离子色谱法测定伊班膦酸钠原料中伊班膦酸的含量

目的: 建立伊班膦酸钠原料中伊班膦酸的离子色谱分析方法.方法: 采用Ion Pac AS11阴离子交换色谱柱,利用在线淋洗液发生器自动产生氢氧化钾梯度淋洗液(20~40 mmol·L^-1,时间程序为25 min),以自动再生抑制型电导检测.结果: 该方法具有较高的精密度[重复性平均值为100.1%,RSD=0.6%(n=6);中间精密度平均值为103.0%,RSD=0.6%(n=6);进样精密度RSD=0.4%(n=5)]、准确度[3个浓度水平的平均回收率(n=3)分别为100.2%、100.5%、102.7%,RSD分别为0.4%、1.2%、1.7%]和专属性,伊班膦酸钠的线性范围为6.06~96.90 μg·mL^-1,r=0.9999.结论: 经方法学验证,本方法可用于伊班膦酸钠中伊班膦酸含量的快速分析.

Objective: To establish an assay method for ibandronate in ibandronate sodium by using ion chromatography. Methods: Ion Pac AS11 was used as anion exchange column.The analysis was conducted with online eluent generator that automatically generated potassium hydroxide which was served as the mobile phase(20-40 mmol·L^-1, time program was 25 minutes)and the conductivity detection with automatic regeneration suppressor was conducted. Results: The method had a good precision the mean repeatability was 100.1%, RSD=0.6%(n=6);the mean intermediate-precision was 103.0%, RSD=0.6%(n=6);RSD of injection-precision was 0.4%(n=5)], accuracy the mean recoveries(n=3)were 100.2%, 100.5%, 102.7%.respectively, and RSDs were 0.4%, 1.2%, 1.7% for three concentration levels] and specificity.The linear range for ibandronate sodium was 6.06-96.90 μg·mL^-1, r=0.99997. Conclusion: Through validation by analytical method, this method can be used for fast analysis of ibandronate sodium content.

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