Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences, Peking Union Medical College, Beijing 100193, China.
J Pharm Biomed Anal. 2012 Nov;70:539-43. doi: 10.1016/j.jpba.2012.05.002. Epub 2012 May 15.
A sensitive and accurate LC-ESI-MS/MS method was developed and validated of for the determination of 6'-hydroxy justicidin A (HJA), a potential antitumor active component isolated from Justicia procumbens in rat plasma using a simple liquid-liquid extraction (LLE) method for sample preparation. Chromatographic separation was achieved on an Agilent Zorbax-C(18) column (2.1 mm × 50 mm, 3.5 μm) using a step gradient program with the mobile phase of 0.1% formic acid aqueous solution and acetonitrile with 0.1% formic acid. HJA and IS (buspirone) were detected using electrospray positive ionization mass spectrometry in the multiple reaction monitoring (MRM) mode. This method demonstrated good linearity and did not show any endogenous interference with the active compound and IS peaks. The lower limit of quantification (LLOQ) of HJA was 0.50 ng/ml in 50 μl rat plasma. The developed and validated method has been successfully applied to the quantification and pharmacokinetic study of HJA in rats after intravenous and oral administration of 0.25 mg/kg HJA. The oral bioavailability (F) of HJA was estimated to be 36.0±13.4% with an elimination half-life (t(1/2)) value of 1.04±0.20 h.
建立并验证了一种灵敏、准确的 LC-ESI-MS/MS 方法，用于测定大鼠血浆中来源于直立金粟兰的潜在抗肿瘤活性成分 6'-羟基汉黄芩素（HJA）。样品制备采用简单的液液萃取（LLE）方法。采用 Agilent Zorbax-C18 柱（2.1mm×50mm，3.5μm）进行色谱分离，流动相为 0.1%甲酸水溶液和含 0.1%甲酸的乙腈，采用梯度洗脱程序。HJA 和内标（丁螺环酮）采用电喷雾正离子化质谱，在多重反应监测（MRM）模式下进行检测。该方法具有良好的线性，无内源性物质和活性化合物与内标峰的干扰。在 50μl 大鼠血浆中，HJA 的定量下限（LLOQ）为 0.50ng/ml。该方法已成功应用于 0.25mg/kg HJA 静脉和口服给药后大鼠体内 HJA 的定量和药代动力学研究。HJA 的口服生物利用度（F）估计为 36.0±13.4%，消除半衰期（t1/2）值为 1.04±0.20h。
