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Research on pollution characteristics and toxicities of emerging polycyclic aromatic sulfur heterocycles (PASHs) in PM2.5 has not been reported due to the lack of analytical method with the needed performance.In the present study,a novel method for the determination of 14 PASHs in PM2.5 was developed using atmospheric pressure gas chromatography-tandem mass spectrometry (APGC-MS/MS).Atmospheric pressure chemical ionization was operated with multiple reaction monitoring in positive ionization mode.High sensitivity (method detection limit ＜ 1.673 pg/m3),acceptable recoveries (67.6％-120.8％) and precisions (RSD of 2.2％-15.4％) were obtained.The method was successfully applied for analyzing PASHs in 10 PM2.5 samples collected from Taiyuan,a typical industrial city in China,in 2016.The total concentrations were from 929 pg/m3 to 14,593 pg/m3.The determined levels indicated that further investigations on environmental fate and toxicities of PM2.5-bound PASHs may be needed,