药学学报, 2002, 37(5): 359-361
引用本文:
徐新军;张正行;盛龙生;刘皋林;安登魁. 柱前荧光衍生化RP-HPLC测定环维黄杨星D含量[J]. 药学学报, 2002, 37(5): 359-361.
XU Xin-jun; ZHANG Zheng-xing; SHENG Long-sheng; LIU Gao-li; An Deng-kui. DETERMINATION OF CYCLOVIROBUXINE D BY RP-HPLC WITH PRECOLUMN FLUORESCENCE DERIVATIZATION[J]. Acta Pharmaceutica Sinica, 2002, 37(5): 359-361.

柱前荧光衍生化RP-HPLC测定环维黄杨星D含量
徐新军;张正行;盛龙生;刘皋林;安登魁
1. 中国药科大学药学院药物分析教研室,江苏 南京 210009; 2. 第二军医大学附属长征医院临床药理研究室,上海 200003
摘要:
目的建立环维黄杨星D含量测定方法。方法环维黄杨星D同异氰酸萘酯反应后,RP-HPLC荧光法测定。色谱柱为C18柱;流动相为甲醇-水(85∶15);流速:1 mL·min-1;荧光检测激发波长305 nm,发射波长385 nm;柱温35℃。结果衍生化反应重复性好,RSD为1.21%,主峰与相关物质分离良好。结论本法简单、准确,可用于环维黄杨星D及其相关物质含量测定。
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DETERMINATION OF CYCLOVIROBUXINE D BY RP-HPLC WITH PRECOLUMN FLUORESCENCE DERIVATIZATION
XU Xin-jun; ZHANG Zheng-xing; SHENG Long-sheng; LIU Gao-li; An Deng-kui
Abstract:
AIMTo establish a RP-HPLC method for determination of cyclovirobuxine D. METHODS Cyclovirobuxine D reacted with a derivative reagent 1-naphthyl isocyanate in chloroform to form fluorescence derivatives, stopped the reaction by adding the mobile phase and then directly injected the solution into the chromatograph to seperate it by RP-HPLC. The analysis was carried out on C18 column, the mobile phase is methanol-water (85∶15), the excitation wavelength was set at 305 nm, emission at wavelength 385 nm, and the flow rate was 1 mL·min-1. The effect of several factors including the reaction medium, temperature, time and amount of 1-naphthyl isocyanate on the yield of the derivatization was also investigated systematically. RESULTSA simple and rapid RP-HPLC method for the simultaneous isolation and analysis of cyclovirobuxine D and its related substances was developed, and the absence of interference between the derivative peak responses of cyclovirobuxine D and its related substances were verified by UV diode array detecter and MS. The linearity was obtained from 0.75 μg·mL-1 to 2.5 μg·mL-1 of cyclovirobuxine D derivatives with a correlation coefficient of 0.9991. The detection limit of cyclovirobuxine D derivative was 1 ng·mL-1, the repeatability of derivatization was good with relative standard derivation no more than 1.2% and derivative was stable within 48 h. The method described conforms to the validation of China Pharmacopiea compendial methods used for pharmaceutical products in general. CONCLUSIONThe established method is proved to be reliable quantitative method for the quality control of cyclovirobuxine D.
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通讯作者: 张正行
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