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Zearalenone is without doubt one of the most well-known mycotoxins, which is one form of estrogenic mycotoxin, might trigger dangerous results on human well being and livestock progress. Thus, the event of efficient pattern pretreatment strategies to take away it from advanced matrices is important. On this paper, we report a brand new and efficient nano-surface-anchored solid-phase extraction (nanoSPE) technique for the willpower of zearalenone in advanced matrices. The as-synthesized Fe(III)-Zn(II) quasi-meso-carbons spheres (FZQMs) with uniform and spherical form have been used as adsorbents and the as-synthesized Fe(III)-Zn(II) carbon nanospheres (FZCNS) with a hierarchical meso-structure have been employed as reference supplies to match the performances. The as-synthesized FZQMs are characterised by XRD, TEM, N2 adsorption-desorption, zeta potential, and ICP-MS measurements. The nSPE process consisted of pattern pretreatment, nanoSPE, and the desorption. In contrast with the standard C18-based silica nano-SPE and Fe(III)-CNS-based nSPE, FZQM-based nSPE had a superb choose