色谱 ›› 2014, Vol. 32 ›› Issue (4): 413-418.DOI: 10.3724/SP.J.1123.2013.11015

• 庆祝《色谱》创刊三十周年暨卢佩章院士九十华诞专刊-研究论文 • 上一篇    下一篇

四氧化三铁/单壁碳纳米管磁性复合纳米粒子分散固相微萃取-高效液相色谱法测定牛奶中的香精添加剂

李海芳1, 杨红云2, 张英1, 王培龙3, 林金明1   

  1. 1. 清华大学化学系, 北京 100084;
    2. 国家人造板与木竹制品质量监督检验中心, 北京 100091;
    3. 中国农业科学院农业质量标准与检测技术研究所, 北京 100081
  • 收稿日期:2013-11-06 修回日期:2014-01-15 出版日期:2014-04-08 发布日期:2014-03-28
  • 通讯作者: 林金明
  • 基金资助:

    高等学校博士学科点专项科研基金项目(20110002110052);国家“211工程”项目“高等学校仪器设备和优质资源共享系统”(CERS-1-75).

Dispersive solid phase microextraction of vanillins in milk using magnetic nanoparticles of ferroferric oxide/carbon nanotubes combining with high performance liquid chromatography analysis

LI Haifang1, YANG Hongyun2, ZHANG Ying1, WANG Peilong3, LIN Jin-Ming1   

  1. 1. Department of Chemistry, Tsinghua University, Beijing 100084, China;
    2. National Center for Quality Supervision and Testing of Wood and Bamboo Products, Beijing 100091, China;
    3. Institute of Quality Standard and Testing Technology for Agro-Products of Chinese Academy of Agricultural Sciences, Beijing 100081, China
  • Received:2013-11-06 Revised:2014-01-15 Online:2014-04-08 Published:2014-03-28

摘要:

通过化学键合的方法制备单壁碳纳米管包覆的四氧化三铁(Fe3O4/CNTs)磁性复合纳米粒子。首先用水热法合成磁性Fe3O4纳米粒子,并进行硅烷氨基化处理,羧基化的单壁碳纳米管通过1-(3-二甲基氨基丙基)-3-乙基碳二亚胺(EDC)和N-羟基琥珀酰亚胺(NHS)交联剂反应修饰到Fe3O4纳米颗粒表面。合成的Fe3O4/CNTs复合纳米粒子具有很高的磁响应度和很好的分散能力,是一种很好的分散固相萃取剂。本研究将合成的Fe3O4/CNTs纳米粒子用于分散固相微萃取富集牛奶中的香精添加剂,并与高效液相色谱分析联用,实现了香兰素和乙基香兰素的快速高效富集和高灵敏度检测,两者的检出限达10 μg/L,回收率大于92%。本研究表明,合成的Fe3O4/CNTs磁性复合粒子是一种很好的奶制品中香兰素添加剂的样品前处理富集材料。

关键词: 磁性纳米粒子, 单壁碳纳米管, 高效液相色谱, 牛奶, 四氧化三铁, 香精添加剂

Abstract:

Magnetic nanoparticles of ferroferric oxide/carbon nanotubes (Fe3O4/CNTs) were synthesized by chemically bonding single-walled carbon nanotubes (SWCNTs) to the Fe3O4 nanoparticles. The pretreated carboxyl SWCNTs were modified on the surface of amino-functioned Fe3O4 nanoparticles through the cross-linking reaction between 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDC) and N-hydroxysuccinimide (NHS). The synthesized Fe3O4/CNTs nanoparticles presented high super paramagnetic property and good dispersion ability, and were considered as good candidate adsorbents for dispersive solid phase microextraction. In this work, the synthesized Fe3O4/CNTs nanoparticles were applied to the extraction of vanillin additives, which was combined with high performance liquid chromatography (HPLC) analysis. The rapid and efficient preconcentration of vanillin and ethyl vanillin from different milk samples were successfully obtained with the detection limits of 10 μg/L and satisfactory recoveries of more than 92%. The results indicated that Fe3O4/CNTs magnetic nanoparticles were good pretreatment alternatives for the concentration of vanillin additives in milk products.

Key words: ferroferric oxide, high performance liquid chromatography (HPLC), magnetic nanoparticles, milk, single-walled carbon nanotubes (SWCNTs), vanillin additives

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