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Gas chromatography and mass spectrometry (GC/MS) was applied for determination of concentrations volatile organic compounds present in human breath samples. The technique allows to rapid determination compounds in human air, at the level of parts per billion. It showed linear correlations ranging from 0.83-234.05 ppb, limit detection in the range of 0.31-0.75 ppb and precision, expressed as RSD, was less then 10.00%. Moreover, trained dogs are able to discriminate breath samples of patients with diagnosed cancer disease. We found positive correlation between dog indications and content of ethyl acetate and 2- pentanone in breath (r=0.85 and r=0.97, respectively)