In this study, nitrogen-doped hollow multi-shelled carbon-silicon nanospheres (NSiC-Homs-NS) were prepared using a template method and employed as a coating material for solid-phase microextraction (SPME) fibers. The extraction efficiency of single-, double-, triple-, and quadruple-shelled NSiC-Homs-NS coated fibers for polycyclic aromatic hydrocarbons (PAHs) were investigated, respectively. The NSiC-Homs-NS based SPME fiber coupled with gas chromatography-mass spectrometry was applied to detect 19 PAHs in milk samples. The extraction parameters of SPME were optimized using a central composite design methodology. Under the optimized conditions, the established method exhibited good linearity for the PAHs, ranging from 0.03 to 500 ng g-1, with coefficients of determination (r2) between 0.9952 and 0.9983. The limits of detection (S/N of 3) of the PAHs in milk samples ranged from 0.01 to 4.0 ng g-1. The relative standard deviations of the single-fiber repeatability (n = 5) and fiber-to-fiber reproducibility (n = 5) were all less than 12 %. The method recoveries of the PAHs in seven milk samples, evaluated at three different spiking concentrations, ranged from 80.4 % to 119 % with RSDs less than 12 %. The developed method exhibited good repeatability and accuracy.
Keywords: Gas chromatograph-mass spectrometer; Milk sample; Multi-shelled carbon-silicon nanosphere; Polycyclic aromatic hydrocarbons; Solid-phase microextraction.
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