化学
色谱法
蛋白质沉淀
选择性反应监测
电喷雾电离
甲酸
药代动力学
三级四极质谱仪
校准曲线
分析物
串联质谱法
质谱法
最大值
高效液相色谱法
电喷雾
检出限
分析化学(期刊)
医学
内科学
作者
Qinghe Zhang,Xi-zhen Li,Han Liu,Pingya Li,Dan Lu
标识
DOI:10.1093/chromsci/bmx097
摘要
A ultra-performance liquid chromatography tandem mass spectrometry method was initially developed and validated for quantification of sophorabioside in rat plasma using kaempferol-3-O-β-D-rutinoside as the internal standard (IS). Analyte and IS were preparation through a protein precipitation procedure with 1.0 mL of methanol to a 0.1 mL plasma sample. The processed samples were separated by C18 analytical column using methanol/water containing 0.1% formic acid with gradient elution as the mobile phase at a flow rate of 0.3 mL/min. Sophorabioside (m/z 577.15 → 269.45) and kaempferol-3-O-β-D-rutinoside (m/z 593.15 → 285.84) were detected by a triple quadrupole tandem mass spectrometer in negative electrospray ionization mode using multiple reaction monitoring. The calibration curve for sophorabioside was linear in the range of 6-1,200 ng/mL (r2 > 0.995) with a lower limit of quantification of 6 ng/mL. The inter- and intra-day precision and accuracy were well within the acceptable limits. The matrix effects were satisfactory in all of the biological matrices examined. The mean recovery of sophorabioside was always >90%. This method was successfully applied to a pharmacokinetic study of sophorabioside in rats after an oral administration of 90 mg/kg sophorabioside. The main pharmacokinetic parameters: Tmax, Cmax and t1/2 were 6.2 ± 0.8 h, 1430.83 ± 183.25 ng/mL, 7.2 ± 0.5 h, respectively.
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