摘要： Mesoporous carbon hollow spheres coated with MoS2 (C@MoS2) were synthesized to obtain a material with large specific surface area, fast electron transfer efficiency and good water dispersibility. The composite material was applied as a matrix for the analysis of small molecules by surface-assisted laser desorption/ionization time-of-flight mass spectrometry (SALDI-TOF MS). The use of a core-shell C@MoS2 matrix strongly reduces matrix background interferences and increases signal intensity in the analysis of sulfonamides antibiotics (SAs), cationic dyes, emodin, as well as estrogen and amino acids. The composite material was applied to the SALDI-TOF MS analysis of selected molecules in (spiked) real samples. The ionization mechanism of the core-shell C@MoS2 as a matrix is discussed. The method exhibits low fragmentation interference, excellent ionization efficiency, high reproducibility and satisfactory salt tolerance.