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-C16) 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°) 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 1-1000 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 ng L-1 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.

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

254th National Meeting (2017)

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