Magnetic metal-organic frameworks coated stir bar sorptive extraction coupled with GC-MS for determination of polychlorinated biphenyls in fish samples

In this work, several kinds of the metal-organic framework (MOF) were evaluated the adsorption performance to PCB. Finally, MOF-5(Fe) was introduced in stir bar sorptive extraction (SBSE) as the adsorbent to extract six polychlorinated biphenyls (PCBs). Nd-Fe-B permanent magnet was employed as stir bar, which was then coated with Fe3O4-MOF-5(Fe) composite magnetic material, which was prepared by solvothermal method. The stir bar was then employed to extract and enrich six indicator PCBs (2,2',5,5'-tetrachlorobiphenyl, 2,2',4,5,5'-pentachlorobiphenyl, 2,2',3,4,4',5-hexachlorobiphenyl, 2,3,4,4,5-pentachlorobiphenyl, 2,2',4,4',5,5'-hexachlorobiphenyl, 2,2',3,4,4',5,5'-heptachlorobiphenyl) under stirring, then eluted by n-hexane under ultrasound. Its saturated adsorption amount was found to be 17.0-17.8 mg g(-1) and only 30 min were needed to reach adsorption equilibrium. The MOF-stir bar can be reused for 60 times with the recovery above 80%, which exhibited good stability. Under the optimal experimental conditions, MOF-5(Fe) based SBSE was coupled with GC-MS for detecting six PCBs. The limits of detection (S/N=3) of the developed method were 0.061-0.096 ng g(-1), with enrichment factors of 50-100 fold. And the linear ranges were 0.01-500 mu L-1. The new method was successfully applied to assess PCBs in fish samples with satisfactory recovery ranging from 94.3% to 97.5%. (C) 2015 Elsevier B.V. All rights reserved.