Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo, Zhejiang 315010, China; Ningbo Key Laboratory of Poison Research and Control, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China.
Ningbo Institute of Technology, Zhejiang University, Ningbo, Zhejiang 315100, China.
Anal Chim Acta. 2016 May 5;919:34-46. doi: 10.1016/j.aca.2016.02.035. Epub 2016 Mar 16.
In this study, graphene oxide-encapsulated core-shell magnetic microspheres (GOE-CS-MM) were fabricated by a self-assemble approach between positive charged poly(diallyldimethylammonium) chloride (PDDA)-modified Fe3O4@SiO2 and negative charged GO sheets via electrostatic interaction. The as-prepared GOE-CS-MM was carefully characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), vibrating sample magnetometer analysis (VSM), and X-ray photoelectron spectroscopy (XPS), and was used as a cleanup adsorbent in magnetic solid-phase extraction (MSPE) for determination of 15 trace-level environmental phenols in seafood coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS). The obtained results showed that the GOE-CS-MM exhibited excellent cleanup efficiency and could availably reduce the matrix effect. The cleanup mechanisms were investigated and referred to π-π stacking interaction and hydrogen bond between GOE-CS-MM and impurities in the extracts. Moreover, the extraction and cleanup conditions of GOE-CS-MM toward phenols were optimized in detail. Under the optimized conditions, the limits of detection (LODs) were found to be 0.003-0.06 μg kg(-1), and satisfactory recovery values of 84.8-103.1% were obtained for the tested seafood samples. It was confirmed that the developed method is simple, fast, sensitive, and accurate for the determination of 15 trace environmental phenols in seafood samples.
在这项研究中，通过正电荷聚二烯丙基二甲基氯化铵（PDDA）修饰的 Fe3O4@SiO2 与带负电荷的 GO 片之间的静电相互作用，制备了氧化石墨烯包裹的核壳型磁性微球（GOE-CS-MM）。通过扫描电子显微镜（SEM）、透射电子显微镜（TEM）、振动样品磁强计分析（VSM）和 X 射线光电子能谱（XPS）对所制备的 GOE-CS-MM 进行了仔细的表征，并将其用作磁性固相萃取（MSPE）中的净化吸附剂，用于结合液相色谱-串联质谱法（LC-MS/MS）测定海鲜中的 15 种痕量环境酚类物质。结果表明，GOE-CS-MM 表现出优异的净化效率，可有效降低基质效应。研究并提到了 GOE-CS-MM 与提取物中杂质之间的π-π堆积相互作用和氢键的净化机制。此外，详细优化了 GOE-CS-MM 对酚类物质的萃取和净化条件。在优化条件下，所测试海鲜样品的检出限（LODs）为 0.003-0.06μgkg-1，回收率为 84.8-103.1%。证实该方法简单、快速、灵敏、准确，可用于测定海鲜样品中 15 种痕量环境酚类物质。
