高效液相色谱-蒸发光散射法测定伊犁贝母鳞茎中贝母素乙和贝母素乙-3β-D-葡萄糖苷的含量

[Determination of imperialine and imperialine-3 beta-D-glucoside in bulbs of Fritillaria pallidiflora by HPLC-ELSD].

作者信息

Li S L, Li P, Zheng L J

机构信息

Department of Pharmacognosy, China Pharmaceutical University, Nanjing 210009, China.

出版信息

Yao Xue Xue Bao. 2001 Apr;36(4):300-2.

PMID:12580061

Abstract

AIM

To establish an HPLC (high performance liquid chromatography)-ELSD (evaporative light scattering detector) method for the quantification of chromophore-lacking imperialine (I) and imperialine-3 beta-D-glucoside (II) in bulbs of Fritillaria pallidiflora.

METHODS

By optimizing the chromatographic conditions of HPLC and the parameters of ELSD to test the methodology. Column: Kromasil C-18 (5 microns, 200 mm x 4.6 mm), mobile phase: acetonitrile-water-triethylamine (71:29:0.03), flow rate: 1.0 mL.min-1, drift tube temperature: 88 degrees C, gas flow-rate: 2.38 L.min-1.

RESULTS

The calibration curves were linear in the range of 60.72-161.92 micrograms.mL-1 for I and 48.72-194.88 micrograms.mL-1 for II. The precisions (RSD) of intra-day and inter-day were less than 1% for I and II. The recoveries of the amounts of 24.28, 30.35 and 36.42 micrograms for I were 97.1%, 96.6% and 96.8%, and 24.20, 30.24 and 36.29 micrograms for II were 95.8%, 96.9% and 96.0%. The minimal detectable concentrations of I and II were 2.43 and 1.53 micrograms.mL-1 respectively.

CONCLUSION

The established method is simple, rapid, accurate and sensitive, and can be utilized to determine the contents of imperialine and imperialine-3 beta-D-glucoside in crude drug Yibeimu (derived from the bulbs of Fritillaria pallidiflora).

摘要

目的

建立一种高效液相色谱-蒸发光散射检测器（HPLC-ELSD）法，用于定量测定暗紫贝母鳞茎中无色花贝母碱（I）和贝母素乙-3β-D-葡萄糖苷（II）的含量。

方法

通过优化HPLC的色谱条件和ELSD的参数来检测该方法。色谱柱：Kromasil C-18（5μm，200mm×4.6mm），流动相：乙腈-水-三乙胺（71:29:0.03），流速：1.0mL·min-1，漂移管温度：88℃，气体流速：2.38L·min-1。

结果

I的校准曲线在60.72-161.92μg·mL-1范围内呈线性，II的校准曲线在48.72-194.88μg·mL-1范围内呈线性。I和II的日内和日间精密度（RSD）均小于1%。I分别加入24.28、30.35和36.42μg时的回收率为97.1%、96.6%和96.8%，II分别加入24.20、30.24和36.29μg时的回收率为95.8%、96.9%和96.0%。I和II的最低检测浓度分别为2.43和1.53μg·mL-1。