Ti3C2Tx-bonded aminopropyl-modified spherical silica: A novel dispersive solid-phase extraction sorbent for determination of 9 fluoroquinolones

To improve the pre-treatment efficiency of fluoroquinolones (FQs) in food testing, a novel functionalized MXene, Ti 3 C 2 T x /SiO 2 -NH 2 , was synthesized via electrostatic interactions between Ti 3 C 2 T x and aminopropyl-modified silica (SiO 2 -NH 2 ). Used as a dispersive solid-phase extraction (d-SPE) adsorbent, it enabled a new UPLC-MS/MS method for nine FQs in pork. Compared to pristine Ti 3 C 2 T x and SiO 2 -NH 2 , the composite had a larger adsorption capacity, achieving a specific surface area of 251.28 m 2 /g. Adsorption was dominated by ionic interactions and followed a monolayer model. Optimized d-SPE conditions: 20 mg adsorbent, 2 min extraction (pH 7), 2 mL 5 % ammoniated methanol desorption (1 min). Notably, extraction in hexane integrated with hexane degreasing, cutting total pretreatment time to <10 min. Under optimal conditions, linearity for FQs was 0.5–100 ng/mL (r 2  > 0.99). Detection limits (DLs) and quantitation limits (QLs) were 0.034–0.553 μg/kg and 0.114–1.845 μg/kg, respectively. Recoveries were 85.80–105.70 %, with intra-day (1.06–7.53 %) and inter-day (1.88–12.27 %) RSDs. After 7 cycles, six FQs still had 71.57–84.92 % recoveries. Ti 3 C 2 T x /SiO 2 -NH 2 is a promising d-SPE adsorbent, and the UPLC-MS/MS method offers rapid, sensitive FQs monitoring in pork.