Department of Analytical Chemistry, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenyang 110016, PR China.
Phytochem Anal. 2011 May-Jun;22(3):225-9. doi: 10.1002/pca.1269. Epub 2010 Nov 2.
Chiisanogenin existing in many Acanthopanax species has been reported to possess anti-inflammatory, antibacterial and antiplatelet aggregatory activities.
To develop and validate a rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry method for the determination of chiisanogenin in rat plasma and to investigate its pharmacokinetics after oral administration of chiisanogenin or the extract of Acanthopanax sessiliflorus fruits.
The sample pretreatment involved a one-step extraction of 0.2 mL plasma with diethyl ether. Acetaminophen was used as the internal standard. The separation was carried out on an ACQUITY UPLC™ BEH C₁₈ column with a mobile phase of acetonitrile-5 mM ammonium acetate (90:10, v/v) at a flow rate of 0.2 mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) mode via electrospray ionization (ESI) source.
A high sample throughput was achieved with an analysis time of 1.1 min per sample. The calibration curve was linear (r² ≥ 0.99) over the concentration range of 5-500 ng/mL with a lower limit of quantification (LLOQ) of 5 ng/mL. The intra-day and inter-day precision (relative standard deviation, R.S.D.) values were below 11% and the accuracy (relative error, R.E.) was within 8% at all three quality control (QC) levels.
The method was successfully applied to the pharmacokinetic study of chiisanogenin in rat after oral administration of chiisanogenin and the extract of Acanthopanax sessiliflorus fruits. Other constituents in the extract affected the pharmacokinetic behavior of chiisanogenin.
在许多刺五加属植物中存在的柴胡皂苷元已被报道具有抗炎、抗菌和抗血小板聚集活性。
建立并验证一种快速灵敏的超高效液相色谱-串联质谱法，用于测定大鼠血浆中的柴胡皂苷元，并考察口服柴胡皂苷元或刺五加果实提取物后柴胡皂苷元的药代动力学。
样品预处理采用一步法，用二乙醚提取 0.2 mL 血浆。对乙酰氨基酚作为内标。采用 ACQUITY UPLC™ BEH C₁₈ 柱，以乙腈-5 mM 乙酸铵（90:10，v/v）为流动相，流速为 0.2 mL/min 进行分离。采用电喷雾电离（ESI）源，通过多反应监测（MRM）模式在三重四极杆串联质谱仪上进行检测。
该方法具有高通量的特点，每个样品的分析时间为 1.1 分钟。在 5-500 ng/mL 的浓度范围内，校准曲线呈线性（r²≥0.99），定量下限（LLOQ）为 5 ng/mL。在所有三个质控（QC）水平下，日内和日间精密度（相对标准偏差，R.S.D.）值均低于 11%，准确度（相对误差，R.E.）均在 8%以内。
该方法成功应用于口服柴胡皂苷元和刺五加果实提取物后大鼠体内柴胡皂苷元的药代动力学研究。提取物中的其他成分影响了柴胡皂苷元的药代动力学行为。
