Facile preparation of hexadecyl-functionalized magnetic core-shell microsphere for the extraction of polychlorinated biphenyls in environmental waters

Alkyl moieties which can retain target analytes due to their lipophilicity are important in sample preparation. In this work, hexadecyl-functionalized magnetic core-shell microspheres (Fe3O4@SiO2-C-16) was successfully prepared by one-pot sol-gel method and used for magnetic solid-phase extraction of polychlorinated biphenyls (PCBs) in environmental water samples. Optimized preparation method was achieved by altering the adding moment of hexadecyl-silane. The resultant materials were systematically characterized by scanning electron microscope, transmission electron microscope, Fourier transform infrared spectroscopy, energy dispersive X-ray spectrometry, tensionmeter, and vibrating sample magnetometer. The results demonstrated that the optimized adsorbent exhibited core-shell structure, superparamagnetic (66 emu/g), and extremely hydrophobic (water contact angle of 122 degrees) properties. To evaluate the extraction performance, the prepared material coupled with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) was applied to determinate PCBs. The extraction conditions were optimized. Under the optimal conditions, the proposed method showed a good linearity range of 1-100 ng L-1 with correlation coefficients (R) of 0.9989-0.9993. Based on a signal-to-noise ratio of 3 and 10, the limits of detection (LODs) and limits of quantification (LOQs) were in the range 0.14-0.27 and 0.39-0.91 ng L-1, respectively. The intra- and inter-day relative standard deviations (RSDs) were less than 9.06%. The absolute recoveries of PCBs in spiked real water samples were in the range of 75.17 to 101.20%. Additionally, reusability and batch-to-batch reproducibility of the resultant material were acceptable with RSDs less than 5.64 and 3.25%, respectively.