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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。
OBJECTIVE: To establish an accurate and quantitative method for the analysis of impurity chromatographic information of cyclovirobuxine in raw materials of Huangyangning tablet. Methods: The pre-column derivatisation reaction was carried out on the reagents which can make the main components and all impurities derivatization. The derivatized products were analyzed by RP-HPLC. The C8 column was separated by acetonitrile-0.01% formic acid solution (71:29) , Flow rate 1 m L · min-1, detection wavelength 230 nm, column temperature 25 ℃. Results: The newly established method can make the lowest separation of Cyclohexene D star and related alkaloids 1.5, 12 peaks detected, of which 9 can be quantified. The detection limit of cloveine D was 0.35 ng (RSD = 2.2%, n = 5) and the limit of quantification was 1.37 ng (RSD = 4.6%, n = 5). The average recovery was 102.4% with RSD of 1.4% = 6). The contents of D-bayanin D in 10 batches of samples from 4 factories ranged from 78.28% to 85.48%. The total content of 9 impurities ranged from 10.14% to 15.57%. Conclusion: The method can not only completely separate the main components and impurities, but also fully reflect the impurity chromatographic information, which can be used for the accurate determination of the content of the main components and impurities in the raw materials.