Effects of fiber coating type on SPME adsorption of 2-acetyl-1-pyrroline, the characteristic odorant compound released from marking fluid of P. tigris altaica with 85 µm CAR/PDMS, 50/30 µm DVB/CAR/PDMS, 100 µm PDMS, 65 µm PDMS/DVB, and 75 µm CAR/PDMS SPME fibers. Marking fluid (0.25 mL) and a stir bar were inserted into a 2 mL glass vial with a PTFE coated septa for a period of 30 min for equilibration. Samples (n = 3) were extracted at a temperature of 37 °C for 1 h. MS scan mode was total ion scan. Two min of the 40 min total scan is shown. Identification of 2-AP was accomplished with two fibers, the 75 µm CAR/PDMS and 65 µm PDMS/DVB SPME fibers. The 75 µm CAR/PDMS fiber had a peak area of 3.5 × 105 counts and the 65 µm PDMS/DVB SPME fiber had a peak area of 8.9 × 105 counts.