Song Yingshi, Yan Huiyu, Xu Jingbo, Ma Hongxi
Department of Pharmacy, the First Hospital of Jilin University, Changchun, People's Republic of China.
Department of Pathology, the First Hospital of Jilin University, Changchun, People's Republic of China.
Biomed Chromatogr. 2017 Sep;31(9). doi: 10.1002/bmc.3948. Epub 2017 Feb 27.
A rapid and sensitive liquid chromatography tandem mass spectrometry detection using selected reaction monitoring in positive ionization mode was developed and validated for the quantification of nodakenin in rat plasma and brain. Pareruptorin A was used as internal standard. A single step liquid-liquid extraction was used for plasma and brain sample preparation. The method was validated with respect to selectivity, precision, accuracy, linearity, limit of quantification, recovery, matrix effect and stability. Lower limit of quantification of nodakenin was 2.0 ng/mL in plasma and brain tissue homogenates. Linear calibration curves were obtained over concentration ranges of 2.0-1000 ng/mL in plasma and brain tissue homogenates for nodakenin. Intra-day and inter-day precisions (relative standard deviation, RSD) were <15% in both biological media. This assay was successfully applied to plasma and brain pharmacokinetic studies of nodakenin in rats after intravenous administration.
建立了一种在正离子模式下使用选择反应监测的快速灵敏的液相色谱串联质谱检测方法,并对其进行了验证,用于定量大鼠血浆和脑中的紫花前胡苷。异前胡素A用作内标。采用一步液液萃取法制备血浆和脑样品。该方法在选择性、精密度、准确度、线性、定量限、回收率、基质效应和稳定性方面进行了验证。血浆和脑组织匀浆中紫花前胡苷的定量下限为2.0 ng/mL。在血浆和脑组织匀浆中,紫花前胡苷在2.0 - 1000 ng/mL的浓度范围内获得了线性校准曲线。在两种生物介质中,日内和日间精密度(相对标准偏差,RSD)均<15%。该方法成功应用于大鼠静脉注射后紫花前胡苷的血浆和脑药代动力学研究。