Synthesis of a Carboxyl-functionalized Magnetic Carbon Nanotube and Its Extraction for Clenbuterol in Pork Samples
  
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KeyWord:clenbuterol  ractopamine  oxidation-precipitation  carbon nanotube  magnetic solid extraction  ultra-high performance liquid chromatography
  
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LIAN Li-li,CHEN Bai-sen,DENG Yi-hui,WANG Xi-yue,ZHANG Ling-he,LOU Da-wei Department of Analytical Chemistry,Jilin Institute of Chemical Technology,Jilin ,China
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Abstract:
      A carboxyl-functionalized magnetic carbon nanotube of Fe3O4-Cys@CNT was synthesized by a facile oxidation-precipitation method under the ultrasonic-assisted condition,with Fe2+,oxygen and L-cysteine(L-Cys) as ferrous precursor,oxidant and protectant,respectively.The obtained magnetic carbon nanotube was characterized by Fourier transform-infrared spectroscopy(FT-IR),X-ray diffractometry(XRD) and transmission electron microscopy(TEM).The results showed that Fe3O4-Cys NPs with a diameter of 20 nm was homogeneously distributed on the surface of CNT.Based on this,an ultra-high performance liquid chromatography with magnetic solid-phase extraction(MSPE/UPLC) was established for the analysis of clenbuterol(CLB) and ractopamine(RAC) in pork samples via using Fe3O4-Cys@CNT as the adsorbent.Under the optimal extraction conditions,there were good linear relationships for CLB and RAC in the concentration range of 0.5-100 μg/L,with correlation coefficients(r) not less than 0.997 4 and the limits of detection(LOD) of 0.15 μg/L.The recoveries for CLB and RAC ranged from 95.1% to 112%,with relative standard deviations(RSD) less than 11%.The extraction efficiency of Fe3O4-Cys@CNT reduced less than 3% after it was used repeatedly for 4 times,indicating that the adsorbent was recyclable.With the advantages of simple preparation,short synthesis time and environmental protection,the Fe3O4-Cys@CNT prepared is a promising MSPE adsorbent,which could separate and enrich CLB and RAC in complex matrix rapidly.The preparation method of the new adsorbent and the established method provide new ideas for the detection of clenbuterol in complex food and biological samples.
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