达肝素钠原料药中游离硫酸盐测定方法的研究

Determination of Free Sulfate in Dalteparin Sodium

目的 建立达肝素钠原料中游离硫酸盐测定方法。方法 采用离子色谱法,色谱柱为Waters IC-Pak Anion（50mm×4.6 mm,10μm）,流动相为7 mmol/L四硼酸钠-0.1 mol/L氢氧化钠,梯度洗脱,流速1.0 mL/min,进样量25μL,电导检测器,抑制电流50 mA。结果 硫酸根离子与其他离子分离度好,在0.4-15μg/mL浓度范围内线性关系良好,相关系数r=0.999,重复性试验的RSD为1.6%,检出限为0.05μg/mL,定量限为0.4μg/mL,平均回收率为103.0%,RSD为2.3%（n=9）。结论 此法可用于达肝素钠中游离硫酸盐测定。

Objective To establish a method for determination of free sulfates in dalteparin sodium. Methods Ion chromatography was used. The determination was performed on the Waters IC-Pak Anion column （50 mm - 4.6 mm, 10 μm）. A gradient elution with 7 mmol/L disodium tetraborate-0.1 mol/L sodium hydroxide as mobile phase wasadopted at the flow rate of 1.0 mL/min. The injection size was 25 IxL. Conductivity detector with depression current of 50 mA was used in the determination. Results The resolution was good between free sulfates and other ions. The linearity was obtained in the range of 0.4-15 ~tg/mL（r=0.999）. The RSD of repeatability was 1.6 %. The limit of detection was 0.05 pg/mL and the limit of quantitation was 0.4 ~tg/mL. The average recovery was 103.0 % and RSD was 2.3 %（n=9）. Conclusion The method can be used to determine free sulfates in dalteparin sodium.