Capillary zone electrophoresis with indirect UV detection at 215 nm was applied for the separation and determination of mannitol (MA), sorbitol (SO) and xylitol in the form of anionic borate-polyol complexes. The separation was carried out in a fused silica capillary (total length 60 cm, effective length 50 cm, I.D. 50 microm) at 25 kV. The optimized background electrolyte was 200 mM borate buffer (pH 9.3, adjusted with triethylamine) containing 10 mM 3-nitrobenzoate as the chromogenic co-ion. The separation took approximately 13 min. The rectilinear calibration range was 0.2-2 mg mL(-1) for MA and SO when using xylitol (1 mg mL(-1)) as the internal standard. The limit of detection at a S/N of 3 was approximately 30 microg mL(-1) for either analyte. The method was used for the assay of MA or SO in pharmaceutical infusion solutions. The RSD values were 0.15% or 1.07% (n=6) when determining 100 mg mL(-1) of MA or 50 mg mL(-1) of SO in commercial infusion solutions. The results were in good agreement with those of pharmacopoeial iodimetric titration.