In this work, fibrous TiO2@g-C3N4 nanocomposites (FTGCNCs) were used as a new adsorbent of dispersive micro-solid phase extraction for speciation of antimony in cow milk, including Sb(III), Sb(V), residual, digestible, and total Sb. Samples were prepared with artificial gastric juice to achieve bioaccessible species of elements before ICP-MS determination. Besides, adsorption behaviors of Sb(III) and Sb(V) on FTGCNCs were investigated. The results showed that Sb(III) was quantitatively adsorbed on FTGCNCs in the pH range of 2.0–4.0, while Sb(V...