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In this work, the feasibility of solid-surface three-dimensional fluorescence (SSTF) in combination with chemometrics to rapidly and directly determine three PAHs in drill cuttings recycling products was studied for the first time. Due to the nondestructive characteristics of SSTF and the “mathematical separation” of chemometric three-way calibration, neither time-consuming sample pretreatments nor toxic organic reagents were involved in the determination. By using the smart “mathematical separation” function of the parallel factor analysis (PARAFAC) algorithm, clear spectral profiles together with reasonable quantitative results for the three target PAHs were successfully extracted from the total SSTF signals of drill cuttings recycling products without the need for chromatographic separation. The linearity of the calibration models was good (R2 > 0.96) and the average spiked recoveries of three target PAHs were between 88.1–102.7% with a relative standard deviation less than 20%. Nevertheless, given the green, fast, low-cost, and nondestructive advantages of the proposed strategy, it has the potential to be used as a fast screening approach and allow for a quick survey of PAHs in drill cuttings recycling products.

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