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