Antibiotic drug residues can adversely affect the human body. Lincomycin is a common veterinary drug that can form residues in foods of animal origin. However, the detection of trace residue levels of lincomycin residues in real samples is challenging. Here, a simple solid phase extraction (SPE) method was developed for the enrichment of lincomycin from cow milk samples before its detection by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The adsorbent used in the SPE was a Cu-based metal-organic framework (Cu-MOF) prepared by the solvothermal synthesis approach. The prepared MOFs were characterized using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), differential thermogravimetric analysis (TG-DTA), and N2 adsorption-desorption experiments. The adsorption capacity (adsorption equilibrium, extraction time, pH), and elution solvent parameters were investigated. Under the optimized conditions of the HPLC-MS/MS method, lincomycin was detected in the linear range of 10–200 g/L with a detection limit of 0.013 ng/mL. Commercial milk samples were spiked with lincomycin, and a recovery rate between 92.3% and 97.2% was achieved. Therefore, the current method can be successfully applied for the enrichment and determination of lincomycin from milk samples.
Fast detection is important in screening large-scale samples. This study establishes a direct competitive ELISA method (dcTELISA) based on an enzyme thermistor for fast atrazine (ATZ) detection. ATZ competes with β-lactamase-labeled ATZ (ATZ–E) for the binding sites on anti-ATZ monoclonal antibody (mAb). The mAb are covalently bound to Controlled Pore Glass (CPG) in an immunoreactor to form immunocomplexes with ATZ and ATZ–E. Several parameters of biosensor performance were optimized, such as the ATZ–E concentration, concentration and nature of the substrate, flow rate, and effect of temperature on the sensor response. After optimization, the assay time for a single sample was 12 min. The work process and result were compared with those of high-performance liquid chromatography (HPLC). The detection results exhibited a recovery rate of 88% to 107% in ATZ-spiked fresh cut corn stalks and silage samples. The results obtained via dcTELISA had good correlation with that of HPLC, and the biosensor response was reproducible and stable even when used continuously for over 4 months. All these properties suggested that the fast detection method, dcTELISA, may be used to detect pesticide residue in large-scale samples.