摘要
目的:建立用手性固定相拆分帕罗西汀中间体的高效液相色谱方法。方法:用多糖衍生化手性固定相,考察了流动相中异丙醇含量、柱温、流速对对映体分离的影响。采用 Chiralpak AD-H 柱(250mm×4.6mm,5μm),以正己烷-异丙醇-二乙胺(96:4:0.2,v/v)为流动相,流速为0.5mL·min^(-1),检测波长266nm,柱温25℃,拆分帕罗西汀中间体。结果:用 Chiral-pak AD-H 手性柱能完全分离帕罗西汀中间体,分离度达2.45,右旋体先于左旋体出峰。结论:流动相中异丙醇含量增大,显著降低保留时间,而对分离因子影响很小。改变温度(20～35℃)对分离因子和保留时间影响不大。
Objective：To develop a chiral stationary phase - HPLC method for the enantiomeric separation of racemic trans-4 - （4 -fluorpherlyl） -3 -hydroxymethyl - 1 -methylpiperidine, the key intermediate of paroxetine. Method ： Effects of isopropanol modifier concentration in hexane mobile phase, the flow rate and column temperature on the enantiomeric separation paroxetinc intermediate using polysaecharide - based chiral stationary phase were investigated. The enantiomers of paroxetine intermediate were separated on a Chiralpak AD - H column （250 mm× 4.6 mm,5 μm） with a mobile phase consisted of n - hexane isopropanol - diethylamine （96： 4： 0.2, v/v） at a flow rate of 0.5 mL ·min ^-1. The UV detector was set at 266 nm. Results：The enantiomers of paroxetine intermediate were separated successfully on Chiralpak AD - H chiral stationary phase. The （ ＋ ） - enantiomer eluted prior to （- ） one with resolution value being 2.45. Conclusion： Increasing tire content of isopropanol from 2% to 10% by volume,resulted in a dramatical decrease in retention, whereas the change in separation factor was minute. Slight variations in retention and separation factor were observed with temperature increased from 20 to 35 ℃.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2006年第10期1445-1447,共3页
Chinese Journal of Pharmaceutical Analysis
基金
高等学校博士学科点专项科研基金(No.20030335070)
