Sui Wenwen, Yang Xiaojing, Yu Wenhong, Jin Yi, Luan Xinyi, Wang Xiangjun, Xu Haiyan
Department of Pharmaceutical Analysis, Pharmacy School, Shenyang Pharmaceutical University, Shenyang 110016, China.
Department of Pharmaceutical Analysis, Pharmacy School, Shenyang Pharmaceutical University, Shenyang 110016, China.
J Pharm Biomed Anal. 2014 Sep;98:228-34. doi: 10.1016/j.jpba.2014.05.034. Epub 2014 May 29.
A rapid and sensitive LC-MS/MS method was developed for the quantification of vilazodone in rat plasma using escitalopram as internal standard. After extracted with organic solvent, post-treatment samples were chromatographed on an Agela C18 column. An isocratic mobile phase of acetonitrile: 5mM ammonium acetate: formic acid (35:65:0.1, v/v/v) was applied at a flow rate of 0.25mL/min. Detection was performed using multiple reaction-monitoring (MRM) modes at m/z 442.4→155.3 for vilazodone and m/z 325.1→109.0 for escitalopram. The method was linear in the concentration range of 1.0-100ng/mL with a correlation coefficient ≥0.993. The intra- and inter-assay precision (%RSD) values were within 13.4%, and intra- and inter-day accuracy (%RE) ranged from -9.8 to 6.9%. The total analysis time was 2.2min. The LC-MS/MS method was fully validated for its sensitivity, selectivity, stability, matrix effect and recovery. The data indicated that the developed method was rapid, specific and sensitive. This method was further and successfully applied in the pharmacokinetics study of vilazodone in rat.
建立了一种快速灵敏的液相色谱-串联质谱法（LC-MS/MS），以艾司西酞普兰为内标定量大鼠血浆中的维拉唑酮。用有机溶剂萃取后，将处理后的样品在艾杰尔C18柱上进行色谱分析。采用乙腈:5mM醋酸铵:甲酸（35:65:0.1，v/v/v）的等度流动相，流速为0.25mL/min。使用多反应监测（MRM）模式进行检测，维拉唑酮的质荷比为m/z 442.4→155.3，艾司西酞普兰的质荷比为m/z 325.1→109.0。该方法在1.0-100ng/mL的浓度范围内呈线性，相关系数≥0.993。批内和批间精密度（%RSD）值在13.4%以内，日内和日间准确度（%RE）范围为-9.8至6.9%。总分析时间为2.2分钟。该LC-MS/MS方法在灵敏度、选择性、稳定性、基质效应和回收率方面得到了充分验证。数据表明所建立的方法快速、特异且灵敏。该方法进一步成功应用于大鼠维拉唑酮的药代动力学研究。
