Abstract: The 2.000 g of coating sample was taken, and 15 mL of acetonitrile was added. The mixture was vortexed for 30 s, and extracted by ultrasound at 30 ℃ for 40 min. After cooling to room temperature, the extract was made its volume up to 20 mL with acetonitrile. An aliquot (1 mL) was taken, and passed through a 0.22 μm filter membrane, and the filtrate was introduced into a high performance liquid chromatograph. Three fluoroalkyl acrylate compounds (FTAs), including 1H,1H,2H,2H-perfluorodecyl acrylate (8∶2 FTA), 1H,1H,2H,2H-perfluorododecyl acrylate (10∶2 FTA), and 1H,1H,2H,2H-perfluorooctyl acrylate (6∶2 FTA) were separated on a ZORBAX SB-Aq column by gradient elution with a mixture of acetonitrile and water at different volume ratios, with external standard method for quantification. It was shown that linear relationships between values of mass concentration and peak area of the 3 FTAs were kept in the range of 0.2-5.0 mg·L⁻¹, and the detection limits (3S/N) were found in the range of 0.27-0.34 mg·kg⁻¹. Test for recovery was made according to the standard addition method, giving recoveries in the range of 93.5%-109%, with RSDs (n=6) of the determined values ranged from 0.50% to 4.7%. The proposed method was used for the analysis of 10 types of coating samples, and 8∶2 FTA was detected in two types of samples, with detection amounts of 226.7 mg·kg⁻¹ and 4.1 mg·kg⁻¹, respectively.