A high-performance liquid chromatography-tandem mass spectrometric (LC-MS/MS) method with a rapid and simple sample preparation was optimized and validated for the determination of phenanthrene-9,10-dione, chrysene-5,6-dione, benzo[a]pyrene-1,6-dione, benzo[a]pyrene-3,6-dione, benzo[a]pyrene-4,5-dione, benzo[a]pyrene-6,12-dione, benzo[a]pyrene-7,8-dione, benzo[a]pyrene-11,12-dione and 6-oxo-7-oxa-benzo[a]pyrene in particulate matter. The mass spectrometer was operated in the multiple reaction monitoring (MRM) mode leading to high sensitivity and selectivity. The limits of quantification (S/N=10) ranged from ca. 0.1 pg/microl to ca. 5.8 pg/microl and matrix dependent recoveries varied between 49 and 92%. The applicability of the LC-MS/MS method was shown by the analysis of particulate matter (PM(2.5)) collected during the course of 2005 in the Munich area, Germany. All oxy-PAHs determined exhibited higher mean and peak concentrations in the winter months compared to the concentration levels in the warmer season.