Synthesis of a Carboxyl-functionalized Magnetic Carbon Nanotube and Its Extraction for Clenbuterol in Pork Samples

LIAN Li-li; CHEN Bai-sen; DENG Yi-hui; WANG Xi-yue; ZHANG Ling-he; LOU Da-wei

doi:10.19969/j.fxcsxb.21051803

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Synthesis of a Carboxyl-functionalized Magnetic Carbon Nanotube and Its Extraction for Clenbuterol in Pork Samples

Experimental Techniques and Methods | 更新时间：2023-01-04

- Synthesis of a Carboxyl-functionalized Magnetic Carbon Nanotube and Its Extraction for Clenbuterol in Pork Samples
- Journal of Instrumental Analysis Vol. 41, Issue 2, Pages: 249-254(2022)
- 作者机构：
  
  吉林化工学院分析化学系，吉林吉林 132022
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.21051803
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连丽丽,陈柏森,邓艺辉等.羧基功能化磁性碳纳米管的制备及其对猪肉中瘦肉精的萃取[J].分析测试学报,2022,41(02):249-254.

LIAN Li-li,CHEN Bai-sen,DENG Yi-hui,et al.Synthesis of a Carboxyl-functionalized Magnetic Carbon Nanotube and Its Extraction for Clenbuterol in Pork Samples[J].Journal of Instrumental Analysis,2022,41(02):249-254.
连丽丽,陈柏森,邓艺辉等.羧基功能化磁性碳纳米管的制备及其对猪肉中瘦肉精的萃取[J].分析测试学报,2022,41(02):249-254. DOI： 10.19969/j.fxcsxb.21051803.

LIAN Li-li,CHEN Bai-sen,DENG Yi-hui,et al.Synthesis of a Carboxyl-functionalized Magnetic Carbon Nanotube and Its Extraction for Clenbuterol in Pork Samples[J].Journal of Instrumental Analysis,2022,41(02):249-254. DOI： 10.19969/j.fxcsxb.21051803.

摘要

该文分别以Fe,2+,、O,2,和半胱氨酸（,L,-Cys）作为铁源、氧化剂和保护剂，在超声辅助条件下，通过氧化－沉淀法制备了羧基功能化磁性碳纳米管复合材料（Fe,3,O,4,－Cys@CNT）。采用傅里叶变换－红外光谱（FT－IR）、X-射线衍射仪（XRD）、透射电镜（TEM）对Fe,3,O,4,－Cys@CNT进行了表征。结果表明，Fe,3,O,4,－Cys NPs均匀地分布在CNT表面，直径约为20 nm。以Fe,3,O,4,－Cys@CNT为吸附剂，建立了猪肉样品中痕量盐酸克伦特罗（CLB）及莱克多巴胺（RAC）的磁性固相萃取/超高效液相色谱（MSPE/UPLC）分析方法。在最佳萃取条件下，CLB与RAC在0.5～100 μg/L质量浓度范围内呈良好的线性关系（,r, ≥ 0.997 4）。该方法对CLB及RAC的检出限均为0.15 μg/L，回收率为95.1%～112%，相对标准偏差小于11%。Fe,3,O,4,－Cys@CNT重复使用4次后萃取效率降低不超过3%，表明Fe,3,O,4,－Cys@CNT可重复使用。所制备的Fe,3,O,4,－Cys@CNT具有制备方法简单、合成时间短、绿色环保等优点，能够实现复杂基质中CLB和RAC的快速分离和富集，是一种具有前景的MSPE吸附剂。新型吸附剂的制备以及新方法的建立为复杂食品和生物样品中瘦肉精的检测提供了新思路。

Abstract

A carboxyl-functionalized magnetic carbon nanotube of Fe,3,O,4,－Cys@CNT was synthesized by a facile oxidation－precipitation method under the ultrasonic-assisted condition，with Fe,2+,，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 Fe,3,O,4,－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 Fe,3,O,4,－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 Fe,3,O,4,－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 Fe,3,O,4,－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．

关键词

盐酸克伦特罗莱克多巴胺氧化－沉淀法碳纳米管磁性固相萃取超高效液相色谱

Keywords

clenbuterolractopamineoxidation－precipitationcarbon nanotubemagnetic solid extractionultra-high performance liquid chromatography

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