In this study, an organic solvent-free microextraction technique termed liquid-gas-liquid microextraction (LGLME) was applied for cleanup and preconcentration of volatile short chain fatty acids in beverages and dairy products. Various parameters affecting the extraction efficiency such as extraction time, stirring speed, sodium chloride content, concentration and volume of donor and acceptor phases, and extraction temperature were studied. Repeatability (RSD, 4.2-8.5%), correlation coefficients (0.998-0.999), LODs (10-20 microg/L) and enrichment factors (152-249) were also investigated. Recoveries were achieved in the range of 90-102% in different matrices. The presented method was applied for the analysis of target analytes in some samples such as grape juice, vinegar and dairy products.