A novel, simple and efficient method for determining persistent organic pollutants (POPs) in tissue samples has been developed. This technique involves the use of simultaneous microwave-assisted digestion (MAD) and micro-solid-phase extraction (micro-SPE), in which the sorbent is held within a propylene membrane envelope, with gas chromatographic-mass spectrometric (GC-MS) analysis. The POPs studied included eleven organochlorine pesticides and five polychlorinated biphenyl congeners. Optimization of the MAD-micro-SPE parameters was performed. The relative standard deviations (RSDs) of the method ranged from 0.14 to 12.7%. Correlation coefficients up to 0.9999 were obtained across a concentration range of 1.25-50 ng g(-1). The method detection limits for POPs ranged from 0.002 to 0.009 ng g(-1). A preliminary study applying the MAD-micro-SPE procedure to human ovarian cancer tissue showed that it was capable of detecting the presence of a wide spectrum of different POPs in benign and malignant tumors.