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A novel sample pretreatment method combining hollow fiber protected liquid phase microextraction and in-tube derivatization followed by gas chromatography, which was used for the determination of trace amounts of synthetic pyrethroids metabolites in field water samples, was described.Metabolites of synthetic pyrethroids were extracted from water samples and enriched by the hollow fiber protected liquid phase microextraction (LPME) technique.The microsyringe pre-filled with derivatizing agents inserted a hollow fiber segment impregnated with extracting solvent as the sampling probe.