高效液相色谱-蒸发光散射检测法测定海南冬青叶中三对三萜类异构体

[Determination of three pair of triterpenoid isomers in leaf of Ilex hainanensis by HPLC-ELSD].

作者信息

Liu Zong-Yang, Zhao Wen-Wen, Wu Jing-Yue, Wu Xia, Chen Xiao-Qing, Zan Ke

机构信息

Beijing Key Laboratory of Traditional Chinese Medicine Collateral Disease Theory Research, School of Traditional Chinese Medicine, Capital Medical University, Beijing 100069, China.

National Institutes for Food and Drug Control, Beijing 100050, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2018 Apr;43(8):1662-1666. doi: 10.19540/j.cnki.cjcmm.20180115.015.

DOI:10.19540/j.cnki.cjcmm.20180115.015

PMID:29751714

Abstract

The present study is to develop an HPLC-ELSD method for simultaneous determination of three pairs of triterpenoid isomers, Ilexsaponin A₁, Ilexhainanoside D, Ilexgenin A, 3β, 19α-dihydroxyolean-12-ene-24, 28-dioic acid (ilexhainanin E) ursolic acid and oleanic acid in the leaf of Ilex hainanensis, which could provide evidence to the quality control of this herb. The six constituents were measured on a Waters XBridge C₁₈ column (4.6 mm×250 mm, 5 μm), with a mobile phase consisting of methanol (A)- 0.5% formic acid in water (B) at a flow rate of 1.0 mL·min⁻¹ (0-18 min，70%-85% A，18-20 min，85%-95% A；20-35 min，95% A). The carrier gas was N₂, and the pressure was 2.8 L·min⁻¹. The drift tube in this experiment were set at 70 °C. The injection volume was 10 μL. The contents of the six triterpenoids in 6 samples were 3.7-8.5, 10.3 -22.1, 2.8-5.9, 7.8-14.1, 2.6-3.8 and 8.8-11.9 mg·g⁻¹, respectively. The established method is proved to be accurate and sensitive for the determination of triterpenoids in Ilicis Hainanensis Folium, and may be used for the quality improvement of this herb.

摘要

本研究旨在建立一种高效液相色谱-蒸发光散射检测法（HPLC-ELSD），用于同时测定海南冬青叶中三对三萜类异构体，即冬青皂苷A₁、海南冬青苷D、冬青苷元A、3β,19α-二羟基齐墩果-12-烯-24,28-二酸（海南冬青素E）、熊果酸和齐墩果酸，为该药材的质量控制提供依据。六种成分在Waters XBridge C₁₈柱（4.6 mm×250 mm，5 μm）上进行测定，流动相为甲醇（A）-0.5%甲酸水溶液（B），流速为1.0 mL·min⁻¹（0 - 18 min，70% - 85% A；18 - 20 min，85% - 95% A；20 - 35 min，95% A）。载气为N₂，压力为2.8 L·min⁻¹。本实验中漂移管温度设定为70℃。进样量为10 μL。6个样品中六种三萜类成分的含量分别为3.7 - 8.5、10.3 - 22.1、2.8 - 5.9、7.8 - 14.1、2.6 - 3.8和8.8 - 11.9 mg·g⁻¹。所建立的方法被证明对海南冬青叶中三萜类成分的测定准确且灵敏，可用于该药材的质量提升。