HPLC-示差折光检测器测定米格列醇片的含量及有关物质

目的建立高效液相色谱-示差折光检测法测定米格列醇片的含量和有关物质。方法用磺酸基阳离子交换键合硅胶(250×4.6mm,5μm)为填充剂;以乙腈-三氟乙酸溶液(4.5→1000mL)(20∶80)为流动相;示差折光检测器检测;检测器温度为40℃。理论板数以米格列醇峰计算,应不低于2000。结果空白辅料不干扰测定,米格列醇主峰和杂质峰分离良好,定量限浓度约为10μg·mL^-1。米格列醇浓度在26.28~210.2μg·mL^-1范围内,与峰面积线性关系良好,线性方程A=2611.5C-2802,r=0.9988;平均回收率100.9%(RSD=1.0%;n=9);溶液在8h内稳定。结论本法专属性强、灵敏度高、准确度和稳定性好,可作为米格列醇片有关物质和含量测定的检测方法。

Determination of Miglitol Tablets and Related Substances by HPLC with Differential Refractive Detector

OBJECTIVE To establish a method for the determination of miglitol tablets and related substances by high performance liquid chromatography(HPLC)with differential refraction detection.METHODS Sulfonated cation exchange bonded silica gel(250×4.6mm,5μm)was used as filler,acetonitrile-trifluoroacetic acid solution(4.5→1000mL)(20∶80)as mobile phase,differential refractive detector was used for detection,and the detector temperature was 40℃.The number of theoretical plates calculated by the peak of miglitol should not be less than 2000.RESULTS The blank excipients did not interfere with the determination.The main peak and impurity peak of miglitol were separated well,and the quantitative limit concentration was about 10μg·mL^-1.The concentration of Miglitol in the range of 26.28-210.2μg·mL^-1 has a good linear relationship with the peak area.The linear equation was A=2611.5C-2802,r=0.9988;the average recovery rate was 100.9%(RSD=1.0%;n=9),and the solution was stable within 8 hours.CONCLUSION The method is specific,sensitive,accurate and stable,and can be used for the determination of related substances and contents in Miglitol Tablets.