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Online sample concentration in partial-filling chiral electrokinetic chromatography - mass spectrometry


Wuethrich, A and Haddad, PR and Quirino, JP, Online sample concentration in partial-filling chiral electrokinetic chromatography - mass spectrometry, Chirality, 26, (11) pp. 734-738. ISSN 0899-0042 (2014) [Refereed Article]

Copyright Statement

Copyright 2013 Wiley Online

DOI: doi:10.1002/chir.22257


The concentration sensitivity of a racemic drug (chlorpheniramine maleate) in chiral capillary electrophoresis with electrospray ionization mass spectrometric detection was improved ~500-fold via stacking. Enantiomeric separation was achieved through the use of a neutral chiral pseudostationary phase (2-hydroxpropyl-β-cyclodextrin), untreated fused-silica capillaries, and the application of a partial-filling technique to prevent the pseudostationary phase from entering the detector. A concentration factor of 50 resulted from field-enhanced sample injection (FESI). However, the higher concentration factor was achieved by combining FESI with micelle-to-solvent stacking (MSS) to increase sample load and focus the analyte band. MSS was achieved by injection of an ammonium lauryl sulfate micellar plug prior to sample injection. The sample diluent was a 20-fold dilution of the background electrolyte (50 mM ammonium acetate, pH 3.5) with 60% acetonitrile. This methodology provided a limit of detection (LOD) of as low as 5 ng/ml of the racemate.

Item Details

Item Type:Refereed Article
Keywords:capillary electrophoresis, chlorpheniramine, enantiomeric separation, field-enhanced sample injection, micelle to solvent stacking
Research Division:Chemical Sciences
Research Group:Analytical chemistry
Research Field:Analytical spectrometry
Objective Division:Expanding Knowledge
Objective Group:Expanding knowledge
Objective Field:Expanding knowledge in the chemical sciences
UTAS Author:Wuethrich, A (Mr Alain Wuethrich)
UTAS Author:Haddad, PR (Professor Paul Haddad)
UTAS Author:Quirino, JP (Associate Professor Lito Quirino)
ID Code:91881
Year Published:2014 (online first 2013)
Web of Science® Times Cited:20
Deposited By:Austn Centre for Research in Separation Science
Deposited On:2014-06-02
Last Modified:2016-11-17

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