Magnetic Metal-Organic Framework/Graphene Oxide-Based Solid-Phase Extraction Combined with Spectrofluorimetry for the De
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Magnetic Metal-Organic Framework/Graphene Oxide-Based Solid-Phase Extraction Combined with Spectrofluorimetry for the Determination of Enrofloxacin in Milk Sample Zhaoqian Li 1 & Mengyu Qi 1 & Chunyan Tu 1 & Weiping Wang 1 & Jianrong Chen 2 & Ai-Jun Wang 2
Received: 17 March 2017 / Accepted: 12 June 2017 # Springer Science+Business Media, LLC 2017
Abstract We have developed an analytical method for the extraction and determination of enrofloxacin in milk sample by magnetic solid-phase extraction with metal-organic framework/graphene oxide (Fe3O4/MIL-100(Fe)/GO) as a sorbent coupling to spectrofluorimetry. The prepared Fe3O4/MIL-100(Fe)/GO nanocomposite were characterized by scanning electron microscopy, FT-IR spectroscopy, xray diffraction, and vibration sample magnetometer. The parameters affecting extraction efficiency including sample pH, amounts of sorbent, adsorption time, and acidity of elution solvent were optimized systematically. The optimal extraction conditions were as follows: 100.0-mL sample at pH of 8.0, 20.0 mg of Fe3O4/MIL-100(Fe)/GO as sorbent, extraction time of 30 min, and 4.00 mL of 15% (v/v) formic acid in methanol as eluent. A matrix-matched linear relationship (10.00–350.00 μg L−1) between the fluorescence intensity and the concentrations of enrofloxacin was obtained with correlation coefficient (r) = 0.9979. The limit of detection (S/N = 3) and the limit of quantification (S/N = 10) were 0.65 and 2.17 μg L−1, respectively. The relative standard deviations of intraday and interday analysis (n = 5) were 1.64 and 2.86%, respectively. The proposed method was successfully applied for the determination of enrofloxacin in milk sample with recoveries ranged from 85.7 to 106.3%.
* Weiping Wang [email protected]
1
College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua 321004, China
2
College of Geography and Environmental Sciences, Zhejiang Normal University, Jinhua 321004, China
Keywords Magnetic metal-organic framework/graphene oxide (Fe3O4/MIL-100(Fe)/GO) . Magnetic solid-phase extraction . Enrofloxacin . Spectrofluorimetry . Milk sample
Introduction Fluoroquinolones (FQs) are an important class of synthetic antibiotics used in human therapy (since the 1980s) and veterinary (since the 1990s) pharmaceuticals (Golet et al. 2002). Their activity is based on the inhibition of bacterial DNA, which prevents bacterial multiplication. Enrofloxacin (ENR), the second generation of the FQs, shows excellent antibacterial activity against a broad spectrum of Gram-negative and Gram-positive bacteria. ENR is effective against Escherichia coli, Enterobacter, Salmonella, Staphylococcus, etc. (Andreu et al. 2007). In the past years, the extensive use of ENR in veterinary has promoted the persistence of antibiotic residues in foodstuffs of animal origin, which would cause harmful effects on human health, such as toxic effects, allergic reactions, resistance to antibiotics, etc. (Andreu et al. 2007; Li and Chauhan 2006). To protect consumer health, the maximum residue levels (MRLs) for EN
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