Although parabens are useful due to their antiseptic properties, their widespread use has caused concerns regarding their potential toxicological effects. In this study, a novel magnetic solid-phase extraction combined with ultra-high-performance liquid chromatography-tandem mass spectrometry (MSPE-UHPLC-MS/MS) was developed, based on ordered magnetic mesoporous carbon (MMC), for paraben analysis. The MMC was prepared by soft-template synthesis, with a unique pore structure and a highly specific surface response, indicating potential as an excellent adsorbent. Several parameters affecting the paraben extraction efficiency were investigated and a novel method for paraben analysis in serum and urine samples using MSPE-UHPLCMS/MS was developed. The concentrations of methylparaben, ethylparaben, isopropylparaben, and propylparaben in these samples were 0.0380–4.36, 0.460–9.65, 0.0118–0.770, and 0.0363–0.641 μg/L, respectively, whereas isobutylparaben and butylparaben were not detected. Furthermore, satisfactory recoveries of 76.4–121% with relative standard deviations (n = 5) of 1.9–8.6% were obtained. Therefore, the developed MSPE-UHPLC-MS/MS method was efficient, highly sensitive, and reliable for analysing parabens in complex biological samples.
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