Objective To develop a novel solid-phase extraction(SPE)method based on a functionalized nanofiber membrane for the efficient co-extraction of structurally diverse antibiotics with markedly different physico-chemical properties from source water,and to establish a high-throughput analysis method by coupling this technique with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods A polydopamine and zirconium(Ⅳ)fumarate metal-organic frameworks(MOF-801)co-modified polyacrylonitrile nanofiber membrane(PDA@PAN/MOF-801 NFMs)was prepared as the SPE adsorbent through hybrid electrospinning and dopamine self-polymerization.Critical SPE and UPLC-MS/MS parameters were optimized,and the method was applied to analyze antibiotic contamination in source water samples from 14 sources of centralized drinking water supply in Suzhou,China,to evaluate the practical application potential of the method.Results The PDA@PAN/MOF-801 NFMs adsorbent demonstrated efficient adsorption of 32 antibiotics from 6 classes through multiple retention mechanisms,including synergistic electrostatic interactions,hydrogen bonding,and π-π interactions.In combination with UPLC-MS/MS,the SPE method we developed enabled high-throughput detection of multiple antibiotics in source water,with limits of detection(LOD)being 0.001-0.05 ng/L and limits of quantitation(LOQ)being 0.005-500 ng/L.Spiked recoveries were 70.14%-111.50%.Intra-day relative standard deviation(RSD)was below 14.12%and the inter-day RSD was below 15.07%.The method demonstrated excellent sensitivity,accuracy,and precision.Conclusion In this study,we successfully developed an efficient analytical method based on a novel nanofiber membrane adsorbent.This approach provides a new technical reference for the high-throughput detection of multiple antibiotics in environmental waters and shows promising potential for practical applications.