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• Enantioseparation and determination of triazole fungicides was developed by ATPE coupled to 2D-LC. • ATPE extraction of triazole fungicides were optimized by single-factor experiments and SRM. • 2D-LC chromatographic conditions of racemates and enantiomers were investigated respectively. • Simultaneous determination of racemates and enantiomers was validated by online heart-cutting 2D-LC. • The approach was successfully used in analysis of triazole fungicides in vegetables and fruits. A novel method for determination of triazole fungicides and their enantiomers in foods was developed by aqueous two-phase extraction (ATPE) coupled with two-dimensional liquid chromatography (2D-LC). With an aqueous two-phase system (ATPS) of ethanol/K 2 HPO 4 as biphasic extractant, the effects of the ATPS composition, extraction temperature and time on extraction yields of triazole fungicides were investigated. Optimum conditions were concluded as follows: ethanol concentration 31% (w/w) and K 2 HPO 4 concentration 21% (w/w), extraction temperature 60 °C, extraction time 21 min. Based on reversed-phase separation systems, a 2D-LC was constructed by optimizing chromatographic conditions and online heart-cutting procedures. As a result, eight triazole fungicides and their enantiomers were separated respectively on C18 and cellulose-tris (3,5-dimethylphenylcarbamate) stationary phases, revealing good linear relationship in the range of 0.1218–30.06 μg/mL (R2 ≥ 0.9984). The detection limits and recoveries were 0.03113–0.3525 μg/mL and 71.57–107.8%, respectively. The ATPE–2D-LC method was successfully applied to chiral analysis of triazole fungicides in fruits and vegetables. [ABSTRACT FROM AUTHOR]