Determination of fluoroquinolones in food samples by magnetic solid-phase extraction based on a magnetic molecular sieve nanocomposite prior to high-performance liquid chromatography and tandem mass spectrometry

摘要

In this study, a magnetic molecular sieve material (Fe3O4@MCM-48) was synthesized by a combination of solvothermal and self-assembly methods. The physicochemical properties of the magnetic molecular sieve material were characterized by scanning electron microscopy, energy-dispersive spectroscopy, magnetic hysteresis loop measurements, transmission electron microscopy, powder X-ray diffraction, N-2 adsorption-desorption analysis, and Fourier transform infrared spectroscopy. The as-synthesized nanocomposite showed various advantages, including easy magnetic-assisted separation, high specific surface area, and a highly interwoven and branched mesoporous structure. The Fe3O4@MCM-48 nanocomposite was then used as an effective adsorbent material for magnetic solid-phase extraction of fluoroquinolones (FQs) from water samples. The FQs in the extract were determined via liquid chromatography-tandem mass spectrometry. Adsorption and desorption factors that affected the extraction performance were systematically optimized using spiked purified water samples. Good linearity (with R-2>0.99) was shown by this FQ detection system for FQ concentrations from 5 to 1000ngL(-1). Moreover, low detection limits (0.7-6.0ngL(-1)) and quantitation limits (2.5-20.0ngL(-1)) and satisfactory repeatability (relative standard deviation <10, n=6) were achieved for water samples. The developed method was also validated for the analysis of FQs in meat and milk samples. Finally, FQs in food and drinking water samples were successfully determined using the developed method.