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Rapid stereoselective separations of amphetamine derivatives with highly sulfated gamma-cyclodextrin
Authors:Rudaz Serge  Geiser Laurent  Souverain Sandrine  Prat Josiane  Veuthey Jean-Luc
Affiliation:Laboratory of Pharmaceutical Analytical Chemistry, School of Pharmaceutical Sciences, EPGL, University of Geneva, Geneva, Switzerland. Serge.Rudaz@pharm.unige.ch
Abstract:The highly sulfated gamma-CD (HS-gamma-CD) is a chiral selector widely used in CE for the enantioseparation of pharmaceutical compounds. This paper investigated different approaches to reduce the stereoselective analysis time of amphetamine (AT) derivatives according to the chiral selector concentration in the BGE. With high HS-gamma-CD concentration, tested analytes were separated in 3.5 min as anionic complexes with short-end injection technique in reversed polarity mode. However, this procedure presented some limitations in terms of efficiency and resolution, excessive Joule heating and poor compatibility with MS detection. With low HS-gamma-CD concentration, compounds were separated as cations. Conventional approaches to reduce CE analysis time demonstrated critical resolution between some analytes. Therefore, the use of the partial-filling technique compatible with MS detection was carried out. Under optimized conditions, the analysis time for the chiral separation of seven AT like compounds was reduced to 6 min. Moreover, sensitivity of CE-MS was sufficient for the determination of ATs in plasma following a simple liquid-liquid extraction.
Keywords:Amphetamine  Chiral separation  Highly sulfated‐γ‐cyclodextrin  Mass spectrometry  Plasma
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