离子抑制色谱法测定伊班膦酸钠原料药中的有关物质  

Determination of related substances in ibandronate sodium raw materials by ion suppression chromatography

作　　者：陈霞 张洁 董瑞 CHEN Xia;ZHANG Jie;DONG Rui(Chengdu Institute for Food and Drug Control,Chengdu 610045)

机构地区：[1]成都市食品药品检验研究院,成都610045

出　　处：《中南药学》2021年第9期1934-1938,共5页Central South Pharmacy

基　　金：四川省科技计划项目(No.2020YFS0570)。

摘　　要：目的建立伊班膦酸钠中有关物质的离子抑制色谱检测方法。方法采用阴离子交换色谱柱Dionexionpac AS11-HC(4 mm×250 mm,9μm),保护柱为AG11-HC(4 mm×50 mm),以100 mmol·L^(-1) NaOH为流动相A、水为流动相B,梯度洗脱,流速为1.0 mL·min^(-1),检测器为电导检测器,柱温30℃,进样量20μL。结果各已知杂质及杂质与主成分之间分离度均大于1.5,主成分与强制破坏产生的降解产物分离度良好;各杂质在检测质量浓度范围内与峰面积线性关系良好;平均回收率在93.48%~100.30%;定量限和检测限均符合要求。结论本方法准确度高,重复性良好,灵敏度高,适用于伊班膦酸钠原料药中有关物质的检查。Objective To determine the related substances in ibandronate sodium raw materials by ion suppression chromatography.Methods The chromatographic separation was performed on a Dionexionpac AS11-HC(4 mm×250 mm,9μm)column and analyzed by conductivity detector,with 100 mmol·L^(-1) sodium hydroxide as the mobile phase A and water as the mobile phase B by gradient elution.The flow rate was 1.0 mL·min^(-1).The column temperature was 30℃and the injection volume was 20μL.Results The separation between the impurity and main components was greater than 1.5,and the main components and degradation products by forced destruction well separated.The linearity was good within the concentration range.The average recovery was 93.48%^-100.30%.The quantitative limit and detection limit met the requirements.Conclusion This method is accurate,reproducible and sensitive for the determination of related substances in ibandronate sodium raw materials.

关 键 词：离子抑制色谱法 伊班膦酸钠 有关物质 N-甲基-N-戊基-β-氨基丙酸盐酸盐 亚磷酸 N-去甲基杂质 

分 类 号：R927[医药卫生—药学]