Various multi-step extraction procedures were used in order to determine the β-hydroxyacid content of a Recent lacustrine sediment. Similar distribution but important quantitative differences were noted. All the β-hydroxyacids are derived from the same origin but the commonly used methanolic saponification is inappropriate for the release of bound β-hydroxyacids. All the extraction techniques produce either 3-methoxy or 3-chloro and Δ²-unsaturated carboxylic acids as artifacts from the 3-substituted fatty acids. A two-step procedure is recommended for the extraction of the maximum amount of β-hydroxyacids with the minimum formation of artifacts.