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In this study, a new Ti 3 C 2 T x -coated fiber was synthesized and utilized as coatings for solid-phase microextraction of seven polychlorinated biphenyls. The as-produced multilayered Ti 3 C 2 T x MXene was characterized by X-ray diffractometer, thermos-gravimetric analysis, scanning electron microscopy, and energy dispersive spectroscopy. It is noteworthy that the Ti 3 C 2 T x showed some attractive features including unique 2D layered structures, large surface area, good hydrophilicity, and rich active recognition sites, endowing it has a high affinity towards the target polychlorinated biphenyls. Subsequently, the affecting parameters on the extraction efficiency of polychlorinated biphenyls were optimized. Under the optimal conditions, a novel method for the analysis of polychlorinated biphenyls in water samples was proposed. The Ti 3 C 2 T x -coated fiberbased solid-phase microextraction method showed good linearity (r 2 > 0.9928), high enrichment factors (268-442), low limits of detection (0.06-0.15 ng/L), and satisfactory repeatability (RSDs < 7.5%) for the polychlorinated biphenyls. The excellent method recoveries were in the range of 90.0-98.4, 92.0-98.2, and 92.0-98.0% for river water, lake water, and tap water samples, respectively. These results suggested that the proposed Ti 3 C 2 T x -coated fiber-based method represents a promising alternative for the analysis of polychlorinated biphenyls.

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