A highly sensitive gas chromatography–mass spectrometry (GC–MS) method for the determination of endocrine disrupting chemicals (EDCs) including parabens, alkylphenols, phenylphenols, bisphenol A and triclosan in human breast milk, blood and urine samples is proposed. Blood and milk require a pretreatment to remove proteins and other substances potentially interfering with the continuous solid-phase extraction (SPE) system used; on the other hand, urine samples can be directly introduced into the system after filtering. Analytes are retained on a LiChrolut EN column and derivatized by silylation following elution with acetonitrile. The resulting trimethylsilyl derivatives are determined by GC–MS. The proposed method exhibited good linearity (r2 > 0.995) for all target EDCs over the concentration range 0.7–10,000 ng/l in urine, and 3.3–50,000 ng/l in blood and milk. Also, it provided low limits of detection (0.2–1.8 ng/l in urine, and 1.0–9.0 ng/l in blood and milk), good precision (relative standard deviations less than 7%) and recoveries from 86 to 104%. A total of 24 human fluid samples were analyzed and most found to contain some target EDC at concentrations from 0.10 to 14 μg/l.