Chen Minting, Wei Suying, Luo Chaohua, Chen Feilong, Song Shuai, Shen Qun, Mo Zhixian, Wei Fenghuan
College of Traditional Chinese Medicine, Southern Medical University, Guangzhou, China.
Department of Chemistry and Biochemistry, Lamar University, Beaumont, Texas, USA.
Biomed Chromatogr. 2017 Oct;31(10). doi: 10.1002/bmc.3966. Epub 2017 Apr 19.
Wogonin and oroxylin A in Scutellariae Radix, schisandrin in Chinensis Fructus, paeoniflorin in Moutan Cortex and emodin in Polygoni Cuspidate Rhizome et Radix are anti-inflammatory active compounds. A method for simultaneous determination of the five compounds in rat was developed and validated using high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS). The separation was performed on a Symmetry C column (4.6 × 50 mm, 3.5 μm) with acetonitrile and 0.1% formic acid aqueous solution as the mobile phases. The detection was performed using multiple-reaction monitoring with electrospray ionization source in positive-negative ion mode. The calibration curves showed good linearity (r ≥ 0.9955). The lower limit of quantification (LLOQ) was 5 ng/mL for wogonin and schisandrin, 10 ng/mL for oroxylin A and emodin, and 15 ng/mL for paeoniflorin, respectively. The relative standard deviations of intraday and interday precisions were <11.49 and 14.28%, respectively. The extraction recoveries and matrix effects were acceptable. The analytes were stable under the experiment conditions. The validated method has been successfully applied to pharmacokinetic studies of the five compounds in rats after oral administration of Hu-gan-kan-kang-yuan capsule. This paper would be a valuable reference for pharmacokinetic studies of Chinese medicine preparations containing the five compounds.
黄芩中的汉黄芩素和木犀草素、五味子中的五味子醇甲、牡丹皮中的芍药苷以及虎杖中的大黄素均为具有抗炎活性的化合物。本文建立了一种采用高效液相色谱-串联质谱法（HPLC-MS/MS）同时测定大鼠体内这5种化合物的方法并进行了方法学验证。采用Symmetry C色谱柱（4.6×50 mm，3.5μm），以乙腈和0.1%甲酸水溶液为流动相进行分离。采用电喷雾电离源，在正、负离子模式下进行多反应监测检测。校准曲线显示出良好的线性关系（r≥0.9955）。汉黄芩素和五味子醇甲的定量下限（LLOQ）均为5 ng/mL，木犀草素和大黄素的LLOQ为10 ng/mL，芍药苷的LLOQ为15 ng/mL。日内和日间精密度的相对标准偏差分别<11.49%和14.28%。提取回收率和基质效应均可接受。在实验条件下，分析物是稳定的。该验证方法已成功应用于大鼠口服护肝抗康源胶囊后这5种化合物的药代动力学研究。本文将为含这5种化合物的中药制剂的药代动力学研究提供有价值的参考。
