During the industrial refining process of edible oils and the manufacture of oil-based foodstuff, contaminants such as 3-monochloropropanediol (3-MCPD) fatty acid diesters can be produced. One hundred samples of different edible oils and related fatty food purchased from local Spanish markets were analyzed to evaluate the occurrence of these contaminants. Data of seven 3-MCPD diesters together with corresponding total 3-MCPD equivalents are presented. The procedure is based on a modified QuEChERS protocol followed by LC-MS/MS analysis. Extra virgin olive oil (EVOO) and unrefined oils did not contain detectable levels of the target analytes. The highest levels of 3-MCPD diesters were found in palm oils, for 1,2-Dilinoleoyl-3-chloropropanediol (LILI) and 1–2-Bispalmitoyl-3-chloropropanediol (PAPA) with concentrations close to 10 mg kg−1 and in the lipid fraction of margarines (8.09, 3.77 and 3.72 mg kg−1 for LILI, PAPA and 1-Oleoyl-2-linoleoyl-3-chloropropanediol (OLLI), respectively).