【摘要】 目的 采用衍生化HPLC法测定艾曲波帕中的基因毒性杂质3,4-二甲基苯肼。方法 用苯甲醛作为衍生化试剂，衍生化样品后，用HPLC法测定。采用Gemini C₁₈色谱柱（250 mm×4.6 mm, 5μm）,以0.1%三氟乙酸溶液-乙腈（30:70）为流动相，流速1.0 mL·min^-1,检测波长348 nm。结果 3,4-二甲基苯肼衍生物与样品中其他组分能完全分离；0.02～0.12μg·mL^-13,4-二甲基苯肼与峰面积的线性关系良好（r=0.9989）,检测限为0.01μg·mL^-1,进样精密度良好，3,4-二甲基苯肼衍生物在8 h内稳定（RSD=1.20%）,平均回收率为102.10%,RSD为1.50%（n=9）。样品中未检出3,4-二甲基苯肼，其含量在1.0 ppm以下，符合要求。结论 所用方法专属、灵敏、准确，适用于检测艾曲波帕中的基因毒性杂质3,4-二甲基苯肼。更多还原

【Abstract】 OBJECTIVE To determine the residual 3,4-dimethylphenylhydrazine as a genotoxic impurity in Eltrombopag by HPLC.METHODS Benzaldehyde was used as the derivatization reagent.The separation was performed on a Gemini C₁₈ column（250 mm×4.6 mm, 5 μm） with 0.1% trifluoroacetic acid solution-acetonitrile（30:70） as mobile phase at a flow rate of 1.0 mL·min^-1.The column temperature was 30 ℃,the detection wavelength was 348 nm, and the injection volume was 20 μL.RESULTS The 3,4-dimethylphenylhydrazine derivatives was completely separated from other components in the sample.The 3,4-dimethylphenylhydrazine derivatives had good linearity in the range of 0.02-0.12 μg·mL^-1（r=0.9989）,and the limit of detection was 0.01 μg·mL^-1.The injection precision was validated; 3,4-dimethylphenylhydrazine derivatives were stable within 8 h（RSD=1.2%）.The average recovery was 102.1% with RSD of 1.5%（n=9）.In the samples, 3,4-dimethylphenylhydrazine was not detected, which meant the contents were below 1.0 ppm, meeting the requirements.CONCLUSION This method is specific, sensitive, accurate, and can be used for the detection of genotoxic impurity 3,4-dimethylphenylhydrazine in Eltrombopag.更多还原