonitrile was mobile phase B in a gradient elution,the flow rate was 1.2 mL/min,column temperature was 30℃.The main substance and its impurities could be well separated.A good linear was obtained in the ranges of 0.5~30μg/mL with the correlation coefficients were all greater than 0.999.The limit of quantification was 0.53~2.1 ng,the limit of detection was 0.16~0.61 ng,and the solution stability was good.The method had good precision and high accuracy,and could be used for the detection of related substances.