色谱

色谱 ›› 2015, Vol. 33 ›› Issue (5): 468-474.DOI: 10.3724/SP.J.1123.2015.02065

• 特别策划：新型分离材料专栏 • 上一篇    下一篇

替代模板分子印迹聚合物的制备及其用于人尿、牛血清和啤酒中7种双酚类物质的选择性固相萃取

杨甲甲1,2, 李云1, 王金成1, 孙晓丽1,2, 陈吉平1   

  1. 1. 中国科学院大连化学物理研究所, 中国科学院分离分析化学重点实验室, 辽宁 大连 116023;
    2. 中国科学院大学, 北京 100049
  • 收稿日期:2015-02-10 发布日期:2015-04-23
  • 通讯作者: 陈吉平
  • 基金资助:

    国家自然科学基金项目(21475130).

Preparation of molecularly imprinted polymers using dummy template and the applications in selective solid-phase extraction of seven bisphenols from human urine, bovine serum and beer samples

YANG Jiajia1,2, LI Yun1, WANG Jincheng1, SUN Xiaoli1,2, CHEN Jiping1   

  1. 1. Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;
    2. University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2015-02-10 Published:2015-04-23

PDF

222

被引次数

2

摘要：

以酚酞(PP)为替代模板,采用本体聚合法制备了选择性识别7种双酚类物质(BPs)的分子印迹聚合物(MIP)。将制备的PP-MIP用作固相萃取(SPE)填料,成功应用于人尿、牛血清和啤酒样品中7种BPs的分离净化。建立了同时测定人尿、牛血清和啤酒样品中的7种BPs的MIP-SPE-HPLC分析方法。3种样品中7种BPs的方法检出限范围均为1.2~2.0 μg/L。结果表明,7种BPs在0.02~2 mg/L范围内线性关系良好,相关系数(r)大于0.9998;空白样品中加标水平为100和500 μg/L的回收率范围为90.1%~107.1%,相对标准偏差(RSD)不高于8.1%。该方法简便、准确、灵敏、可靠,可用于人尿、牛血清和啤酒中7种BPs的快速检测。

关键词: 分子印迹聚合物, 高效液相色谱, 固相萃取, 牛血清, 啤酒, 人尿, 双酚类物质, 替代模板

Abstract:

A molecularly imprinted polymer (MIP) for selective recognition of seven bisphenols (BPs) was prepared using dummy template phenolphthalein (PP) by bulk polymerization. The characterization results of scanning electron microscopy and nitrogen adsorption-desorption measurements showed that the prepared PP-MIP possessed narrow particle diameter distribution (40-60 μm), a specific surface area (SBET) of 359.77 m2/g and a total pore volume (Vt) of 0.730 cm3/g. The adsorption capacity for bisphenol A (BPA) of PP-MIP was evaluated by static adsorption experiment. And the Scatchard analysis revealed that the maximum specific adsorption capacity of PP-MIP was 4.661 μmol/g. Good class selectivity for BPA and its six structural analogues of bisphenol B (BPB), bisphenol E (BPE), bisphenol AF (BPAF), bisphenol S (BPS), bisphenol AP (BPAP) and bisphenol Z (BPZ) was demonstrated by the chromatographic evaluation experiment. The prepared PP-MIP was successfully used as solid-phase extraction (SPE) sorbent for the separation and purification of the seven BPs in human urine, bovine serum and beer samples. Meanwhile, an accurate and sensitive MIP-SPE-HPLC method was established for the determination of the seven BPs in human urine, bovine serum and beer samples. The limits of detection (LODs) for the three samples were in the range of 1.2-2.0 μg/L. The results showed that good linearities were obtained in the range of 0.02-2 mg/L for the seven BPs and the correlation coefficients (r) were higher than 0.9998. The recoveries of the BPs spiked in blank samples at two spiked levels (100 and 500 μg/L for each BP) were in the range of 90.1%-107.1% with the RSDs≤8.1%. The proposed method is simple and reliable for the rapid detection of the seven BPs in human urine, bovine serum and beer samples.

Key words: beer, bisphenols (BPs), bovine serum, dummy template, high performance liquid chromatography (HPLC), human urine, molecularly imprinted polymers (MIP), solid-phase extraction (SPE)

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