首页|液质联用结合手性固定相法拆分辛弗林对映体

液质联用结合手性固定相法拆分辛弗林对映体

扫码查看
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.
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

陈伟康、朱艳艳、刘德鸿、杨毅生、陈希

展开 >

江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,江西 南昌 330029

江西中医药大学,江西 南昌 330004

辛弗林 对映体 拆分 液质联用 固定相拆分

江西省重点研发计划江西省药品监督管理局科研项目

20212BBG730252021KY44

2024

化学工程师
黑龙江省化工研究院

化学工程师

CSTPCD
影响因子:0.243
ISSN:1002-1124
年,卷(期):2024.38(3)
  • 11