离子色谱法测定头孢曲松钠中的钠离子含量以及成盐率

目的: 建立离子色谱法测定注射用头孢曲松钠中钠离子的含量并计算其成盐率. 方法: 采用IonPac CS-12A阳离子交换色谱柱(250 mm×4 mm),IonPac CS-12A保护柱(50 mm×4 mm),以淋洗液发生器产生的20 mmol·L^-1甲烷磺酸(MSA)溶液作为流动相,流速1.0 mL·min^-1,抑制器电流值设定为65 mA. 结果: 钠离子在浓度为1~15 μg·mL^-1范围内与峰面积呈良好的线性关系,r=0.999 7(n=8);检测限为0.25 ng,定量限为2.5 ng;回收率(n=9)为99.0%~100.3%.测定了12家不同企业提供的27批注射用头孢曲松钠中钠的含量在6.8%~7.2%之间,其成盐率在1.88~2.06之间,无明显差异. 结论: 本方法可用于注射用头孢曲松钠中钠离子的测定.

Objective: To establish an ion chromatographic method to determine the content of sodium ion and salt-forming rate in ceftriaxone sodium. Methods: A column of IonPac CS-12A (250 mm×4 mm) and a protect column of IonPac CS-12A (50 mm×4 mm) were used.20 mmol·L^-1 of MSA solution produced by eluent generator was used as the mobile phase.The flow rate was 1.0 mL·min^-1 and the suppressor current value was set as 65 mA. Results: Sodium,potassium,lithium and the degradation products could be separated completely in this chromatographic condition.The linear range was 1-15 μg·mL^-1(r=0.999 7).The LOD was 0.25 ng,and the LOQ was 2.5 ng.The recoveries (n=9) of sodium were in the range of 99.0%-100.3%.The contents of sodium ion in ceftriaxone sodium for injection provided by 12 different companies were between 6.8% and 7.2%,and the salt-forming rates were between 1.88 and 2.06,and there were no significant differences. Conclusion: This method can be used for the determination of sodium ion in ceftriaxone sodium for injection.

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