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目的 建立醋酸亮丙瑞林注射液中亮丙瑞林及杂质的测定方法。方法 采用高效液相色谱法。色谱柱 :KromasilC18 ODS(15 0mm× 4 . 6mm ,5 μm)不锈钢柱 ;流动相 :水相 (80 0ml水 +2 1ml三乙胺 ,磷酸调pH 3 .0 ,加水至 10 0 0ml) 有机相 (正丙醇 乙腈 =2∶3)为 84∶16 ;检测波长 :2 2 0nm ;含量测定采用外标法 ,杂质检查采用自身对照法。结果 在优化的色谱条件下 ,亮丙瑞林及杂质间均能完全分离 ,注射液辅料不干扰测定 ,亮丙瑞林线性范围 9. 198～ 82. 780 μg·ml 1,检测限 1 93ng(S/N =3) ,含量测定的回收率 98. 74 %～ 10 0. 3% ,RSD <1. 5 %。结论 该法专属性强 ,操作方便 ,结果准确 ,重现性好。
Objective To establish a method for the determination of leuprolide and impurities in leuprolide acetate injection. Methods Using high performance liquid chromatography. Column: Kromasil C18 ODS (15 0 mm × 4. 6 mm, 5 μm) stainless steel column; mobile phase: water phase (80 0 ml water + 21 ml triethylamine and phosphoric acid adjusted to pH 3.0 with water up to 10 0 ml) (N-propanol, acetonitrile = 2: 3) was 84:16, detection wavelength was 220 nm, external standard method was used for the determination of content, and the self-control method was used for impurity inspection. Results Under the optimized chromatographic conditions, the separation between leuprolide and impurities was complete. The injection excipient did not interfere with the determination. The linear range of leuprolide was 9. 198 ~ 82. 780 μg · ml 1, the detection limit was 1 93 ng S / N = 3), the determination of the recovery rate of 98. 74% ~ 10 0.3%, RSD <1.5%. Conclusion The method is highly specific, easy to operate, accurate and reproducible.