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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,5μm),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 a RP-HPLC method for the determination of nomectine in small-molecule targeted anti-tumor drugs. Methods: Agilent Zorbax eclipse plus C18 column (250 mm × 4.6 mm, 5 μm) was used. The mobile phase consisted of 0.68% potassium dihydrogen phosphate solution (containing 0.1% triethylamine and adjusted to pH 3.1 with phosphoric acid) ); Flow rate: 1.0 mL.min-1; detection wavelength: 231 nm; column temperature: 35 ° C. RESULTS: The main peak was well separated from the adjacent impurity peaks. The calibration curve was linear in the range of 0.062-0.62 mg.mL-1 (r = 0.9999). The average recovery was 99.9% (RSD = 0.58%, n = 9). The repeatability was 0.23% (n = 6). The limit of detection was 0.5 ng and the limit of quantification was 1.0 ng. Conclusion: The method is sensitive, accurate and specific, and can be used for the determination of Minocytin raw materials.