达肝素钠分子量及分子量分布的测定与计算方法改进

目的建立用高效分子排阻法测定达肝素钠分子量与分子量分布的方法,并与欧洲药典(EP)7.0版低分子肝素专论中的方法比较。方法采用高效分子排阻法,示差检测器,色谱柱TSK G3000SWXL(300 mm×7.8 mm,5μm)和TSKG2000SWXL(300 mm×7.8 mm,5μm)串联,柱温30℃,流动相0.1 mol/L乙酸铵溶液,流速0.5 mL/min。结果方法专属性强,重复性试验中重均分子量(Mw)的RSD为0.6%,Mw3000级分比例的RSD为2.1%,Mw 3000~8000级分比例的RSD为0.9%,样品测定结果与EP7.0方法测定结果接近。结论本方法操作简便,重复性好,结果准确可靠,可用于测定达肝素钠分子量与分子量分布。

Improvement of Determination and Calculation of Molecular Weight and Its distribution of Dalteparin Sodium

Objective To establish a method for determination of molecular weight and its distribution of dalteparin sodium and compare the method with that listed in European Pharmacopoeia（EP） 7.0.Methods Size-exclusion chromatography with refractive index detector was used.The samples were analyzed on a TSK G3000SWxL column（300 mm×7.8 mm,5 μm） in series with a TSK G2000SWxL column（300 mm×7.8 mm,5 μm） and the column temperature was 30 ℃.The mobile phase was 0.1 mol/L ammonium acetate,with a flow rate of 0.5 mL/min.Results The method is specific,with the RSD for weight average molecular weight（Mw） of 0.6 ％,and the RSD for proportion of the fraction with Mw less than 3000 and that of the fraction with Mw 3000-8000 in the repeatability test were 2.1％ and 0.9 ％,respectively.The results were closed to those determined by the method listed in EP 7.0.Conclusion The new method is simple,accurate and reliable,and can be used to determine molecular weight and its distribution of dalteparin sodium.