Micellar electrokinetic chromatography (MEKC) has been applied for the determination of 5-hydroxymethylfurfural in several foodstuffs. A 75 mM phosphate buffer solution at pH 8.0 containing 100 mM sodium dodecylsulphate was used as background electrolyte (BGE), and the separation was performed by applying +25 kV in a 50 mu m I.D. uncoated fused-silica capillary. Good linearity over the range 2.5-250 mg kg(-1) (r(2) >= 0.999) and run-to-run and day-to-day precisions at low and medium concentration levels were obtained. Sample limit of detection (0.7 mg kg(-1)) and limit of quantification (2.5 mg kg(-1)) were established by preparing the standards in blank matrix. The procedure was validated by comparing the results with those obtained with liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Levels of HMF in 45 different foodstuffs such as breakfast cereals, toasts, honey, orange juice, apple juice, jam, coffee, chocolate and biscuits were determined. (c) 2010 Elsevier Ltd. All rights reserved.