Abstract: 3-Nitrobenzanthrone, a persistent organic pollutants (POPs), is an extremely potential mutagen and susceptible carcinogen as proved by the tests using both animal and human cells. The major sources of 3-nitrobenzanthrone are believed to be vehicle exhaust from diesel engines, as well as photooxidation reaction in the atmosphere. Its atmospheric concentration is far below polycyclic aromatic hydrocarbons. This paper reported an analytical method that was established by using high pressure liquid chromatography (HPLC) to separate and enrich the target fraction and consequently measured with gas chromatography-mass spectrometry (GC/MS). The instrument detection limit (IDL) is 13.7 pg， and the method detection limit(MDL) is 1.86 pg•m^-3. The method recoveries for the deuterated surrogate, 1-nitropyrene-d9, and 3-nitrobenzanthrone are 88.5% and 78.2%, respectively. The method features good accuracy, precision and reproducibility, and could be used for regular measurements of 3-nitrobenzanthrone.