Enantioseparation and Determination of β-Blocker Enantiomers in Human Plasma by Cyclodextrin-bonded Phase by HPLC
In this paper,a new type of bridged bis-β-cyclodextrin stationary phase was used to improve the separation selectivity by making full use of its multiple recognition effects such as synergistic inclusion.By optimizing the chromatographic conditions,six enantiomers of common β-blockers(carvedilol,arotinolol and atenolol)were completely separated,and the resolutions were 1.6,1.9 and 1.7 respectively.A new HPLC method for simultaneous resolution and determination of the above six enantiomers in human plasma was established with R-aproprolol as internal standard.The alkalized plasma samples were extracted and purified with ethyl acetate,and the polar organic mobile phase(ACN/MeOH/TEA/HOAc)was selected.The enantiomers were completely separated by gradient elution,detected by a diode-array detector at 275 nm,and quantified by an internal standard method.The experimental results showed that the six enantiomers of β-blockers had good linear relationship with R2 of 0.9923-0.9989 within their respective mass concentration ranges.The detection limit(LOD)and quantitative limit(LOQ)of all enantiomers were in the range of 0.4-1.5 mg/L and 1.5-4.0 mg/L,respectively.The average recoveries from plasma samples were 85.96％-103.88％.The RSDs of the determination results were 1.88％-3.29％for intra-day and 3.02-5.17 for inter-day,respectively.This method has the advantages of simple operation,high recoveries,good accuracy and resolution.Simultaneous determination of multiple enantiomers can save analysis time,improve analysis efficiency and reduce test cost.
β-BlockersBridged bis-β-cyclodextrin CSP for HPLCChiral resolutionEnantiomeric quantificationHuman plasma
NETL
NSTL
万方数据
