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A magnetic graphene-like molybdenum disulfide nanocomposite was prepared by liquid-phase exfoliation and hydrothermal synthesis. The morphology, structure, and magnetic behavior of the nanocomposite were characterized by X-ray diffraction, FTIR spectroscopy, thermogravimetric analysis, vibrating sample magnetometry, scanning electron microscopy and transmission electron microscopy. The nanocomposite was employed as a sorbent for magnetic solid-phase extraction (MSPE) of eight triazine and ten sulfonylurea herbicides from environmental water and corn samples. Specifically, this was studied with cyanazine, simetryn, atrazine, methoprotryne, ametryn, prometryn, terbutryn, dipropetryn, metsulfuron-methyl, sulfometuron-methyl, amidosulfuron, rimsulfuron, nicosulfuron, bensulfuron-methyl, halosulfuron-methyl, pyrazosulfuron-ethyl, chlorimuron-ethyl, and cyclosulfamuron. The parameters affecting extraction efficiency (sorbent amount, pH value of the sample, extraction and elution conditions) were studied and optimized. Following MSPE, the multi-residue herbicides were quantified by ultra-high performance liquid chromatography combined with ion trap mass spectrometry and electrospray ionization. The limits of detection range between 20 and 170 ng·L−1. The extraction recoveries of eighteen herbicides from corn samples were in the range between of 64.7% and 103.1%, with RSDs of <17.6%. [ABSTRACT FROM AUTHOR]