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Electrokinetic supercharging (EKS) as a powerful online preconcentration technique in CE,was hyphenated with ESI-MS.The electrophoretic separation was performed in a co-EOF mode using an EOF reversal agent,and the separation was optimised by variation of the ionic strength of the separation buffer as well as the percentage of the organic modifier added to the buffer; this optimisation was performed in a multivariate mode.After optimisation of separation parameters,the potential of EKS-ESI-MS for the separation and online preconcentration of five hypolipidaemic drugs was then investigated.The presented work shows the first method for separation and online preconcentration of hypolipidaemic drugs mixture.We here also present the first hyphenation of EKS with ESI-MS.This combination of EKS-ESI-MS allowed the sensitivity to be enhanced by 1000-fold over conventional field amplified sample stacking FASS-ESI-MS,giving limits of detection (LODs) of 200 ng/l.The developed method was validated and then applied for the determination of target drugs in real water samples form Hobart city.