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目的:建立柱前衍生化HPLC法测定小儿金丹片中朱砂的含量。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HPLC法,使用C_(18)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1.0 ml·min~(-1),柱温35℃。结果:Hg~(2+)在0.10~0.63μg范围内线性关系良好,r=0.999 2,平均加样回收率98.4%(RSD为0.40%,n=9)。结论:本法结果准确,便于操作,可作为小儿金丹片的质量控制方法之一。
OBJECTIVE: To establish a pre-column derivatization HPLC for the determination of cinnabar in children’s saxophone tablets. Methods: Sodium diethyldithiocarbamate (NaDDC) was used as a derivatization reagent. The samples were determined by digestion, derivatization and organic solvent extraction. The mobile phase consisted of methanol - water (NaDDC containing 0.02 mmol·L -1) (87:13), detection wavelength at 272 nm and flow rate of 1.0 ml · min ~ (- 1), column temperature 35 ℃. Results: The linear range of Hg 2+ in the range of 0.10-0.63 μg was good, r = 0.999 2, and the average recovery was 98.4% (RSD = 0.40%, n = 9). Conclusion: The results of this method are accurate and easy to operate and can be used as one of the quality control methods for pediatric saxophone tablets.