Abstract: HPLC was applied to the determination of formaldehyde,acetaldehyde and acetone in nail polish.The sample was extracted with acetonitrile and water with 2,4-dinitrophenylhydrazine as derivative agent.Kromasil-C18 chromatographic column was used as stationary phase and a mixture of acetonitrile and water (65+35) was used as mobile phase.UV-detection at 364 nm was adopted in the determination.Linear relationships between values of peak area and mass concentration of formaldehyde,acetaldehyde and acetone were kept in the same range of 0.01-20.0 mg·L-1,with detection limits (3S/N) in the range of 0.001 5-0.003 5 mg·L-1.Values of recovery found by standard addition method were in the range of 88.6%-110%,and values of RSD′s (n=6) in the range of 1.2%-9.7%.