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An original method based on ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of perfluorooctanoic acid (PFOA) perfluorooctanesulfonate (PFOS) and their precursors in biological matrix. Target compounds were extracted with water or methanol in corresponding biological matrix by ultrasonic. Then the extract was purified by solid phase extraction (Waters Oasis (R) WAX 6cc), after that the precursors compounds were eluted with methanol and PFOA and PFOS were eluted with 9% NH4 OH in methanol. Finally the target compounds were separated on a Waters ACQUITY (TM) BEH C-18 column (50 mm X 2.1 mm X 1.7 mu m) and detected by negative electrospray ionization mass spectrometry in multiple reaction monitoring mode. The average recoveries for four target compounds in two biological matrixs were 94.6%-128.4% by using internal standard method and the relative standard deviations were 2.5%-14.9%. For the four target compounds in two biological matrixs, the limits of detection of the method were in the range of 0.01-0.42 mu g/L and the limits of quantification were in the range of 0.04-1.5 mu g/L. With high accuracy and sensitivity, the method was simple and rapid, and can apply to evaluate the metabolic characterization and the source of exposure for PFOA and PFOS in biological matrix.