液质联用结合手性固定相法拆分辛弗林对映体

Separation of Synephrine enantiomers by LC-MS/MS combined with chiral stationary phase

建立了液质联用结合手性固定相法拆分辛弗林对映体的方法。考察了流动相的组成、pH值、盐浓度、柱温及质谱检测条件对辛弗林对映体分离的影响。采用资生堂Chiral CD-Ph色谱柱(250mm×4.6mm),流动相为乙腈-10mmol·L^(-1)乙酸铵溶液(8∶92)(甲酸调节pH值至5.0);流速为0.5mL·min^(-1);柱温:40℃;质谱采用电喷雾正离子多反应监测模式,母离子为168.1,子离子为150.2(定量)、135.2。辛弗林对映体在10~1000ng范围内线性关系良好,检出限(S/N=3)为2.5ng。辛弗林对映体能实现基线分离,分离度为2.2。该方法简便、快速,适用于辛弗林对映体的分离。

A method was established for separation of Synephrine enantiomers by LC-MS/MS combined with chiral stationary phase.The effects of mobile phase composition,pH value,salt concentration,column temperature and mass spectrometry detection conditions on the separation of Synephrine enantiomers were investigated.The separation was performed on a Shiseido Chiral CD-Ph column(250mm×4.6mm)with the mobile phase consisting of acetonitrile-10mmol·L^(-1) ammonium acetate solution(pH value adjusted to 5.0 by formic acid)(8:92).The flow rate was 0.5mL·min^(-1).Column temperature:40℃.The mass spectrum was achieved with electrospray positive ion multiple reaction monitoring mode,and the parent ion was 168.1,the daughter ions were 150.2(quantitative)and 135.2.The linear range of each Synephrine enantiomer was 10~1000ng,and the detection limit(S/N=3)was 2.5ng.The enantiomers of Synephrine were completely separated with a resolution of 2.2.This method is simple,rapid and suitable for the separation of Synephrine enantiomers.