摘要
目的建立用高效液相色谱测定一捻金中朱砂含量的方法。方法以二乙基二硫代氨基甲酸钠(NaDDC)为衍生化试剂,样品经消解、衍生化和有机溶剂提取后测定。采用高效液相色谱法,使用C18柱,流动相为甲醇-水(含0.02 mmoL.L-1的NaDDC)(87:13);检测波长272 nm;流速1 mL.min-1,柱温35℃。结果 Hg2+在0.1052~0.6312μg范围内线性关系良好,平均加样回收率99.23%。结论本法结果准确,便于操作,可作为一捻金的质量控制方法之一。
Objective To establish an HPLC method with pre-column derivatization for determination of cinnabar in Yinianjin.Methods Sodium diethyldithiocarbamate(NaDDC) was used as a derivatization reagent,the samples were treated by digested,derivatized and extracted by organic solvent.The determination was carried out by HPLC method,using C18 column,and mobile phase was methanol-water(including 0.02 mmoL·L-1 of NaDDC)(87:13);The detection wavelength was 272 nm;The flow rate was 1 L·min-1,the column temperature was 35 ℃.Results Hg2+ had good linear relationship in the range of 0.105 2~0.631 2 μg,the average recovery was 99.23%.Conclusion The method was simple and accurate,it was suitable for quality control of Yinianjin.
出处
《齐鲁药事》
2011年第4期204-206,共3页
qilu pharmaceutical affairs