山楂叶化学成分的HPLC-DAD/ESI-MS分析

目的：通过液相色谱-二极管阵列光谱检测／电喷雾离子化质谱（HPLC—DAD／ESI—MS）联用技术定性分析山楂叶中的主要化学成分。方法：以60％乙醇回流提取山楂叶原药材，再经D101大孔吸附树脂纯化。高效液相色谱条件：使用YMCODS—C18（250mm×4．6mmi．d．；5μm）色谱柱进行分析，以乙腈-0．1％甲酸溶液（15：85v／v）为流动相，流速为0．6mL／min，检测波长为254nm。ESI质谱条件：负离子扫描模式，喷针电压3500V，毛细管电压-20V，干燥气（N2）压力21psi，扫描范围300—800amu，雾化温度300℃。结果：通过液-质联用技术以及紫外扫描，鉴定出山楂叶中11个主要化学成分。结论：通过HPLC-DAD／ESI-MS联用技术，为鉴定山楂叶中的化学成分建立起了一种快速、高效的分析方法。

Analysis on chemical constituents of hawthorn leaves by HPLC-DAD/ESI-MS

Objective： To analyze the chemical constituents of hawthorn leaves by high-performance liquid chromatography （HPLC）-diode array detector/electrospray ionization-mass spectrometry （HPLC-DAD/ESI-MS）. Methods： Dried hawthorn leaves were extracted under reflux with 60% ethanol and purified by D101 macroporous resin again. The chromatographic separation was performed on a YMC ODS-C18 column （250 mm ×4.6 mm i. d. ;5 μm） with a mobile phase composed of aceonitrile-0.1% formic acid （15 ： 85 v/v） ,eluted at a flow rate of 0.6 mL/min, and UV detection was set at 254 nm. The negative ionization mode with needle voltage 3 500 V, capillary voltage -20V, gas （ N2 ） press 21 psi and temperature of the capillary 300 ℃ was selected. Relative molecular mass data acquisition was performed from m/z 300 to 800 in full MS scan mode. Results ： Eleven of the major chemical constituents of hawthorn leaves were characterized based on their retention behavior obtained on-llne by their UV spectra and the HPLC-DAD/ESI-MS. Conclusion：A rapid and efficient method for studying the chemical constituents of hawthorn leaves by HPLC-DAD/ESI-MS was established.