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

Simultaneous Content Determination of Related Substances and Content of Compound Megestrol Injection by HPLC

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1.0mL·min-1,进样量为20μL,柱温为40℃,检测波长为280nm。结果:醋酸甲地孕酮和雌二醇的检测浓度分别在0.5～100.0、3.0～90.0μg·mL-1范围内与其峰面积积分值呈良好的线性关系(r=0.9999)。醋酸甲地孕酮定量限为17ng,最低检测限为5ng;雌二醇定量限为12ng,最低检测限为3.5ng。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 C18 Column with the mobile phase of methanol-water（70：30）.The flow rate was 1.0 mL·min-1 with column temperrature at 40 ℃.The detection wavelength was 280 nm.The injection volumn was 20 μL.RESULTS：The linear range was 0.5～100.0 μg·mL-1 for megestrol acetate（r=0.999 9） and 3.0～90.0 μg·mL-1 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%（n=9）.CONCLUSION：The method is simple,accurate and reproducible for the quality control of Compound megestrol injection.