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,3 μm) 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31。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。 |
关键词: 淫羊藿 化学成分 鉴别 飞行时间质谱法 |
DOI:10.3724/SP.J.1008.2011.0306 |
投稿时间:2011-01-11修订日期:2011-02-22 |
基金项目: |
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RRLC-TOF/MS in rapid identification of 43 chemical constituents of epimedium |
L Lei, ZHANG Hai, ZHAO Liang, JIA Jing, LI Yue-yue, ZHANG Guo-qing* |
(Department of Pharmacy, Eastern Hepatobiliary Surgery Hospital, Second Military Medical University, Shanghai 200438, China) |
Abstract: |
ObjectiveTo use rapid-resolution liquid chromatography-time of flight mass spectrometry (RRLC-TOF/MS) for analyzing the chemical constituents of epimedium. MethodsThe 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. ResultsA total of 43 chemical constituents were identifled from epimedium by RRLC-TOF/MS in one run. ConclusionA 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. |
Key words: Epimedium brevicornum chemical constituents identification time of flight mass spectrometry |