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快速液相-高分辨飞行时间质谱技术鉴别大鼠血中淫羊藿及其代谢产物
吕磊,赵亮,张海,李悦悦,张国庆*
0
(第二军医大学东方肝胆外科医院药材科,上海 200438
*通信作者)
摘要:
目的 运用快速液相-高分辨飞行时间质谱(RRLC-TOF/MS)技术鉴别淫羊藿大鼠给药后的入血成分及代谢产物,以探索淫羊藿可能的药效成分及体内代谢过程。 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(A相)和0.1%甲酸水溶液(B相),梯度洗脱:0~3 min(5%~19%A),3~13 min(19%~32%A),13~25 min(32%~52%A),25~30 min(52%~70%A);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 鉴别出淫羊藿中3种入血成分及4种代谢物。结论 所建方法快捷、有效,可用于淫羊藿体内成分鉴别,为进一步的药效试验提供了参考和依据。
关键词:  淫羊藿  入血成分  代谢产物  飞行时间质谱
DOI:
投稿时间:2013-06-05修订日期:2013-07-01
基金项目:
RRLC-TOF/MS in identification of plasma constituents and metabolites of epimedium in rats after intragastric administration
L Lei,ZHAO Liang,ZHANG Hai,LI Yue-yue,ZHANG Guo-qing*
(Department of Pharmacy, Eastern Hepatobiliary Surgery Hospital, Second Military Medical University, Shanghai 200438, China
*Corresponding author.)
Abstract:
Objective To identify the constituents and metabolites of epimedium in rat plasma by rapid-resolution liquid chromatography-time of flight mass spectrometry (RRLC-TOF/MS) after intragastric administration, so as to explore the active ingredients and metabolites of epimedium in vivo. 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 and acetonitrile was used as gradient elute.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) were applied for qualitative analysis under positive ion mode, with the mass scan range being m/z 100-1 000. Results Three prototype constituents and 4 metabolites of epimedium were identified in rat plasma. Conclusion A rapid and efficient RRLC-TOF/MS method has been established for studying the constituents and metabolites of epimedium in vivo, which provides a reference for further pharmacodynamics experiments.
Key words:  Epimedium brevicornum  prototype constituents  metabolites  time of flight/mass spectrometry