School of Life Science, Beijing Institute of Technology, No.5 Zhongguancun South Street, Beijing 100081, China.
J Pharm Biomed Anal. 2012 Jan 25;58:172-6. doi: 10.1016/j.jpba.2011.09.023. Epub 2011 Oct 1.
A new high-performance liquid chromatography/tandem mass spectrometry (LC-MS/MS) was developed for quantitative analysis of atractylenolide I in rat plasma using buspirone as internal standard (I.S.). Rat plasma samples were deproteined with methanol and acetonitrile (1:1, v/v). Atractylenolide I and I.S. were separated on a Phenomenex Gemini C(18) column (50 mm × 2.0 mm, 5 μm) with gradient mobile phase at the flow rate of 0.4 ml/min. The detection was performed by positive ion electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. The linear calibration curve of atractylenolide I in rat plasma ranged 2.0-5000 ng/ml (R>0.9979). The limit of detection (LOD) and the limit of quantification (LOQ) were 0.6 ng/ml and 2.0 ng/ml, respectively. Both accuracy and precision of the assay were satisfactory. The recoveries of atractylenolide I and I.S. were 91.4% and 87.8%, respectively. This fully validated method was applied to a pharmacokinetic study of atractylenolide I in rats administered with 20 g/kg Atractylodis extract. The main pharmacokinetic parameters T(max) (the time to peak), C(max) (the concentration to peak), T(0.5) (the biological half time), and K(e) (the elimination rate constant) were 0.81 ± 0.11h, 7.99 ± 1.2 ng/ml, 1.94 ± 0.27 h, 0.365 ± 0.06/h, respectively.
建立了一种新的高效液相色谱/串联质谱（LC-MS/MS）方法，用于以丁螺环酮为内标（IS）定量分析大鼠血浆中的苍术内酯 I。大鼠血浆样品用甲醇和乙腈（1:1，v/v）沉淀蛋白。苍术内酯 I 和 IS 在 Phenomenex Gemini C(18)柱（50mm×2.0mm，5μm）上以梯度流动相（流速为 0.4ml/min）分离。检测采用正离子电喷雾电离（ESI）在多重反应监测（MRM）模式下进行。苍术内酯 I 在大鼠血浆中的线性校准曲线范围为 2.0-5000ng/ml（R>0.9979）。检测限（LOD）和定量限（LOQ）分别为 0.6ng/ml 和 2.0ng/ml。该测定方法的准确性和精密度均令人满意。苍术内酯 I 和 IS 的回收率分别为 91.4%和 87.8%。该方法经充分验证后，应用于大鼠灌胃 20g/kg苍术提取物后苍术内酯 I 的药代动力学研究。主要药代动力学参数 T(max)（达峰时间）、C(max)（峰浓度）、T(0.5)（生物半衰期）和 K(e)（消除率常数）分别为 0.81±0.11h、7.99±1.2ng/ml、1.94±0.27h 和 0.365±0.06/h。
