MIL-88B(Fe)/cellulose microspheres as sorbent for the fully automated dispersive pipette extraction towards trace sulfonamides in milk samples prior to UPLC-MS/MS analysis.

MIL-88B(Fe)/cellulose microspheres (MIL-88B(Fe)/CMs) were characterized by the means of SEM, XRD, TGA and N2 adsorption-desorption test. The composite was used as the sorbent for fully automated dispersive pipette extraction (DPX), after introducing CMs as the support, the loss of MIL-88B(Fe) in DPX was avoided. Coupled to UPLC-MS/MS, the proposed method was employed for the analysis of trace sulfonamides (SAs) in milk samples. The parameters affecting the extraction efficiency, including pH of sample solution, the rate of aspiration and dispense, amount of the adsorbent, type and volume of elution solvent were optimized. Under the optimal conditions, good linearity (r ≥ 0.9978 for five analytes), high sensitivity (limit of detection: 0.00660-0.0136 μg kg-1) and satisfactory recovery (69.8%-100.9%) were achieved. Furthermore, the sorbent showed desirable reusability over eight extraction cycles. Compared with other methods for the pretreatment of SAs, the proposed method showed advantages of high sensitivity, less sorbent consumption, environmental friendliness and automation, providing a promising protocol for sample preparation.