A denuder-filter sampling technique for the simultaneous collection of gas and particle phase carbonyl compounds has been developed and tested. The denuder was coated with XAD-4 resin and the derivatizing agent O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine (PFBHA) to enable on-tube conversion of gas-phase carbonyls to their oxime derivatives which were extracted and identified by GC-MS. The performance of the PFBHA-coated denuder was tested on a range of carbonyls, dicarbonyls, aromatic aldehydes, carbonyl-containing furans, and benzoquinones. The collection efficiency of the PFBHA-coated denuder was over 90% for sampling times of 10 min and significantly higher than when using only XAD-4 as the sorbent. The collection efficiency and rate of on-tube derivatization was highest for aldehydes and lowest for ketones, consistent with the expected reactivity of carbonyls with PFBHA. The method was used to separate the gas and particle phase carbonyl products formed during the photooxidation of toluene in order to assess its potential for application to simulation chamber experiments of VOC oxidation. The results indicate that when compared to a conventional filter sampling setup, the PFBHA-coated denuder-filter reduced the extent of gas phase adsorption onto the filter by at least a factor of 2 for each of the carbonyls formed. Further potential applications of the denuder-filter sampling method are discussed.