Yang Shenbao, Qu Ruiying, Zhu Zhe, Li Wei, Zhao Chengliang, Li Liantai
Jiaozhou People's Hospital, Qingdao, China.
Hand and Foot Surgery and Reparative and Reconstruction Surgery Center, Department of Orthopaedics, the Second Hospital of Jilin University, Changchun, China.
Biomed Chromatogr. 2018 Aug;32(8):e4241. doi: 10.1002/bmc.4241. Epub 2018 Apr 17.
A sensitive and rapid LC-MS/MS method was developed and validated for quantitation of sciadopitysin in rat plasma using amentoflavone as an internal standard. Sample processing was accomplished after deproteinization with 150 μL aliquot of acetonitrile. Chromatographic separation was achieved using an Agela C column with an isocratic mobile phase comprising 2 mm ammonium acetate-acetonitrile (35:65, v/v) at a flow rate of 0.4 mL/min. Detection was performed by selection reaction monitoring on a triple-quadrupole mass spectrometer following the transitions m/z 579 → 547 and 537 → 375 for sciadopitysin and internal standard, respectively, in the negative ionization mode. The calibration curve was linear from 2.90 to 1160 ng/mL for sciadopitysin. Intra- and inter-day precisions were in the ranges 4.1-11.4 and 5.7-9.1% for sciadopitysin. Sciadopitysin was stable under different stability conditions. The validated assay was applied to pharmacokinetic and bioavailability studies in rats.
建立了一种灵敏、快速的液相色谱-串联质谱(LC-MS/MS)方法,并以穗花杉双黄酮为内标,对大鼠血浆中的穗花杉双黄酮进行定量分析。用150μL乙腈等分试样进行脱蛋白处理后完成样品处理。采用Agela C柱,以含2mM醋酸铵-乙腈(35:65,v/v)的等度流动相,流速为0.4mL/min进行色谱分离。在负电离模式下,通过三重四极杆质谱仪上的选择反应监测进行检测,穗花杉双黄酮和内标的跃迁分别为m/z 579→547和537→375。穗花杉双黄酮的校准曲线在2.90至1160ng/mL范围内呈线性。穗花杉双黄酮的日内和日间精密度分别在4.1-11.4%和5.7-9.1%范围内。穗花杉双黄酮在不同稳定性条件下均稳定。该验证方法应用于大鼠的药代动力学和生物利用度研究。