RRLC-TOF/MS快速鉴别中药淫羊藿中43种化学成分

RRLC-TOF/MS in rapid identification of 43 chemical constituents of epimedium

目的运用快速液相-高分辨飞行时间质谱(RRLC-TOF/MS)技术对中药淫羊藿化学成分进行快速鉴别。方法色谱分离采用SHISEIDO MG C18(3.0 mm×100 mm,3μm)色谱柱;流动相为乙腈和0.1%甲酸水溶液,梯度洗脱,A相比例随时间的变化:5%～19%(0～3 min),19%～32%(3～13 min),32%～52%(13～25 min),52%～70%(25～30 min);柱温25℃;流速0.6 ml/min,柱后分流比为3∶1。质谱定性采用飞行时间质谱,电喷雾离子源(ESI),正离子模式,质量数扫描范围m/z 100～1 000。结果一次性鉴别出淫羊藿中43种的化学成分。结论建立了一种基于RRLC-TOF/MS技术对淫羊藿中的化学成分进行快速鉴别的方法,为中药淫羊藿的质量控制及体内的深入研究奠定了基础。

Objective To use rapid-resolution liquid chromatography-time of flight mass spectrometry（RRLC-TOF/MS） for analyzing the chemical constituents of epimedium.Methods The separation was performed on a SHISEIDO MG C18 reverse phase column（3.0 mm×100 mm,3 μm）.The mobile phase consisted of water containing 0.1% formic acid;acetonitrile was used as gradient elute.The gradient of A phase was as following： 5%-19%（0-3 min）,19%-32%（3-13 min）,32%-52%（13-25 min）,and 52%-70%（25-30 min）.The flow rate was 0.6 ml/min,post-column split ratio was 31,and the temperature of column was 25℃.Time-of-flight mass spectrometer（TOF/MS） and electrospray ion source（ESI） was applied for qualitative analysis under the positive ion mode,and mass scan range was m/z 100-1 000.Results A total of 43 chemical constituents were identifled from epimedium by RRLC-TOF/MS in one run.Conclusion A rapid and efficient RRLC-TOF/MS approach for identifying the chemical constituents of epimedium has been successfully established,which paves a way for quality control and further in vivo studies of epimedium.