Abstract:Objective Headspace solid-phase microextraction (HS-SPME) was used as a clean-up and pre-concentration procedure for the simultaneous determination of organochlorine pesticides(OCPs)in pork samples. Method Two stable isotopic compounds, 13C labeled mirex and 13C labeled hexachlorobenzene, were used as internal standard. Gas chromatographic analysis with mass spectrometry (GC-MS) facilitates sensitive detection of the selected pesticides. Several parameters controlling SPME were studied and optimised: choice of SPME fiber, extraction temperature, extraction time, desorption time, desorption temperature and content of salt. Result Under optimal conditions, detection limits obtained were in the range of 1 to 100 ng/g depending on pesticide. Good recoveries (range from 90% to 120% in most cases) were achieved. Conclision The result showed that the HS-SPME/GC-MS method is suitable for the analysis of multi-residue OCPs in pork sample.