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Synchronous fluorescence spectroscopy (SFS) is a technique that involves the simultaneous detection of fluorescence excitation and emission at a constant wavelength difference. The spectrum yields bands that are narrower and less complex than the original excitation and emission bands. The SFS bands correspond uniquely to the fluorescing molecule. Our investigation focuses on evaluating the sensitivity of the SFS technique for the detection and quantitation of PAHs relevant to astrochemistry. Results are presented for naphthalene, anthracene, and pyrene in three different solvents: n-hexane, water, and ethanol. SF bands are obtained with a constant wavelength difference between the peak excitation and emission wavelength (Δλ = λex − λem) at a concentration ranging from 10−4 to 10−10 M. Limit of detection (LOD) and limit of quantitation (LOQ) calculations are based on integrated SF band areas at different concentrations. Spectra of 23 pg/g of anthracene, 16 pg/g, and 2.6 pg/g of pyrene are recorded using ethanol as the solvent. The PAHs exhibit detection limits in the fractions of parts-per-billion (ng/g) range. Through comparison with similar prior studies employing fluorescence emission, our findings reveal a better detectability limit, demonstrating the effectiveness and applicability of the SFS technique.