title: Three Birds with One Fe3O4 Nanoparticle: Integration of Microwave Digestion, Solid Phase Extraction, and Magnetic Separation for Sensitive Determination of Arsenic and Antimony in Fish.
abstract: An environmentally friendly and fast sample treatment approach that integrates accelerated microwave digestion (MWD), solid phase extraction, and magnetic separation into a single step was developed for the determination of arsenic and antimony in fish samples by using Fe3O4 magnetic nanoparticles (MNPs). Compared to conventional microwave digestion, the consumption of HNO3 was reduced significantly to 12.5%, and the digestion time and temperature were substantially decreased to 6 min and 80 °C, respectively. This is largely attributed to Fe3O4 magnetic nanoparticles being a highly effective catalyst for rapid generation of oxidative radicals from H2O2, as well as an excellent absorber of microwave irradiation. Moreover, potential interferences from sample matrices were eliminated because the As and Sb species adsorbed on the nanoparticles were efficiently separated from the digests with a hand-held magnet prior to analysis. Limits of detection for arsenic and antimony were in the range of 0.01-0.06 μg g(-1) and 0.03-0.08 μg g(-1) by using hydride generation atomic fluorescence spectrometry, respectively, and further improved to 0.002-0.005 μg g(-1) and 0.005-0.01 μg g(-1) when inductively coupled plasma mass spectrometry was used as a detector. The precision of replicate measurements (n = 9) was better than 6% by analyzing 0.1 g test sample spiked with 1 μg g(-1) arsenic and antimony. The proposed method was validated by analysis of two certified reference materials (DORM-3 and DORM-4) with good recoveries (90%-106%).
authors.forename: Yun
authors.initials: Y
authors.lastname: Jia
authors.forename: Huimin
authors.initials: H
authors.lastname: Yu
authors.forename: Li
authors.initials: L
authors.lastname: Wu
authors.forename: Xiandeng
authors.initials: X
authors.lastname: Hou
authors.affiliation: §Chemical Metrology, Measurement Science and Standards, National Research Council Canada, Ottawa, Canada, K1A 0R6.
authors.forename: Lu
authors.initials: L
authors.lastname: Yang
authors.forename: Chengbin
authors.initials: C
authors.lastname: Zheng
mesh_terms: D000818:Animals; D000965:Antimony / Q000032:analysis*; D001151:Arsenic / Q000032:analysis*; D005399:Fishes; D060328:Magnetic Phenomena; D058185:Magnetite Nanoparticles / Q000737:chemistry*; D008872:Microwaves; D052616:Solid Phase Extraction
chemical_list: D058185:Magnetite Nanoparticles; D000965:Antimony; D001151:Arsenic