School of Life Science, Beijing Institute of Technology, China.
Anal Bioanal Chem. 2011 May;400(4):1181-7. doi: 10.1007/s00216-011-4868-8. Epub 2011 Mar 24.
A simple HPLC-MS/MS method for simultaneous determination of loureirin A and loureirin B in rat urine, feces, and bile after oral administration of 10.6 g/kg of longxuejie (one rare traditional Chinese medicinal herb) was developed for the first time. The analytes and buspirone (internal standard) were separated on a C(5) column with acetonitrile-water (containing 0.1% formic acid) as mobile phase at a flow rate of 0.4 min/mL. The detector was a Q-trap™ mass spectrometer with an electrospray ionization interface operating in the multiple reaction monitoring mode. Calibration curves of loureirin A in rat urine, feces, and bile were linear over the concentration range of 1.00-5,000 ng/mL. Loureirin B in rat urine, feces, and bile ranged between 0.08 and 20, 0.20 and 20, and 0.10 and 500 ng/mL, respectively. Validation revealed that the method was specific, accurate, and precise. The fully validated method was applied to the excretion study of loureirin A and loureirin B in rats. After oral administration of 10.6 g/kg longxuejie, cumulative excretion amount of loureirin A and loureirin B in rat urine were 2.94 ± 0.81 and 0.36 ± 0.16 μg at 72 h, respectively. Of the total dose, 5.35% of loureirin A and 5.46% of loureirin B were excreted from feces at 60 h. The cumulative amounts of loureirin A and loureirin B in rat bile reached 4.49 ± 0.98 and 5.11 ± 0.83 μg, respectively, at 36 h after dosing, accounting for 0.054% and 0.056% of the total dose.
首次建立了一种简单的 HPLC-MS/MS 方法，用于同时测定口服 10.6 g/kg 龙血竭（一种珍稀中药）后大鼠尿、粪和胆汁中的 loureirin A 和 loureirin B。采用 C(5)柱，以乙腈-水（含 0.1%甲酸）为流动相，流速为 0.4 min/mL，对分析物和丁螺环酮（内标）进行分离。检测采用电喷雾电离接口的 Q-trap™质谱仪，在多反应监测模式下进行检测。loureirin A 在大鼠尿、粪和胆汁中的校准曲线在 1.00-5,000 ng/mL 浓度范围内呈线性。loureirin B 在大鼠尿、粪和胆汁中的浓度范围分别为 0.08-20、0.20-20 和 0.10-500 ng/mL。验证结果表明，该方法具有特异性、准确性和精密度。该完全验证的方法应用于大鼠中 loureirin A 和 loureirin B 的排泄研究。口服 10.6 g/kg 龙血竭后，大鼠尿液中 loureirin A 和 loureirin B 的累积排泄量分别在 72 h 时达到 2.94 ± 0.81 和 0.36 ± 0.16 μg。在 60 h 时，粪便中 5.35%的 loureirin A 和 5.46%的 loureirin B 被排泄。在给药后 36 h，大鼠胆汁中 loureirin A 和 loureirin B 的累积量分别达到 4.49 ± 0.98 和 5.11 ± 0.83 μg，分别占总剂量的 0.054%和 0.056%。
