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作 者:吕磊[1] 张海[1] 赵亮[1] 贾静[1] 李悦悦[1] 张国庆[1]
机构地区:[1]第二军医大学东方肝胆外科医院药材科,上海200438
出 处:《第二军医大学学报》2011年第3期306-310,共5页Academic Journal of Second Military Medical University
摘 要: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 31,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.
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