RP-HPLC法测定小分子靶向民诺莫司汀的含量

目的:建立RP-HPLC法测定小分子靶向抗肿瘤创新药民诺莫司汀的含量。方法:采用安捷伦Zorbax eclipse plus C₁₈柱(250 mm×4.6 mm,5 μm),流动相:0.68%磷酸二氢钾溶液(含0.1%三乙胺,用磷酸调节pH至3.1)-乙腈(75∶25);流速:1.0 mL·min^-1;检测波长:231 nm;柱温:35 ℃。结果:主峰能与相邻杂质峰较好地分离,民诺莫司汀在0.062~0.62 mg·mL^-1 范围内呈良好的线性关系(r=0.9999);平均回收率为99.9%(RSD=0.58%,n=9);重复性试验测得的精密度为0.23 %(n=6);检测限为0.5 ng、定量限为1.0 ng。结论:该方法灵敏、准确、专属性好,可用于民诺莫司汀原料的含量测定。

Objective:To establish an RP-HPLC method for the determination of minomustine,an innovative small molecular targeted antineoplastic drug.Methods:Agilent Zorbax eclipse plus C₁₈ column(250 mm×4.6 mm,5 μm)was adopted with the mobile phase consisting of 0.68% potassium dihydrogen phosphate(containing 0.1% triethylamine,adjust to pH 3.1 with phosphoric acid)-acetonitrile(75∶25)at the flow rate of 1.0 mL·min^-1; detection wavelength was at 231 nm,and the column temperature was 35 ℃.Results:The main peak was well separated from adjacent impurities and the linear range of the method was 0.062-0.62 mg·mL^-1(r=0.9999),the average recovery was 99.9%(RSD=0.58%,n=9),RSD of repetitive test was 0.23%(n=6),the limit of detection and quantitation was 0.5 ng and 1.0 ng,respectively.Conclusion:The established method was sensitive,accurate and specific,which can be used for minomustine determination.

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