A sensitive liquid–chromatography–electrospray tandem mass spectrometry multiclass method for determination of 45 veterinary compounds belonging to 9 different antibiotic groups, including aminoglicosides (4), β-lactams (13), diaminopyrimidines (1), fluoroquinolones (10), lincosamides (1), macrolides (5), pleuromutilins (1), sulfonamides (6) and tetracyclines (4), in water from breeding animal watering supply system has been developed. Isolation of the analytes was carried out by solid phase extraction with heptafluorobutyric acid as an ion-pair agent on the Strata-X reversed phase cartridges. All analytes were determined simultaneously in one single run on a C18 column with gradient elution and short analysis time (13min). Method was validated, average relative recoveries were in the range of 84.3–109.3% with satisfactory precision are repeatability for all compounds are in the range of 4.7–12.2%, within-laboratory reproducibility are in the range of 4.4–13.5% for. The limit of quantitation (LOQ) of the method was in the range of 0.02–10μgL−1, depending of analyte. The applicability of the method was tested by determining antimicrobial compounds in real water samples collected from water supply systems in breeding animal farms. The average antibiotics concentration in real water samples were, respectively, in the range of 0.14–1670μgL−1.

A molybdenum disulfide(MoS2)-based core-shell magnetic nanocomposite (Fe₃O₄@MoS₂) was synthesized by the stepwise hydrothermal method. Two-dimension ultrathin MoS₂ sheets with a thickness of approximately 20 nm were grown in situ on the surface of Fe₃O₄ (∼200 nm). They were employed as an adsorbent for the magnetic solid-phase extraction (MSPE) of sulfonamide antibiotics (SAs) from water samples. High-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was used for SA quantitation. Extraction parameters, including the pH effect, amount of Fe₃O₄@MoS₂, extraction time, temperature, and desorption conditions, were systematically investigated. The electrostatic interaction between the positively charged SAs and negatively charged MoS₂ nanoparticles in the optimal extraction conditions enhanced the adsorption of SAs on the sorbent surface. Under chosen conditions, the proposed strategy achieved wide linear range of 1.0–1000 ng·L⁻¹ SAs, low limits of detection (LOD, 0.20–1.15 ng·L⁻¹, S/N = 3:1), good trueness (recoveries between 85.50–111.5%), satisfactory repeatability and reproducibility (relative standard deviation, <10%, n = 5), and excellent recoveries between 80.20% and 108.6% for SAs determination in spiked waste water samples. The proposed strategy was validated and successfully applied for the analysis of water, milk, pork meat and fish meat. The nanocomposites, which have the combined advantages of magnetic separation and high adsorption affinity toward SAs, are a promising sorbent for antibiotics extraction from real samples.

Efficient extraction of polar sulfonamides antibiotics from aqueous samples and food is very challenging, because they are hydrophilic, their concentration is very low, and the matrix is complex. Covalent organic frameworks (COFs), a novel porous organic material, have attracted great attention. In this work, the spherical triphenylbenzene-dimethoxyterephthaldehyde-COFs (TPB-DMTP-COFs) were synthesized by a simple room temperature method, and due to their attractive properties, such as high outstanding acid-base stability, large specific surface area, low skeletal density, inherent porosity and high crystallinity, so TPB-DMTP-COFs as ideal solid phase extraction adsorbents showed excellent adsorption performance for trace polar sulfonamides in food and water. TPB-DMTP-COFs were characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, powder X-ray diffraction, and so on. The important parameters were optimized to improve the extraction efficiency of TPB-DMTP-COFs toward sulfonamides. Analysis of sulfonamides was performed by liquid chromatography–tandem mass spectrometry. The developed method based on TPB-DMTP-COFs material achieved low limits of detection (0.5–1.0 ng L⁻¹), wide linearity (5–1000 ng L⁻¹), and good repeatability (2.5%–8.7%). The possible extraction mechanism was also discussed. Finally, the method was successfully applied to the enrichment and detection of sulfonamides in environmental water samples and food samples. The present study indicated that TPB-DMTP-COFs had splendid prospects in highly sensitive analysis of other pollutants in complex matrix.