Sun Hui, Lv Haitao, Zhang Yanmei, Wang Xijun, Bi Kaishun, Cao Hongxin
School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, China.
J Sep Sci. 2007 Dec;30(18):3202-6. doi: 10.1002/jssc.200700251.
Isofraxidin is one of the main bioactive constituents in the root of Acanthopanax senticosus, which has antifatigue, antistress, and immuno-accommondating effects. In this study, an ultraperformance LC (UPLC)-ESI MS method was developed for analyzing isofraxidin and its metabolites in rat plasma. The analysis was performed on a UPLC coupled with ESI MS (quadropole MS tandem TOF MS). The lower LOD (LLOD) for isofraxidin was 0.25 ng/mL, the intraday precision was less than 10%, the interday precision was less than 10%, and the extraction recovery was more than 80%. Isofraxidin and two metabolites (M1 and M2) were detected in rat plasma after oral administration of isofraxidin, and the molecular polarities of M1 and M2 were both increased compared to isofraxidin. The metabolites were identified as 5,6-dihydroxyl-7-methoxycoumarin and 5-hydroxyl-6,7-dimethoxycoumarin when subjected to parent ion spectra, product ion spectra, and extract mass and element composition analyses.
异嗪皮啶是刺五加根中的主要生物活性成分之一,具有抗疲劳、抗应激和免疫调节作用。本研究建立了一种超高效液相色谱(UPLC)-电喷雾电离质谱(ESI MS)方法,用于分析大鼠血浆中的异嗪皮啶及其代谢产物。分析采用UPLC与ESI MS(四极杆质谱串联飞行时间质谱)联用。异嗪皮啶的最低检测限(LLOD)为0.25 ng/mL,日内精密度小于10%,日间精密度小于10%,提取回收率大于80%。口服异嗪皮啶后,在大鼠血浆中检测到异嗪皮啶和两种代谢产物(M1和M2),与异嗪皮啶相比,M1和M2的分子极性均增加。通过母离子光谱、产物离子光谱以及提取质量和元素组成分析,将代谢产物鉴定为5,6-二羟基-7-甲氧基香豆素和5-羟基-6,7-二甲氧基香豆素。