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Abstract: The aim of this paper was to use the air classification technology to produce barley flours enriched in phenolic compounds and to obtain naturally enriched ingredients for pasta and bakery industry. Phenolic compounds in barley have been described in literature using different methodologies that are not easily comparable. This paper describes a comparative study between different separative and spectrophotometric methods to determine free and bound phenolic compounds in barley flours and their air classified fractions from three different cultivars grown in the same experimental field. To this end, reversed phase-high performance liquid chromatography, micellar electrokinetic chromatography, and spectrophotometric determinations were applied. The barley phenolic compounds analyzed included mainly catechins and proanthocyanidins as free phenols, and hydroxycinnamic acids and their derivatives as bound phenols. The enriched fractions obtained by air classification showed an increase of free flavan-3-ols of 157–173% compared to whole flour. The same fractions also reported larger concentration of bound phenolic compounds (160–236%) with respect to whole flours. Air classification results a good technique to enrich the flours and to utilize the barley co-products. [Copyright &y& Elsevier]