高效液相色谱-蒸发光散射检测法测定毛冬青叶中的三萜类化合物和三萜皂苷

HPLC-ELSD determination of triterpenoids and triterpenoid saponins in Ilex pupurea leaves.

作者信息

Xie Jun-bo, Bi Zhi-ming, Li Ping

机构信息

Department of Pharmacognosy, China Pharmaceutical University, Nanjing 210038, China.

出版信息

Yao Xue Xue Bao. 2003 Jul;38(7):534-6.

PMID:14515801

Abstract

AIM

To establish an HPLC-ELSD method for the quantification of pedunculoside, ziyuglycoside I and rutundic acid, in the leaves of Ilex purpurea Hassk.

METHODS

By optimizing the chromatographic conditions of HPLC and the parameters of ELSD to study the methodology. Column: Allsphere ODS-2 (250 mm x 4.6 mm ID, 5 microns), mobile phase: methanol-water (59:41), flow rate: 1.0 mL.min-1, drift tube temperature: 59 degrees C, gas flow rate: 2.38 L.min-1.

RESULTS

The calibration curves were linear in the range of 2.56-25.60 micrograms for pedunculoside, 1.64-16.40 micrograms for ziyuglycoside I and 3.74-37.40 micrograms for rutundic acid. The average recovery of pedunculoside was 96.3%, RSD 1.59% (n = 5), ziyuglycoside I 97.3%, RSD 3.82% (n = 5), rutundic acid 97.7%, RSD 2.11% (n = 5). All of RSDs of the precision were less than 4% (n = 6), and the reproduciblities less than 5% (n = 6).

CONCLUSION

The method is simple, accurate, effective and feasible. It can be used for the determination of the contents of pedunculoside, ziyuglycoside I and rutundic acid in leaf of Ilex purpurea Hassk.

摘要

目的

建立高效液相色谱-蒸发光散射检测法（HPLC-ELSD）测定紫背四季青叶中紫背四季青苷、紫菀苷I和圆叶鼠李酸的含量。

方法

通过优化HPLC色谱条件和ELSD参数研究该方法。色谱柱：Allsphere ODS-2（250 mm×4.6 mm内径，5微米），流动相：甲醇-水（59:41），流速：1.0 mL·min-1，漂移管温度：59℃，气体流速：2.38 L·min-1。

结果

紫背四季青苷在2.56 - 25.60微克范围内、紫菀苷I在1.64 - 16.40微克范围内、圆叶鼠李酸在3.74 - 37.40微克范围内校准曲线呈线性。紫背四季青苷平均回收率为96.3%，相对标准偏差（RSD）为1.59%（n = 5）；紫菀苷I平均回收率为97.3%，RSD为3.82%（n = 5）；圆叶鼠李酸平均回收率为97.7%，RSD为2.11%（n = 5）。精密度的所有RSD均小于4%（n = 6），重现性小于5%（n = 6）。