Yang Yimin, Ying Sha, Li Te, Zhen Juan, Chen Dongmei, Wang Jianmeng
Department of Intensive Care Unit, the First Hospital of Jilin University, Changchun, China.
Department of Geriatrics, the First Hospital of Jilin University, Changchun, China.
Biomed Chromatogr. 2018 Aug;32(8):e4259. doi: 10.1002/bmc.4259. Epub 2018 May 10.
A selective and sensitive liquid chromatography tandem mass spectrometry method was developed for the simultaneous determination of salviaflaside and rosmarinic acid in rat plasma. Sample preparation was carried out through liquid-liquid extraction with ethyl acetate using curculigoside as internal standard (IS). The analytes were determined by selected reaction monitoring operated in the positive ESI mode. Chromatographic separation was performed on an Agilent Eclipse Plus C column (100 × 4.6 mm, 1.8 μm) with a mobile phase consisting of methanol-water-formic acid (50:50:0.1, v/v/v) at a flow rate of 0.3 mL/min. The run time was 1.9 min per sample and the injection volume was 5 μL. The method had an LLOQ of 1.6 ng/mL for salviaflaside and 0.94 ng/mL for rosmarinic acid in plasma. The linear calibration curves were fitted over the range of 1.6-320 ng/mL for salviaflaside and 0.94-188 ng/mL for rosmarinic acid in plasma with correlation coefficients (r ) >0.99. Intra- and inter-day precisions (relative standard deviation) were < 13.5%, and accuracies (relative error) were between -8.6% and 14.5% for all quality control samples. The method was validated and applied to the pharmacokinetics of salviaflaside and rosmarinic acid in plasma after oral administration of Prunella vulgaris extract to rats.
建立了一种选择性和灵敏的液相色谱串联质谱法，用于同时测定大鼠血浆中丹酚酸苷和迷迭香酸。样品制备采用以仙茅苷为内标，用乙酸乙酯进行液液萃取。采用正离子电喷雾电离模式下的选择反应监测测定分析物。在安捷伦Eclipse Plus C柱（100×4.6mm，1.8μm）上进行色谱分离，流动相为甲醇-水-甲酸（50:50:0.1，v/v/v），流速为0.3mL/min。每个样品的运行时间为1.9分钟，进样量为5μL。该方法对血浆中丹酚酸苷的定量下限为1.6ng/mL，对迷迭香酸的定量下限为0.94ng/mL。血浆中丹酚酸苷的线性校准曲线在1.6 - 320ng/mL范围内拟合，迷迭香酸的线性校准曲线在0.94 - 188ng/mL范围内拟合，相关系数（r）>0.99。所有质量控制样品的日内和日间精密度（相对标准偏差）<13.5%，准确度（相对误差）在-8.6%至14.5%之间。该方法经过验证，并应用于大鼠口服夏枯草提取物后血浆中丹酚酸苷和迷迭香酸的药代动力学研究。
