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A new, simple and rapid capillary electrophoresis-mass spectrometry (CE-MS) method, using a cationic polymer-coated capillary to reverse electroosmotic flow, is proposed and validated for the separation and simultaneous quantification of 11 gibberellins (GAs). Under optimum conditions, a baseline separation of 11 GAs, including GA(1), GA(3), GA(4), GA(5), GA(6), GA(7,) GA(13), GA(19), GA(20), GA(24) and GA(53) was accomplished within 25 min using 70 mM ammonium formate/formic acid buffer (pH 3.8) and 2% (v/v) acetonitrile with -25 kV as the separation voltage. Satisfactory results were obtained in terms of linearity (R-2 between 0.984 and 0.995), precision (RSD of migration time below 0.8%) and sensitivity (LOD between 0.31 and 1.02 mu M). Furthermore, a novel solid-phase extraction (SPE) procedure was developed for the pre-concentration and purification of GAs using Oasis MAX cartridges. The combination of SPE and CE-MS approach was applied to screen for endogenous GAs present in coconut (Cocos nucifera L.) water sample. To illustrate the applicability of the method, GA(1) and GA(3) were successfully detected and quantified in coconut water. Finally, the GA(1) and GA(3) identities were further unequivocally confirmed by CE-tandem MS experiments operating in the multiple reaction monitoring mode. (c) 2007 Elsevier B.V. All rights reserved.