Yan Han, Sun Yuanyuan, Zhang Qili, Yang Mingjing, Wang Xiaorui, Wang Yang, Yu Zhiguo, Zhao Yunli
School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenhe District, Shenyang 110016, China.
School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenhe District, Shenyang 110016, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Jul 1;993-994:86-92. doi: 10.1016/j.jchromb.2015.05.006. Epub 2015 May 14.
A simple and rapid ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of Atractylenolide I, II and III in rat plasma. Plasma samples were processed by liquid-liquid extraction with ethyl acetate, using schisandrin as internal standard (IS). Chromatographic separation was accomplished on a Thermo Hypersil GOLD C18 column (2.1mm×50mm, 1.9μm) with mobile phase consisting of acetonitrile and 0.1% formic acid-water (50:50, v/v). The detection was carried out by ESI-MS (positive ionization mode) and low-energy collision dissociation tandem mass spectrometric analyses using the multiple-reaction monitoring (MRM) scan mode. The quantification was performed using the transitions of the protonated molecule→product ion at m/z 231.0→185.1 for Atractylenolide I, at m/z 233.1→187.1 for Atractylenolide II and at m/z 249.1→231.1 for Atractylenolide III, respectively. Method validation revealed excellent linearity over investigated range together with satisfactory intra- and inter-day precision, accuracy, matrix effects and extraction recoveries. This method was successfully applied to the comparative pharmacokinetic study of Atractylenolide I, II and III in rat plasma after intragastric administration of Baizhufuling extract and Atractylodis extract.
建立了一种简单快速的超高效液相色谱-串联质谱法(UPLC-MS/MS),用于同时测定大鼠血浆中白术内酯I、II和III的含量。血浆样品采用乙酸乙酯液-液萃取法处理,以五味子醇甲作为内标(IS)。色谱分离在Thermo Hypersil GOLD C18柱(2.1mm×50mm,1.9μm)上进行,流动相由乙腈和0.1%甲酸-水(50:50,v/v)组成。采用电喷雾电离质谱(ESI-MS,正离子模式)和低能碰撞解离串联质谱分析,以多反应监测(MRM)扫描模式进行检测。分别采用白术内酯I的质子化分子→产物离子m/z 231.0→185.1、白术内酯II的m/z 233.1→187.1以及白术内酯III的m/z 249.1→231.1进行定量分析。方法验证表明,在所研究的范围内具有良好的线性,同时日内和日间精密度、准确度、基质效应和提取回收率均令人满意。该方法成功应用于大鼠灌胃给予白术茯苓提取物和苍术提取物后,白术内酯I、II和III在大鼠血浆中的比较药代动力学研究。