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A single laboratory validation of a quantitative capillary gas chromatography tandem quadrupole mass spectrometer (GC-MS/MS) method utilizing a Quick, Easy, Cheap, Effective, Rugged, Safe (QuEChERS) approach for the extraction of 24 organochlorine analytes in liver and blood serum is presented here. The QuEChERS approach utilizes an acetonitrile extraction, partitioning facilitated by the addition of salts and a dispersive solid phase extraction cleanup. This method simultaneously monitored 24 organochlorine pesticide residues representing four different classes, including chlordecone, cyclodienes, dichlorodiphenylethanes, and hexachlorocyclohexanes. Calculated limits of detection (LOD) varied from 0.002 to 2.4 ppb and limits of quantification (LOQ) varied from 0.01 to 7.4 ppb. This multi-residue method proved to be a sensitive approach to the measurement of persistent organic pollutants in biological matrices.