离子色谱法测定那屈肝素钙中亚硝酸盐含量

目的建立那屈肝素钙原料中亚硝酸盐测定方法。方法采用离子色谱法,电化学检测器,工作电极为玻碳电极,参比电极为Ag/AgCl,流速1.0 mL/min,进样体积100μL,色谱柱为Waters Anion HC(150 mm×4.6 mm,10μm)。结果亚硝酸根离子与其他离子分离度良好,在0.004~0.056μg/mL范围内浓度与峰面积线性关系良好,r=0.999,重复性试验的RSD为2.1%,检出限为0.002μg/mL,定量限为0.0032μg/mL。平均回收率为101.2%,RSD为2.6%(n=9)。结论该方法可用于那屈肝素钙中亚硝酸盐测定。

Determination of Nitrite in Nadroparin Calcium by Ion Chromatography

Objective To establish a method for determination of nitrite in nadroparin calcium. Methods Ion chromatography was used. The detector was electrochemical device with glassy carbon electrode as the working electrode versus Ag/AgCl reference electrode. The flow rate was 1.0 mL/min. The injection size was 100 gL. The determination was performed on the Waters Anion HC column （150 mm× 4.6 mm, 10 μm）. Results The resolution was good between nitrite and other ions. There was good linearity between the concentration and peak area of nitrite in the range of 0.004-0.056 μg/mL（r=0.999）. The RSD of repeatability test was 2.1%. The limit of detection was 0.002 gg/mL and the limit of quantitation was 0.0032 μg/mL. The average recovery was 101.2 % with RSD of 2.6 %（n=9）. Conclusion The method can be used for determination of nitrite in nadroparin calcium.