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Several carbonyl compounds are important because of their irritant and toxic properties, mutagenicity andcarcinogenicity. Therefore, they are regulated in korean odor emission standard.In this study, atmospheric pressure ionization-mass spectrometry (API-MS) is used for the analysis of carbonylcompounds after derivatization with 2, 4-dinitrophenylhydrazine (DNPH) and liquid chromatographic separation.-H]- pseudomolecular ions are most abundant for the carbonyls. Analyticalparameters such as linearity, repeatability and minimum detection limit were evaluated. The linearities (r2) for carbonyls were 0.9977~ 0.9999 when analyte concentration ranges from 25 to 250g/L(n= ~ 3.51% for concentration of 100g/L(n= 5). The minimum detection limit (MDL) was 1.88g/L (0.27 ppb) for i-valeraldehyde. It was shown that LC-MS method has a great potential for carbonyl compounds analysis.