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Simultaneous electrophoretic concentration and separation of herbicides in beer prior to stacking capillary electrophoresis UV and liquid chromatography–mass spectrometry

Wuethrich, Alain, Haddad, Paul R., Quirino, Joselito P.
Electrophoresis 2016 v.37 no.9 pp. 1122-1128
beers, capillary electrophoresis, detection limit, electric field, electrolytes, liquid chromatography, mass spectrometry, quaternary ammonium herbicides
Simultaneous electrophoretic concentration and separation (SECS) was used as a simple and environmental friendly sample preparation strategy for herbicides in beer samples. An electric field was used to facilitate the separation and concentration of the analytes based on their charge from a 20 mL sample of diluted beer into two separate 20 μL aliquots of an acceptor electrolyte housed inside a micropipette. The anionic organophosphonate and cationic quaternary ammonium herbicides were concentrated in the anodic and cathodic pipette, respectively. Under optimized conditions, SECS was completed in 30 min at an applied voltage of 150 V, which provided analyte concentration factors of up to 90. After sample preparation, the SECS concentrate of cationic and anionic herbicides was analyzed by stacking CE with UV detection and also by LC–MS, respectively. The method detection limit for the diluted and undiluted sample was as low as 3 and 15 ng/mL, respectively. The method was linear over two orders of concentration with repeatability and intermediate precision of better than 5.8 and 7.0%RSD, respectively. Accuracy values were between 91.0–115.1%.