4.5 Article

Decyl-perfluorinated magnetic mesoporous microspheres for extraction and analysis perfluorinated compounds in water using ultrahigh-performance liquid chromatography-mass spectrometry

Journal

JOURNAL OF SEPARATION SCIENCE
Volume 35, Issue 19, Pages 2629-2636

Publisher

WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201200300

Keywords

Extraction and enrichment; Fluorous affinity; Interior-walls perfluorinated functionalized magnetic mesoporous microspheres; Perfluorinated compounds; Ultrahigh-performance liquid chromatography (UHPLC)-ESI; MS; MS

Funding

  1. National Basic Research Priorities Program [2012CB910601]
  2. National Natural Science Foundation of China [21075022, 20875017, 21105016]
  3. Graduate Innovation Fund of Fudan University
  4. Research Fund for the Doctoral Program of Higher Education of China [20110071110007, 20100071120053]
  5. Shanghai Municipal Natural Science Foundation [11ZR1403200]
  6. Shanghai Leading Academic Discipline Project [B109]

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In this work, the interior-walls decyl-perfluorinated functionalized magnetic mesoporous microspheres (F17Fe3O4@mSiO2) were synthesized for the first time, and applied as adsorbents to extract and concentrate perfluorinated compounds (PFCs) from water samples. The fluorous functionalized interior pore-walls contributed to the high-selective preconcentration of PFCs due to fluorous affinity; and abundant silanol groups on the exterior surface of microspheres contributed to the good dispersibility in water sample. Four kinds of PFCs were selected as model analytes, including perfluorooctanoic acid, perfluorononanoic acid, perfluorododecanoic acid, and perfluorooctane sulphonate. In addition, UHPLC-ESI/MS/MS was introduced to the fast and sensitive detection of the analytes after sample pretreatment. Important parameters of the extraction procedure were optimized, including salinity, eluting solvent, the amount of F17Fe3O4@mSiO2 microspheres, and extraction time. The optimized procedure took only 10 min to extract analytes with high recoveries and merely 800-mu L acetonitrile to elute analytes from the magnetic adsorbents. Validation experiments showed good linearity (0.9940.998), precision (2.67.6%), high recovery (93.4105.7%) of the proposed method, and the limits of detection were from 0.008 to 0.125 mu g/L. The F17Fe3O4@mSiO2 magnetic microspheres have the advantages of great dispersibility in aqueous solution, high specificity of extraction, large surface area, and efficient separation ability. The results showed that the proposed method based on F17Fe3O4@mSiO2 microspheres is a simple, fast, and sensitive tool for the analysis of PFCs in water sample.

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