Application of a sensitive and specific LC-MS/MS method for determination of wilforine from Tripterygium wilfordii Hook. F. in rat plasma for a bioavailability study.
Application of a sensitive and specific LC-MS/MS method for determination of wilforine from Tripterygium wilfordii Hook. F. in rat plasma for a bioavailability study.
复制标题
DOI：
10.1002/bmc.3390
复制
发表时间：
2015-07
期刊：
影响因子：
--
通讯作者：
Mengxiang Su;Min Song;Bin Di;T. Hang
中科院分区：
文献类型：
--
作者：
Mengxiang Su;Min Song;Bin Di;T. Hang
建立了一种高选择性、高特异性的LC-MS/MS测定大鼠血浆中wilforine的方法。采用甲基叔丁基醚液-液萃取法，以bulleyaciniine A为内标（IS）从血浆基质中分离分析物。在Sepax GP-Phenyl色谱柱上进行分析，流动相为甲醇与含0.1%甲酸（75:25,v/v）的10 mmol/L甲酸铵缓冲溶液的混合物，泵送流速为1.0 mL/min。采用三重四极杆质谱仪进行多重选择反应监测，母体到产物的定量器跃迁为[M + H](+) M /z， wilforine为867.6→206.0，IS为664.1→584.1。该方法的主要优点是灵敏度高（定量下限为0.02 ng/mL），样品量少（每个样品0.1 mL血浆）。结果表明，该方法在0.02 ~ 100 ng/mL的线性范围内具有良好的准确度和精密度，并成功应用于大鼠静脉和口服给药后威福林的生物利用度研究。据估计，大鼠口服wilforine的绝对生物利用度为84%。
A highly selective and specific LC-MS/MS method was developed and validated for the determination of wilforine in rat plasma. The analyte was separated from plasma matrix by using methyl tertiary butyl ether liquid-liquid extraction with bulleyacinitine A as internal standard (IS). The analysis was carried out on a Sepax GP-Phenyl column using a mixture of methanol and 10 mmol/L ammonium formate buffer solution containing 0.1% formic acid (75:25, v/v) as the mobile phase pumped at a flow rate of 1.0 mL/min. The detection was operated using a triple-quadrupole mass spectrometer in multiple selected reaction monitoring with the parent-to-product quantifier transitions [M + H](+) m/z 867.6 →206.0 for wilforine and 664.1 →584.1 for IS. The main advantage of this method was the high sensitivity (a lower limit of quantification of 0.02 ng/mL) and the small amount of sample (0.1 mL plasma per sample). The method was fully validated to be accurate and precise with a linear range of 0.02-100 ng/mL, and successfully applied to a bioavailability study of wilforine in rats after intravenous and oral administration. The oral absolute bioavailability of wilforine in rats was estimated to be 84%.