柱前衍生化RP-HPLC法对黄杨宁片原料中环维黄杨星D和杂质的定性定量研究
发布时间：2019-01-30 07:51
【摘要】：目的:建立黄杨宁片原料中环维黄杨星D准确定量和全面反映杂质色谱信息的分析方法。方法:选择可使主成分和所有杂质衍生化反应的试剂进行柱前衍生化反应,采用RP-HPLC法对衍生产物进行分析,C8柱分离,乙腈-0.01%甲酸水溶液(71∶29)洗脱,流速1 m L·min 1,检测波长230 nm,柱温25℃。结果:新建立的方法能使环维黄杨星D与有关生物碱的最低分离度达1.5,检测到的12个杂质峰,其中9个可被定量。环维黄杨星D检测限为0.35 ng(RSD=2.2%,n=5),定量限为1.37ng(RSD=4.6%,n=5);平均回收率为102.4%,RSD为1.4%(n=6)。来自4个厂家的10批样品中环维黄杨星D含量范围为78.28%~85.48%;9个杂质总含量范围为10.14%~15.57%。结论:该法既可使主成分与杂质完全分离,又可全面反映杂质色谱信息,能同时用于准确测定原料中主成分含量和杂质检查。
[Abstract]:Objective: to establish an accurate quantitative and comprehensive method for the determination of impurity chromatographic information in Huangyangning tablets. Methods: precolumn derivatization reaction was carried out with the reagent which could make the principal component and all impurity derivatization reaction. The derivative was analyzed by RP-HPLC, separated on C 8 column, and eluted by acetonitrile-0.01% formic acid solution (71:29). The flow rate was 1 m L min / 1, the detection wavelength was 230 nm, and the column temperature was 25 鈩，
本文编号：2417916
[Abstract]:Objective: to establish an accurate quantitative and comprehensive method for the determination of impurity chromatographic information in Huangyangning tablets. Methods: precolumn derivatization reaction was carried out with the reagent which could make the principal component and all impurity derivatization reaction. The derivative was analyzed by RP-HPLC, separated on C 8 column, and eluted by acetonitrile-0.01% formic acid solution (71:29). The flow rate was 1 m L min / 1, the detection wavelength was 230 nm, and the column temperature was 25 鈩，
本文编号：2417916
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