离子色谱法测定伊班膦酸钠注射液主成分的方法探讨

为建立一种药物伊班膦酸钠注射液主成分-伊班膦酸的离子色谱分析方法,采用Ion Pac AS18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(12~70 mmol·L~(-1),时间程序为17 min),并使用自动再生抑制型电导检测。结果表明,伊班膦酸浓度在0~75.25?g·m L~(-1)范围内,线性相关系数R2=0.9995,呈现显著的线性相关关系;供试液重复进样5次,峰面积RSD为0.21%,保留时间RSD为0.01%,理论板数均大于50 000,方法系统适用性良好;5份供试样品溶液伊班膦酸含量的RSD值为0.80%,小于等于2.0%,方法重复性良好;供试样品3个浓度水平的回收率均在99%~101%之间,加标回收率试验的RSD均小于1.00%,符合药品规定要求。该方法稳定、重复性好且回收率高,可满足伊班膦酸钠注射液中主成分含量的测定要求。

Determination of the main components in ibandronate sodium injection by ion chromatography

A method for determination of ibandronate in ibandronate sodium injection using ion chromatography was established in this study.Ion Pac AS 18 was used as anion exchange column.The analysis was conducted with an online eluent generator that automatically generated a gradient of potassium hydroxide (12-70mmol·L-1,time program was 25 minutes),and an automatic regeneration suppressor was used to detecte the conductivity.Our results showed that a good linear relationship (R2=0.9995) was obtained in the measurement of ibandronic acid at a concentration range from 0 to 75.25 μg·mL-1.As for the deternination of the product solution,after being repeated five times,the RSD value of the peak area and retention time was 0.21％ and 0.01％,respectively,and the theoretical plate number was more than 50 000,which suggested a good applicability of this method.The RSD value of the ibandronic acid content was 0.80％ that was less than 2.0％,which indicated a good repeatability of this method.Recovery rates of the tested samples at three concentrations were between 99％-101％,and RSD of the recovery rate was smaller than 1.00％,which was in line with the requirements of pharmaceutical regulations.This assay method is proved to be satisfactory for determination of ibandronic acid in ibandronate sodium injection with good repeatability,high recovery rate,which can meet the requirements for determination of the main components in ibandronate sodium injection.