色谱

色谱 ›› 2019, Vol. 37 ›› Issue (3): 293-298.DOI: 10.3724/SP.J.1123.2018.11026

• 研究论文 • 上一篇    下一篇

绿原酸亲水性磁性分子印迹树脂的合成及其固相萃取性能评价

彭胜1,2, 李奂3, 施树云1,2,3   

  1. 1. 吉首大学林产化工工程湖南省重点实验室, 湖南 张家界 427000;
    2. 吉首大学杜仲综合利用技术国家地方联合工程实验室, 湖南 吉首 416000;
    3. 中南大学化学化工学院, 湖南 长沙 410083
  • 收稿日期:2018-11-18 出版日期:2019-03-08 发布日期:2015-01-21
  • 通讯作者: 施树云.E-mail:shishuyun@126.com.
  • 基金资助:

    国家自然科学基金（81673585）；林产化工工程湖南省重点实验室项目（JDZ201802）；杜仲综合利用技术国家地方联合工程实验室项目（NLE201601）.

Preparation of hydrophilic, magnetic molecularly imprinted resins of chlorogenic acid and evaluation of its solid-phase extraction performance

PENG Sheng1,2, LI Huan3, SHI Shuyun1,2,3   

  1. 1. Key Laboratory of Hunan Forest Products and Chemical Industry Engineering, Jishou University, Zhangjiajie 427000, China;
    2. National & Local United Engineering Laboratory of Integrative Utilization Technology of Eucommiaulmoides, Jishou University, Jishou 416000, China;
    3. College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China
  • Received:2018-11-18 Online:2019-03-08 Published:2015-01-21
  • Supported by:

    National Natural Science Foundation of China (No. 81673585); Project of Key Laboratory of Hunan Forest Products and Chemical Industry Engineering (No. JDZ201802); Project of National & Local United Engineering Laboratory of Integrative Utilization Technology of Eucommia ulmoides (No. NLE201601).

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摘要：

以绿原酸（CGA）为模板分子、间苯二酚和三聚氰胺为双功能单体、甲醛为交联剂在磁性介孔二氧化硅（Fe3O4@mSiO2）的介孔中一步聚合形成亲水性磁性分子印迹树脂（MMIRs）。除去mSiO2载体后，MMIRs具有多孔结构且印迹位点位于材料表面。透射电镜、傅里叶变换红外光谱、振动样品磁强计、热重分析和水接触角实验表明：分子印迹聚合物层成功地包覆在Fe3O4表面，MMIRs具有良好的亲水性和磁固相萃取性能。MMIRs对CGA具有较强的吸附容量（50.87 mg/g）、较快的吸附速率（吸附平衡时间70 min）和较好的特异性吸附性能。将MMIRs用于杜仲黑茶中CGA的选择性分离，采用高效液相色谱分析检测，检出限为0.7 mg/L，回收率为93.1%~109.4%，相对标准偏差（RSD）小于9.6%。结果表明MMIRs可简单、快速、高选择性地分离富集复杂水体系样品中的CGA。

关键词: 复杂样品, 高效液相色谱, 固相萃取, 绿原酸, 亲水性分子印迹树脂

Abstract:

Hydrophilic, magnetic molecularly imprinted resins (MMIRs) were fabricated inside Fe3O4@mSiO2 pores by the one-pot copolycondensation of chlorogenic acid (CGA), resorcinol, melamine, and formaldehyde. The final porous MMIRs with larger numbers of surface recognition sites were obtained by removing mSiO2. The successful preparation of MMIRs was confirmed using transmission electron microscopy, Fourier transform infrared spectroscopy, vibrating sample magnetometry, thermo-gravimetric analysis, and water contact angle analysis. The analyses suggest that the MMIRs have excellent hydrophilicity and magnetic solid-phase extraction efficiency. The MMIRs had a good adsorption capacity (50.87 mg/g), fast rate of adsorption (equilibrium was attained at 70 min), and specific recognition for CGA. The MMIRs, in combination with high performance liquid chromatography, were directly used for the selective extraction and determination of CGA in Duzhong brick tea. The limit of detection and recovery were 0.7 mg/L and 93.1%-109.4%, respectively, with relative standard deviations of less than 9.6%. The proposed strategy was extremely promising for the facile, rapid, and selective determination of CGA in real aqueous samples.

Key words: chlorogenic acid, complex sample, high performance liquid chromatography (HPLC), hydrophilic molecularly imprinted resin, solid phase extraction (SPE)

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