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A method was developed for the rapid screening and confirmation of 18 perfluorinated compounds (PFCs) and 21 precursors in fish muscle by solid phase extraction and liquid chromatography coupled with quadrupole/exactive orbitrap mass spectrometry (LC-Q Exactive Orbitrap MS). In this method, the sample was firstly extracted with acetonitrile. water (90. 10, V/V), cleaned. up by solid-phase extraction using Oasis PRiME HLB column. Then, 39 target compounds were separated on a BEH C1(8()2. 1 mm. 100 mm, 1. 7 mu m) column, and the background interference caused by LC system was eliminated by a short C-18 HPLC column located between the mixer and the auto sampler. In the process of quantification and qualification, a full MS/ dd.-MS2 experiment was adopted in mass spectrometry acquisition, accompanied with the full scan MS date for quantification, as well as the date dependent MS2 product ion spectra for qualification. The mass accuracy error was less than 3x10(-6), and the calibration curves were linear well with correlation coefficient over 0. 99. The limits of detection ranged from 0. 02 to 0. 50 mu g/kg. The average spiked recoveries for 39 target compounds were between 61. 7% and 122. 0%, with relative standard derivations (RSDs) from 6. 9% to 18. 8%. The developed method was successfully applied to the simultaneous determination of 18 PFCs and 21 precursors in fish muscle with satisfactory results.