摘要
目的:建立一种用于测定注射用益气复脉(冻干)中钠离子含量的HPLC-ELSD方法。方法:采用Sepherisorb SCX(250 mm×4.6 mm,5μm)色谱柱,以0.05 mol·L^(-1)醋酸铵(醋酸调节p H 4.8)-乙腈(50∶50)为流动相,流速1.0 m L·min^(-1),柱温30℃,蒸发光散射器漂移管温度80℃,气体压力241 k Pa,增益15。结果:钠离子进样量在14.799~123.325μg(r=0.9995)范围内线性关系良好,平均回收率(n=9)为96.9%;样品中钠离子含量为19.05~20.67 mg·g^(-1)。结论:本法可为注射用益气复脉(冻干)生产中钠离子的控制提供实验方法。
Objective:To establish an HPLC-ELSD method for the determination of the content of sodium ion in lyophilized Yiqi Fumai for injection.Methods:The chromatographic separation was achieved on a Sepherisorb SCX(250 mm×4.6 mm,5μm)column with mobile phase at a flow rate of 1.0 mL·min^-1.The mobile phase was water solution consisting of 0.05 mol.L^-1 ammonium acetate(pH was adjusted to 4.8 by acetic acid)-acetonitrile(50:50).The column temperature was 30℃.The drift tube temperature for the ELSD was set at 80 with the carrier gas pressure of 241 kPa and the detector gaining of 15.Results:Good linearity(r=0.9995)was observed in the standard curves of sodium in the range of 14.799-123.325μg,and the average recovery n=9 ot me method for sodium was 96.9%.The content of sodium ion in lyophilized Yiqi Fumai for injection was 19.05-20.67 mg.g^-1.Conclusion:The present process can provide an experimental method for the production quality control of sodium ion in lyophilized Yiqi Fumai for injection.
作者
习斌斌
徐敏
李德坤
周大铮
杨悦武
寇俊萍
鞠爱春
XI Bin–bin;XU Min;LI De–kun;ZHOU Da–zheng;YANG Yue-wu;KOU Jun-ping;JU Ai-chun(Jiangsu Key Laboratory of TCM Evaluation and Translational Researeh,Department of Complex Prescription of TCM,Nanjing 211198,China;Tianjin Tasly Pride Pharmaceutical Co.,Ltd.,Tianjin 300402,China;Tianjin Key Laboratory of Safety Evaluation Enterprise of TCM Injections,Tianjin 300402,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2016年第8期1503-1507,共5页
Chinese Journal of Pharmaceutical Analysis
基金
科技重大专项"重大新药创制"(No.2013ZX09402202)
