This paper describes a new analytical method, using a combination of ammonium pyrrolidine dithiocarbamate/methyl isobutyl ketone (APDC-MIBK) microextraction and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), for the determination of the concentrations of Cd and Pb in aqueous samples. Only 200 µL of organic solvent was used throughout the entire analysis process, with enhancement factors as high as 25. Recoveries from replicate analyses of natural water [NIST 1640(a)] containing mean concentrations of 3.1 mg Cd L -1 and 9.3 mg Pb L -1 were 95 ± 3 and 104 ± 4%, respectively. The corresponding detection limits were 0.6 mg L -1 for Cd and 0.9 mg L -1 for Pb. The main advantage of this approach is its simplicity in terms of sample preparation, as demonstrated by quantifying the levels of Cd and Pd in real samples, including tap water, groundwater, and seawater, using a standard addition method.