高效分子排阻色谱法测定头孢曲松钠原料药中的聚合物

Determination of Polymers in Ceftriaxone Sodium by HPSEC

目的：建立测定头孢曲松钠原料药中聚合物的方法。方法：采用高效分子排阻色谱法。色谱柱为TSK-GEL G2000SWXL,流动相为0.01 mol/L磷酸盐缓冲液[0.01 mol/L Na H2PO4溶液-0.01 mol/L Na2HPO4溶液（38∶62,V/V）]-乙腈（95∶5,V/V）,检测波长为240 nm,柱温为25℃,进样量为10μl,流速为0.6 ml/min。结果：头孢曲松质量浓度在0.56～28μg/ml范围内与峰面积呈良好的线性关系（r=0.999 7）;精密度、重复性试验的RSD≤1.4%;以头孢曲松计,检测限为0.2 ng,定量限为0.7 ng。该方法聚合物检测结果略高于2010年版《中国药典》方法。结论：该方法专属性强、灵敏度高、重复性好,可有效控制头孢曲松钠原料药中聚合物的量。

OBJECTIVE： To establish a method for the determination of polymers in ceftriaxone sodium. METHODS： High performance size exclusion chromatography （HPSEC） was adopted. The determined was performed on TSK-GEL G 2000SWXL col- umn with mobile phase consisted of 0.01 mol/L phosphate buffer solution [0.01 mol/L NaH2PO4 solution-0.01 mol/L Na2HPO4 solu- tion（38 ： 62, V/V）]-acetonitrile（95 ： 5, V/V）at the flow rate of 0.6 ml/min. The detection wavelength was set at 240 nm, and column temperature was 25 %. The sample size was 10 μl. RESULTS： The linear range of ceftriaxone were 0.56-28 μg/ml（r=0.999 7）. RSD of precision and repetitive tests were ≤ 1.4% ; counted by ceftriaxone,the limits of detection and quantization were 0.2 ng and 0.7 ng respectively. The quantity of polymers was little higher by new method than by the method stated in Chinese Pharmacopeia （2010 edition）. CONCLUSIONS： The method is specific, sensitive and reproducible, and can control the quantity of polymers in ceftriaxone sodium effectively.