醋酸亮丙瑞林杂质谱研究和有关物质HPLC分析方法建立

醋酸亮丙瑞林杂质谱研究和有关物质HPLC分析方法建立

赵丽佳;俞炯;蒋惠娣

【期刊名称】《药物分析杂志》 【年(卷),期】2017(037)008

【摘要】Objective:To study the impurity profile of leuprorelin acetate and develop an HPLC method for the determination of related substances.Methods:The analysis was conducted on a full coverage chemically bonded silica column [Sepax GP-C18 column (150 mm × 4.6 mm,3 μm)] with a mobile phase of triethylamine buffer,n-propyl alcohol and acetonitrile mixed solution by isocratic at the flow rate of 0.9 mL· min-1 for 90 min.The column temperature was 35 ℃,the detection wavelength was 220 nm and the injection volume was 20 μL.Results:The known impurities and degraded products by forced degradation were completely separated from leuprorelin acetate.The calibration curves of impurity B (2-D-His-leuprorelin) and impurity M (deletion 4-Ser-leuprorelin) were linear in the self-concentration range of 0.001-0.02 mg· mL-1 (r2 ≥ 0.999,n=6) and the correction factors were 1.09.The average recoveries of the impurities B and M (n=9)were 96.1％ and 108.3％,respectively,and the RSDs (n=9) were 1.6％ and 3.0％,respectively.The RSDs of repeatability (n=6) for impurity B,impurity M and total impurities were 0.85％,1.9％ and 1.7％,respectively.The RSD of peak area (n=5) for all validation items was no more than 1.4％,and