高效分子排阻色谱法测定头孢唑肟钠中聚合物的含量

Determination of impurities including polymers in ceftizoxime sodium by HPSEC

目的建立高效分子排阻色谱法（HPSEC）测定头孢唑肟钠中的聚合物等杂质。方法采用球状蛋白亲水改性硅胶柱（Zenix SEC-150，7．8mm×300mm，3gm）；流动相为磷酸盐缓冲液（pH7．0）[0．075mol／L磷酸氢二钠溶液-0．075mol／L磷酸二氢钠溶液（61：39）1-乙腈（90：10）；流速为1．0mL／min；检测波长为254nm；进样量为10此。结果头孢唑肟的线性范围为1．15～57．40gg／mL（r=0．9999）；定量限为3．2ng、检出限为1．2ng；聚合物等杂质测定的线性范围为0．0500～4．998mg／mL（r=0．9995）；对照品溶液重复进样的精密度（RSD）为0.31％（n=6），样品测定的重复性（RSD）为0．67％（n=6）。结论该方法适于测定头孢唑肟钠中聚合物等杂质，灵敏度高，重复性好，操作简便。

Objective To establish a high performance size exclusion chromatography （HPSEC） method for the determination of impurities including polymers in ceftizoxime sodium. Methods The analysis was performed on a Zenix SEC-150 column （7.8mm×300mm, 3μm） with the mobile phase consisting of phosphate buffer solution [0.075mol/L disodium hydrogen phosphate-0.075mol/L sodium dihydrogen phosphate （61：39）, adjusted to a pH of 7.0]-acetonitrile （90：10） at a flow rate of 1.0mL/min. The detection wavelength was set at 254 nm. The injection volume was 10μL. Results The impurities including polymers in ceftizoxime sodium were completely separated from ceftizoxime. The linear range of ceftizoxime was 1.15-57.40μg/mL （r=0.9999）. The limit of quantitation of ceftizoxime was 3.2ng, and the detection limit was 1.2ng. The linear range of the total impurities was 0.0500-4.998mg/mL （r=0.9995）. The RSD for replicate injection of reference solution was 0.31% （n=6）, and the RSD for the measurement of total impurities was 0.67% （n=6）. Conclusion This established method is accurate, rapid, reproducible, and suitable for the determination of impurities including polymers in ceftizoxime sodium.