色谱

色谱 ›› 2019, Vol. 37 ›› Issue (9): 932-938.DOI: 10.3724/SP.J.1123.2019.03005

• 研究论文 • 上一篇    下一篇

替米考星磁性表面分子印迹聚合物的制备及应用

夏张悦怿, 杨丙成, 章飞芳, 梁鑫淼   

  1. 华东理工大学药学院, 制药工程与过程化学教育部工程研究中心, 上海 200237
  • 收稿日期:2019-03-05 出版日期:2019-09-08 发布日期:2015-07-30
  • 通讯作者: 章飞芳
  • 基金资助:
    国家自然科学基金（21477037）.

Preparation and application of tilmicosin-templated magnetic surface molecularly imprinted polymer

XIA Zhangyueyi, YANG Bingcheng, ZHANG Feifang, LIANG Xinmiao   

  1. Engineering Research Center of Pharmaceutical Process Chemistry, Ministry of Education, School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China
  • Received:2019-03-05 Online:2019-09-08 Published:2015-07-30
  • Supported by:
    National Natural Science Foundation of China (No. 21477037).

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摘要： 报道了一种替米考星磁性表面分子印迹聚合物吸附剂。它以Fe3O4@SiO2为磁性基质，替米考星为模板分子，甲基丙烯酸为功能单体，通过硅烷化反应在Fe3O4@SiO2表面键合上3-（甲基丙烯酰氧）丙基三甲氧基硅烷制备得到。该吸附剂对大环内酯类抗生素表现出高选择性和高富集能力（对4种模型大环内酯的富集倍数为212~675倍）。相比传统的非表面分子印迹聚合物，吸附平衡时间可缩短为30 min，可以重复使用至少6次；结合高效液相色谱-紫外检测，将该吸附剂应用于奶粉中4种大环内酯类抗生素的残留检测，所得检出限和定量限分别为0.58~1.36 μg/kg和1.92~4.55 μg/kg，日内（n=5）和日间（n=3）回收率在83.2%~123.0%之间，RSD均小于12.2%。

关键词: 表面分子印迹聚合物, 磁性固相萃取, 大环内酯类抗生素, 高效液相色谱, 奶粉

Abstract: A novel magnetic surface molecularly imprinted adsorbent is described. Fe3O4@SiO2, tilmicosin, and methacrylic acid were chosen as the support substrate, template molecule, and functional monomer, respectively. 3-Methacryloxypropyltrimethoxysilane was chemically bonded onto the surface of Fe3O4@SiO2 via a silanization reaction and used as the crosslinking agent in the subsequent reaction. The obtained magnetic surface molecularly imprinted polymer (MS-MIP) showed high selectivity and high enrichment capacity towards macrolide antibiotics (MACs), as indicated by the 212-, 275-, 675-, and 293-fold enrichment factors for spiramycin, josamycin, tilmicosin, and tylosin tartrate, separately. Because of the marked cavities onto the surface of the MS-MIP, the time required to reach adsorption equilibrium (30 min) was shorter than that for traditional MIP sorbents. Moreover, the adsorbent could be reused at least 6 times. Finally, the MS-MIP was used in combination with high performance liquid chromatography-ultraviolet detection (HPLC-UV) for the extraction and enrichment of four MACs in milk powder samples. The limits of detection (LODs) and limits of quantitation (LOQs) for the four MACs were in the range of 0.58-1.36 μg/kg and 1.92-4.55 μg/kg, respectively. The interday (n=5) and intraday (n=3) recoveries were in the range of 83.2%-123.0% at three spiked levels of 80, 200, and 500 μg/kg, under all the experimental conditions employed, and the relative standard deviations were less than 12.2%.

Key words: high performance liquid chromatography (HPLC), macrolide antibiotics, magnetic solid phase extraction, milk powder, surface molecularly imprinted polymer

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