State Key Laboratory of Natural and Biomimetic Drugs, School of Pharmaceutical Sciences, Peking University, Beijing 100191, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Sep 1;879(25):2513-8. doi: 10.1016/j.jchromb.2011.07.002. Epub 2011 Jul 18.
A simple, rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for quantifying sibiricaxanthone F (SF) in rat plasma following oral and intravenous dosings. After addition of the internal standard (IS) kaempferol and the antioxidant, 20% ascorbic acid, plasma samples were precipitated with acetonitrile and separated on an Aglient Zorbax XDB-C(18) column (50 mm × 4.6mm I.D., 2.1 μm) with gradient acetonitrile and water (both containing 0.01% formic acid) as the mobile phase. The detection was performed on a Sciex API 4000 LC-MS/MS with electrospray ionization (ESI) inlet in the negative multiple reaction monitoring (MRM) mode. Good linearity was achieved over the concentration range of 0.5-500.0ng/mL (r>0.996). Intra- and inter-day precisions were less than 7.60%, and accuracy ranged from 97.18% to 99.84%. The lower limit of quantification for SF was 0.5 ng/mL, and analytes were stable under various conditions (during freeze-thaw, at room temperature and under deep-freeze conditions). This validated method was successfully applied to the preliminary pharmacokinetic study of SF in rats for the first time, and the absolute bioavailability of SF was found to be only 0.22 ± 0.15%.
建立并验证了一种灵敏、快速的液相色谱-串联质谱（LC-MS/MS）法，用于测定大鼠口服和静脉给予西伯利亚酮 F（SF）后的血浆样品中的含量。加入内标（IS）山柰酚和抗氧化剂 20%抗坏血酸后，用乙腈沉淀血浆样品，在 Aglient Zorbax XDB-C（18）柱（50mm×4.6mm ID，2.1μm）上以梯度乙腈和水（均含 0.01%甲酸）为流动相进行分离。检测采用 Sciex API 4000 LC-MS/MS，以电喷雾电离（ESI）入口在负多重反应监测（MRM）模式下进行。SF 的浓度范围为 0.5-500.0ng/mL 时具有良好的线性（r>0.996）。日内和日间精密度均小于 7.60%，准确度范围为 97.18%-99.84%。SF 的定量下限为 0.5ng/mL，在各种条件下（冻融、室温及深冻条件下）均稳定。该方法首次成功应用于 SF 在大鼠体内的初步药代动力学研究，SF 的绝对生物利用度仅为 0.22±0.15%。
