HPLC法同时测定复方甲地孕酮注射液中主药的含量及有关物质

摘要

目的:建立测定复方甲地孕酮注射液中主药的含量及有关物质的方法.方法:采用高效液相色谱法.色谱柱为Diamon-sil C18柱,流动相为甲醇-水(70:30),流速为1.0 mL·min-1,进样量为20 μL,柱温为40℃,检测波长为280 nm.结果:醋酸甲地孕酮和雌二醇的检测浓度分别在0.5～100.0、3.0～90.0μtg·mL-1范围内与其峰面积积分值呈良好的线性关系(r=0.999 9).醋酸甲地孕酮定量限为17 ng,最低检测限为5 ng;雌二醇定量限为12 ng,最低检测限为3.5 ng.醋酸甲地孕酮和雌二醇的低、中、高平均回收率分别为102.0％、100.0％、99.9％和101.0％、101.7％、99.4％,RSD分别为0.37％、0.06％、0.10％和0.21％、0.17％、0.46％(n=9).结论:该方法简便准确、重复性好,可用于复方甲地孕酮注射液的质量控制.%OBJECTIVE: To establish a method for the content and related substances determination of Compound megestrol injection. METHODS: The chromatographic separation was achived on a Diamonsil Ci8 Column with the mobile phase of metha-nol-water (70:30). The flow rate was 1.0 mL-min"1 with column temperrature at 40 °C. The detection wavelength was 280 nm. The injection volumn was 20 u.L. RESULTS: The linear range was 0.5~ 100.0 ug-mL"1 for megestrol acetate (r=0.999 9) and 3.0~90.0 ig-mL1 for estradiol (r=0.999 9). The quantitative limit and detection limit of megestrol acetate were 17 ng and 5 ng; those of estradiol were 12 ng and 3.5 ng. The average recoveries rates of it at low, medium and high concentrations were 102.0%, 100.0%, 99.9% and 101.0%, 101.7%, 99.4% and RSD was 0.37%, 0.06%, 0.10% and 0.21%, 0.17%, 0.46% (?=9). CONCLUSION: The method is simple, accurate and reproducible for the quality control of Compound megestrol injection.