3-Monochloropropane-1,2-diol (3-MCPD) monoesters are a form of 3-MCPD esters known as potential food contaminant that may occur in a variety of food samples. A dispersive solid-phase extraction (dSPE) was developed to provide clean-up and pre-concentration in the determination of 1-palmitoyl-3-MCPD and 1-oleoyl-3-MCPD prior to gas chromatography-flame ionization detector analysis (GC-FID). Dispersive solid-phase extraction (dSPE) involves the direct addition of C18 sorbent into the sample solution and the subsequent collection of the aqueous solution. After separation of target analytes with matrices, the analytes were quantified using GC-FID. Under optimum conditions (6 mL of 80:20 v/v of ACN; ethyl acetate as extraction solvent, 10 mg of C18 sorbent, 10 µL of reconstituted solvent volume, and 300 µL of sample volume), the proposed method was validated and the calibration curve was found to be linear with R2 > 0.998. The limit of detection (LOD) of 1.03 mg L−1 and 2.00 mg L−1 were obtained for 1-palmitoyl-3-MCPD and 1-oleoyl-3-MCPD, respectively, whereby the limit of quantification (LOQ) obtained for 1-palmitoyl-3-MCPD and 1-oleoyl-3-MCPD were 3.43 mg L−1 and 6.68 mg L−1, respectively. The developed method was applied to seven palm oil-based food samples where the amount of 3-MCPD detected was higher than recommended by the European Food Safety and Authority (ESFA). The recoveries for spiked samples ranged from 59.3 to 115.9% and the relative standard deviation (RSD) for inter-day and intra-day was less than 15%. The method was applied for the determination of 3-MCPD monoesters in palm oil-based food samples. [ABSTRACT FROM AUTHOR] more...