色谱

色谱 ›› 2015, Vol. 33 ›› Issue (2): 123-131.DOI: 10.3724/SP.J.1123.2014.10008

• 研究论文 • 上一篇    下一篇

双酚A分子印迹固相微萃取头的快速制备(英文)

胡梅1, 张毅军1, 杨靖华1,2, 周小毛2, 魏竹清1, 丁肖庆1, 张裕平1   

  1. 1. 河南科技学院应用化学所, 河南 新乡 453003;
    2. 湖南农业大学农药研究所, 湖南 长沙 410128
  • 收稿日期:2014-10-20 修回日期:2014-12-02 出版日期:2015-02-08 发布日期:2015-01-24
  • 通讯作者: 张裕平
  • 基金资助:

    National Training Programs of Innovation and Entrepreneurship for Undergraduates (No. 201310467026).

Rapid fabrication of molecularly imprinted polymer fibers for solid phase microextraction of bisphenol A

HU Mei1, ZHANG Yijun1, YANG Jinghua1,2, ZHOU Xiaomao2, WEI Zhuqing1, DING Xiaoqing1, ZHANG Yuping1   

  1. 1. Institute of Applied Chemistry, Henan Institute of Science and Technology, Xinxiang 453003, China;
    2. Pesticide Research Institute, Hunan Agricultural University, Changsha 410128, China
  • Received:2014-10-20 Revised:2014-12-02 Online:2015-02-08 Published:2015-01-24
  • Supported by:

    National Training Programs of Innovation and Entrepreneurship for Undergraduates (No. 201310467026).

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摘要：

以双酚A(BPA)为模板分子,乙腈(ACN)为致孔剂,α-甲基丙烯酸为功能单体(MAA),乙二醇二甲基丙烯酸酯(EDMA)为交联剂,偶氮二异丁腈(AIBN)为引发剂,快速制备了双酚A分子印迹聚合物(MIP)萃取头。聚合反应在内径为530 μm的毛细管中进行,微波聚合7 min。得到的双酚A分子印迹聚合物从毛细管中推出,在安培瓶中洗脱后再次插入毛细管中用于固相微萃取(SPME)。在不同的模板分子和功能单体的比例(BPA/MAA)、NaCl浓度、萃取和解吸时间、pH值和解吸溶剂条件下考察了聚合物的萃取性能。选取结构类似物苯酚(P)、对羟基联苯(PP)和非结构类似物二聚氰胺(DCD),对MIP和非印迹聚合物(NIP)的选择性吸附性能进行了对比。所建立的SPME方法结合高效液相色谱法(HPLC)成功用于饮料中双酚A的检测。在优化的实验条件下,双酚A的线性范围为10~400 μg/L,检出限(LOD)为0.45 μg/L,在矿泉水中的回收率为88.4%~102.8%。结果表明所建立的方法能够用于检测实际样品中的BPA,具有样品预处理简便、分析快速、检出限低和消耗低的优点。

关键词: 分子印迹聚合物萃取头, 高效液相色谱, 固相微萃取, 双酚A

Abstract:

The rapid preparation of molecularly imprinted polymer (MIP) fibers was reported using bisphenol A (BPA) as the template molecular, acetonitrile (ACN) as the porogenic solvent, α -methacrylic acid (MAA) as the functional monomer, ethylene dimethacrylate (EDMA) as the crosslinker, and azodiisobutyronitrile (AIBN) as the thermal initiator. It was carried out within a capillary of 530 μm inner diameter (I. D.) by microwave irradiation in 7 min. The resulted BPA-MIP fibers were pushed out from the capillary, eluted in a vial and inserted in the capillary again followed by the application of the solid phase microextraction (SPME) procedure. The extraction performance was investigated in detail by varying the molar ratios between the template and the monomer (BPA/MAA), the concentration of NaCl, the extraction and desorption time, the pH value and the desorption solvents. The selectivity of the prepared MIP and non-molecularly imprinted polymer (NIP) fibers was comparatively evaluated by selecting two structurally-related compounds, phenol (P) and 4-phenylphenol (PP), and non-analogue dicyandiamide (DCD). The established method was successfully applied for the pretreatment and determination of BPA from beverage samples coupled to high performance liquid chromatography (HPLC). Under the optimal conditions, the linear range of BPA was 10-400 μg/L; the detection limit (LOD) was 0.45 μg/L and the recoveries spiked in the mineral water were 88.4%-102.8%. The results demonstrated that the developed method can determine BPA in real samples with some advantages of simple pretreatment, rapid analysis, low limit of detection and low consumption of materials.

Key words: bisphenol A (BPA), high performance liquid chromatography (HPLC), molecularly imprinted polymer fiber, solid phase microextraction (SPME)

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