摘要:
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YMC ODS-C18(250 mm×4.6 mm i.d.;5μm)色谱柱进行分析,以乙腈-0.1%甲酸溶液(15:85 v/v)为流动相,流速为0.6 mL/min,检测波长为254 nm。ESI质谱条件:负离子扫描模式,喷针电压3 500 V,毛细管电压-20 V,干燥气(N2)压力21 psi,扫描范围300-800 amu,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。
Abstract:
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(1585 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-line 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.
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