The Affiliated Wuxi Second Hospital, Nanjing Medical University, Wuxi 214002, Jiangsu Province, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Dec 12;911:34-42. doi: 10.1016/j.jchromb.2012.09.006. Epub 2012 Oct 4.
A new metabolite of taxifolin: 3'-O-methyltaxifolin (3'-O-MTAX) in Caco-2 cells and in rat plasma was identified. The chemical structure of 3'-O-MTAX was determined by MS and (1)H NMR. A rapid, sensitive and specific UPLC-MS method to determine 3'-O-MTAX in rat plasma was also developed. Following ethyl acetate extraction, 3'-O-MTAX in plasma was separated on a Sunfire™ (2.1mm×50mm, 3.5μm) column and analyzed in the selected ion recording with a negative electrospray ionization mode using puerarin as the internal standard. The lower limit of quantification (LLOQ) was 2.75ng/mL. Intra- and inter-day precisions (% RSD) were all within 7.2% and accuracy (% deviation) ranged from -5.0 to 4.7%. The overall recoveries at four concentrations were all >72.0%. This validated method was successfully applied to measure 3'-O-MTAX in rat plasma after oral administration of taxifolin.
在 Caco-2 细胞和大鼠血浆中鉴定出了一种新的杨梅素代谢物：3'-O-甲基杨梅素（3'-O-MTAX）。通过 MS 和 1H NMR 确定了 3'-O-MTAX 的化学结构。还建立了一种快速、灵敏和特异的 UPLC-MS 方法来测定大鼠血浆中的 3'-O-MTAX。在乙酸乙酯提取后，血浆中的 3'-O-MTAX 在 Sunfire™（2.1mm×50mm，3.5μm）柱上分离，并在负离子电喷雾电离模式下采用以葛根素为内标物的选择离子记录进行分析。定量下限（LLOQ）为 2.75ng/mL。日内和日间精密度（%RSD）均在 7.2%以内，准确度（%偏差）在-5.0 至 4.7%之间。四个浓度的总回收率均>72.0%。该经验证的方法成功应用于测定杨梅素灌胃后大鼠血浆中的 3'-O-MTAX。
