A simple, inexpensive and efficient procedure was developed for solid-phase microextraction of nicotine from the headspace above an aqueous sample. A thin layer chromatography (TLC) plate modified with carbon dots (TLC@CDs) was used as a sorbent. Nicotine is absorbed and then can be eluted with ethanol and submitted to isocratic reverse-phase HPLC with UV detection. The method excels by extraction efficiency and rapid extraction. Under optimized conditions, the calibration graph was linear in the nicotine concentration range from 10 to 400 μg L−1, with a correlation coefficient of 0.9998. The limit of detection was 6 μg L−1. This procedure was successfully applied to the determination of nicotine in spiked biological samples. The relative mean recoveries ranged from 94.4 to 105.8 %.
