色谱 ›› 2018, Vol. 36 ›› Issue (8): 723-729.DOI: 10.3724/SP.J.1123.2018.03034

• 研究论文 • 上一篇    下一篇

螺旋霉素分子印迹磁性纳米吸附剂的合成及应用

孙佳佳, 章飞芳, 梁鑫淼   

  1. 华东理工大学药学院, 上海 200237
  • 收稿日期:2018-03-27 出版日期:2018-08-08 发布日期:2014-06-28
  • 通讯作者: 章飞芳,Tel:(021)64250627,E-mail:zhangff@ecust.edu.cn
  • 基金资助:

    国家自然科学基金(21477037).

Synthesis and application of a magnetic spiramycin-templated molecularly imprinted nanoparticle adsorbent

SUN Jiajia, ZHANG Feifang, LIANG Xinmiao   

  1. School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China
  • Received:2018-03-27 Online:2018-08-08 Published:2014-06-28
  • Supported by:

    National Natural Science Foundation of China (No.21477037).

摘要:

制备了一种以螺旋霉素为模板分子的分子印迹磁性纳米吸附剂。以磁性纳米Fe3O4为内核,经丙烯酸表面修饰后再以螺旋霉素为模板分子、甲基丙烯酸为功能单体、乙二醇二甲基丙烯酸酯为交联剂,通过表面自由基聚合反应制备得到。该吸附剂对螺旋霉素、交沙霉素、替米考星和酒石酸泰乐菌素4种大环内酯类抗生素表现出良好的富集效果(富集倍数分别为310、118、758和72),其选择性明显优于常规C18吸附剂。该吸附剂可重复使用至少6次。结合高效液相色谱-紫外检测器建立了上述4种抗生素的分析方法。方法检出限为0.53~2.75 μg/L,定量限为1.78~9.16 μg/L;在50、100和150 μg/L低中高3个添加水平下,方法回收率在80.78%~123.02%之间,相对标准偏差<15.8%(n=5)。该方法被应用于分析蜂蜜中的上述4种抗生素。

关键词: 磁性分子印迹纳米颗粒, 大环内酯类抗生素, 蜂蜜, 高效液相色谱, 吸附剂

Abstract:

A magnetic spiramycin-templated molecularly imprinted nanoparticle adsorbent is described. It was synthesized by choosing Fe3O4 nanoparticles as the core, and then modified with acrylic acid, followed by the addition of spiramycin as a template molecule, methacrylic acid as a functional monomer, and ethylene glycol dimethacrylate as a crosslinking agent. Finally, the adsorbent was prepared via surface radical polymerization. The adsorbent demonstrated effective enrichment for four macrolide antibiotics (MA) including spiramycin, josamycin, tilmicosin, and tylosin tartrate, whose enrichment factors were 310, 118, 758, and 72, respectively. Its selectivity toward the trace MA was obviously higher than that of the common C18 adsorbent. In addition, the adsorbent also showed favorable reusability (at least six times). A corresponding analytical method for MA was established by subjecting the adsorbent to high-performance liquid chromatography with ultraviolet absorbance. For the above four model MAs, the limits of detection were in the range of 0.53-2.75 μg/L, and the limits of quantitation were in the range of 1.78-9.16 μg/L. The recoveries of the method were in the range of 80.78%-123.02% for three spiked levels of 50, 100 and 150 μg/L, and the relative standard deviation was less than 15.8% (n=5). The method was used for the determination of the four MAs above in honey.

Key words: adsorbent, high performance liquid chromatography (HPLC), honey, macrolide antibiotics (MA), magnetic molecularly imprinted nanoparticle

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