HPLC法测定1-氟萘中工艺杂质和遗传毒性杂质含量

Determination of process-related impurities and genotoxic impurities in 1-fluoronaphthalene by HPLC

建立了1-氟萘中的2种工艺杂质和1种遗传毒性杂质含量检测的HPLC方法。采用Phenomenex Gemini色谱柱(C18250×4.6mm,5µm);流动相为10mM碳酸氢钠+6mM三乙胺∶乙腈=55∶45,等度洗脱,采集时间为主峰的2倍保留时间;柱温为40℃;检测波长为220nm;流速为1.0mL/min;进样量为20μL。采用加校正因子的主成分自身对照法对各杂质进行计算,各杂质分离度良好,定量限为0.005~0.008μg/ml,线性关系良好,精密度和高中低三浓度准确度符合要求。实验结果表明该方法专属性强、灵敏度高、操作简便、重复性好、结果准确可靠,可用于1-氟萘中杂质控制。

To establish an HPLC method for the detection of two known impurities and one genotoxic impurities contents in 1-fluoronaphthalene.The chromatographic column was Phenomenex Gemini C18250×4.6 mm,5μm;the mobile phase was 10 mM sodium bicarbonate+6 mM triethylamine:acetonitrile=55:45,isometric elution,and the collection time was twice the retention time of the main peak;the column temperature was 40℃;the detection wavelength was 220 nm;the flow rate was 1.0 mL/min;the injection volume was 20μL.The main component self-comparison with correction factor was used to calculate each impurity,and each impurity could be well separated,the LOQ was 0.005-0.008μg/ml,and the linear relationship is good,and the precision and accuracy of high,medium and low three concentrations meet the requirements.The results show the method has strong specificity,high sensitivity and easy operation,good repeatability,accurate and reliable results,can be used for impurity control of 1-fluoronaphthalene.