A fast and simple sample preparation procedure for the speciation of organolead compounds is described. Separation and detection of the different species was carried out using gas chromatography hyphenated to microwave-induced plasma atomic emission spectrometry. Derivatization was performed using in situ propylation with sodium tetrapropylborate in an acetic acid-sodium acetate buffer medium of pH 4.5 with simultaneous extraction of the propylated species into hexane. Detection limits (as Pb) ranging from 77 fg (0.15 ng kg ^–1 ) to 102 fg (0.21 ng kg ^–1 ) and relative standard deviations between 4 and 6% were achieved. Accuracy of the procedure was confirmed by analysis of a certified reference material (CRM 605, Road Dust), where the desorption of the different species from the matrix by acid leaching was also integrated in the derivatization and extraction step. The optimized sample preparation procedure was applied to the analysis of alpine snow sampled at the Mont-Blanc in France.