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Advanced analytical platforms are required for accurate detection and quantification of small molecular substances exhibiting certain toxicity. Small molecules detection in complex biological fluids are challenged by the complexity of the samples and the low throughput of the existing methods. In the present study, to detect a batch of samples (50) in 1 h, the plasmonic nanoshell enhanced matrix-assisted laser desorption/ionization mass spectrometry (MALDI-TOF MS) was tested. The limit of quantification (LOQ) was determined as 0.01 mu g/mL (for alpha-dicarbonyl compounds) by vortex-assisted liquid-liquid microextraction (VALLME). The developed method can be adopted to study the high-throughput metabolomics and employed for clinical precision diagnosis with MALDI-TOF MS.