A high performance liquid chromatographic (HPLC) method for determining the concentration of trace amounts of benzo(a)pyrene (B(a)P) in particulate matter from combustion of forest fuels was validated. Particulate matter was prepared for analysis by a small-scale (1 mg), simplified preparation followed by HPLC with fluorescence detection. The chromatographic system had a limit of detection of 2.67 ng/mL, a precision of 6.4% relative standard deviation, and a working range of 2.67 to 100 ng/mL. The complete method gave a mean recovery of 100.6% across its working range with an 8.3% relative standard deviation. With National Bureau of Standards' Standard Reference Material 1649 (urban particulate matter), a mean recovery of 93.2% of the certified B(a)P content was obtained with a 9.9% relative standard deviation. After storing loaded filters for 4 months under refrigeration, the B(a)P content of the particulate matter from forest fire smoke had not significantly changed.