UPLC-MS/MS法测定大鼠肝微粒体中26-OH-PD的含量  

Determination of 26-OH-PD in Rat Liver Microsome Incubation Solution by UPLC-MS / MS

作　　者：林美妤[1] 李平亚[1] 高红梅[1,2] 韩柳[1] 刘海燕[1] 刘金平[1] 

机构地区：[1]吉林大学药学院,长春130021 [2]长春中医药大学,长春130021

出　　处：《特产研究》2015年第1期43-46,57,共5页Special Wild Economic Animal and Plant Research

基　　金：吉林大学研究生创新研究计划资助项目(2014115)

摘　　要：建立测定大鼠肝微粒体孵育液中26-OH-人参二醇(26-OH-PD)含量的方法。肝微粒体孵育液样品处理采用蛋白沉淀法,利用超高效液相色谱-电喷雾串联质谱法,样品以V(甲醇)∶V(水)(10mmol/L乙酸铵-0.1%甲酸)=83∶17为流动相进行分离,以多反应离子监测方式进行定量分析,用于监测的离子为m/z 477.4→143.1(26-OH-PD),477.4→143.1(内标PDQ)。2.5min内完成26-OH-PD的检测,工作曲线线性范围为0.02μmol/L^4μmol/L,日内、日间精密度分别小于4.49%、7.00%,平均回收率为93.9%~96.8%,稳定性的RSD小于8.83%。本方法专属性强、灵敏度高且快速,可以用于肝微粒体孵育液样品中26-OH-PD的检测。A method was established for the content determination of 26- OH- PD in rat liver microsome incubation solution. Ultra- perfor- mance liquid chromatography coupled with tandem mass spectrometry（UPLC - MS/MS） was developed for the detection of 26- OH- PD in rat liver microsome incubation solution. Pre - treatment of the sample involved a single protein precipitation step. The extracts were separated by U- PIE using methanol： 10mmol/L ammonium acetate - 0.1% formic acid in water（83 ： 17） as mobile phase. Multiple reaction monitoring（ MRM ） mode with the transition of m/z 477.4-143.1（26- OH- PD） ,477.4-143. I（PDQ,I.S. ）was used for quantitative analysis.The determina- tion of 26 - OH - PD was completed within 2.5min. The linear range of 26 - OH - PD was 0.02tanol/L- 4tanol/L with average recovery of 93.9 % - 96.8 %. The RSD of intra - day and inter - day were lower than 4.49 % and 7.00%. The RSD of stability was lower than 8.83 %. The method is sensitive,accurate and rapid for the determination of 26- OH- PD in rat liver microsome incubation solution.

关 键 词：26-OH-人参二醇 超高效液相色谱-电喷雾串联质谱法 肝微粒体孵育液 大鼠 

分 类 号：Q503[生物学—生物化学]