期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1371, 期 -, 页码 74-81出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2014.10.088
关键词
Fe3O4/MIL-101; Magnetic solid-phase extraction; Organophosphorus pesticides; Biological samples
资金
- National Natural Science Foundation of China [21305026, 21305013]
- Zhejiang Provincial Natural Science Foundation of China [LQ13B050005]
- Scientific Research Foundation of Hangzhou Dianzi University [KYS205612034]
An active magnetic metal-organic framework (MOF) hybrid material was prepared using a novel in situ solvothermal method in the presence of magnetite (Fe3O4) particles, that holds much promise for largescale synthesis. MIL-101(Fe), an iron terephthalate with pore structure and high resistance to water and common solvents, was functionalized as a model with superparamagnetic qualities, using Fe3O4. The electrostatic interaction between Fe3O4 and metal ions was thereby used to chemically stabilize magnetic nanoparticles, and thus MOF crystals were uniformly enclosed by Fe(3)o(4) to form a homogeneous magnetic product identified as a Fe3O4/MIL-101 composite. This hybrid material with magnetic susceptibility but with the lowest possible loading amount of Fe3O4 was examined, and its potential application for magnetic solid-phase extraction of six organophosphorus pesticides (OPPs) from human hair and urine samples, followed by gas chromatography analysis, was assessed. The main effect parameters including solution ionic strength, desorption solvent, extraction time and desorption time were investigated in sequence. Under optimized conditions, this method showed low detection limits (0.21-2.28 ng/mL), wide linearity, and good precision (1.8-8.7% for intra-day, 2.9-9.4% for inter-day). The matrix interference produced by hair or urine could be effectively eliminated using this method, and satisfactory recoveries of the spiked samples were 76.8-94.5% and 74.9-92.1%, respectively, indicating that the Fe3O4/MIL-101 sorbents are feasible for the analysis of trace analytes from biological samples. (C) 2014 Published by Elsevier B.V.
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