毛细管区带电泳法测定山茱萸中齐墩果酸和熊果酸的含量
Determination of Oleanolic and Ursolic Acids in Fructus Corni by Capillary Zone Electrophoresis
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摘要: 提出了毛细管区带电泳、高频电导法测定山茱萸中齐墩果酸和熊果酸含量的方法.采用未涂层弹性融硅石英毛细管柱(55 cm×75 μm,有效长度50 cm),pH 10.60的1.2 mmol·L-1三乙胺-盐酸-0.08 mmol·L-1 β-环糊精为运行缓冲溶液,分离电压12.5 kV,流体静压进样10 s(高度20 cm).以布洛芬为内标,齐墩果酸、熊果酸线性范围分别为4.1~114.8 mg·L-1和4.3~120.4 mg·L-1.测得平均回收率均为96.0%,所提出方法用于山茱萸药材中齐墩果酸和熊果酸含量测定,测得相对标准偏差(n=6)分别为2.03%,2.29%.Abstract: Capillary zone electrophoresis (CZE) with high frequency conductivity detection was applied to the determination of oleanolic and ursolic acids in Fructus corni.An uncoated elastic fused quartz capillary column (55 cm×75 μm,effective length 50 cm) was used and efficient separation was achieved by using the buffer mixture (containing 1.2 mmol·L-1 triethylaminehydrochloric acid solution and 0.08 mmol·L-1 β-cyclodextrin solution with its acidity adjusted to pH 10.60) as moving solution,and the separation voltage at 12.5 kV.The sample was introduced hydrostatically at a height of 20 cm for 10 s.“Buluofen” was used as internal standard.Linear relationships between values of ratio of peak area of the analyte to peak area of the internal standard and mass concentration of the analyte were obtained in the ranges of 4.1-114.8 mg·L-1 (for oleanolic acid) and 4.3-120.4 mg·L-1 (for ursolic acid).Recovery was tested by standard addition method,values of average recovery of 96.0% were found for the both analytes.The proposed method was used for determination of oleanolic acid and ursolic acid in samples of Fructus corni,giving values of RSD′s (n=6) of 2.03%,2.29%,respectively.