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Graphene‐Fe 3 O 4 as a magnetic solid‐phase extraction sorbent coupled to capillary electrophoresis for the determination of sulfonamides in milk
Author(s) -
Li Zhaoqian,
Li Yazhen,
Qi Mengyu,
Zhong Shuxian,
Wang Weiping,
Wang AiJun,
Chen Jianrong
Publication year - 2016
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201600308
Subject(s) - capillary electrophoresis , analytical chemistry (journal) , extraction (chemistry) , solid phase extraction , graphene , chromatography , chemistry , detection limit , nanoparticle , magnetic nanoparticles , sorbent , materials science , adsorption , nanotechnology , organic chemistry
Graphene‐Fe 3 O 4 nanoparticles were prepared using one‐step solvothermal method and characterized by X‐ray diffraction, FTIR spectroscopy, scanning electron microscopy, and vibrating sample magnetometry. The results demonstrated that Fe 3 O 4 nanoparticles were homogeneously anchored on graphene nanosheets. The as‐synthesized graphene‐Fe 3 O 4 nanoparticles were employed as sorbent for magnetic solid‐phase extraction of sulfonamides in milk prior to capillary electrophoresis analysis. The optimal capillary electrophoresis conditions were as follows: 60 mmol/L Na 2 HPO 4 containing 2 mmol/L ethylenediaminetetraacetic acid disodium salt and 24% v/v methanol as running buffer, separation voltage of 14 kV, and detection wavelength of 270 nm. The parameters affecting extraction efficiency including desorption solution, the amount of graphene‐Fe 3 O 4 nanoparticles, extraction time, and sample pH were investigated in detail. Under the optimal conditions, good linearity (5–200 μg/L) with correlation coefficients ≥0.9910 was obtained. The limits of detection were 0.89–2.31 μg/L. The relative standard deviations for intraday and interday analyses were 4.9–8.5 and 4.0–9.0%, respectively. The proposed method was successfully applied to the analysis of sulfonamides in milk samples with recoveries ranging from 62.7 to 104.8% and relative standard deviations less than 10.2%.