色谱

色谱 ›› 2013, Vol. 31 ›› Issue (6): 587-595.DOI: 10.3724/SP.J.1123.2012.12014

• 研究论文 • 上一篇    下一篇

橄榄醇分子印迹聚合物的制备及评价(英文)

靳亚峰1, 陈娜1, 刘润强1,2, 陈军1,2, 柏连阳2, 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:2012-12-05 修回日期:2013-01-14 出版日期:2013-06-28 发布日期:2013-06-06
  • 通讯作者: 张裕平
  • 基金资助:

    Scientific Research Foundation for the Returned Overseas Chinese Scholars,State Education Ministry and the National Natural Science Foundation of China (30771436).

Preparation and evaluation of molecularly imprinted polymer of olivetol for solid phase extraction

JIN Yafeng1, CHEN Na1, LIU Runqiang1,2, CHEN Jun1,2, BAI Lianyang2, 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:2012-12-05 Revised:2013-01-14 Online:2013-06-28 Published:2013-06-06
  • Contact: 10.3724/SP.J.1123.2012.12014

PDF

381

被引次数

8

摘要：

以橄榄醇为模板分子,α-甲基丙烯酸(MAA)为功能单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,甲苯和十二醇为溶剂,通过本体聚合法制备了橄榄醇分子印迹聚合物。利用平衡结合实验、扫描电镜(SEM)及红外光谱(FTIR)对分子印迹聚合物(MIP)进行了表征,并用该聚合物进行了加标麦麸中橄榄醇的固相萃取(SPE)研究。平衡结合实验表明MIP对模板分子具有更好的识别性。Scatchard分析表明对橄榄醇分子的吸附存在2类不同结合位点,其中高亲和力结合位点和低亲和力结合位点的解离常数分别为0.021和1.002 mmol/L,相应的最大表观结合量分别为18.74和135.9 μmol/g。在优化的固相萃取条件下,MIP固相萃取柱对加标麦麸中橄榄醇的回收率达到97.8%~98.8%,相对标准偏差为2.8%~4.2%(n=5),线性范围为0.1~100 mg/L,检出限(S/N=3)为0.062 mg/L。与非印迹聚合物(NIP)柱及市售聚苯乙烯/二乙烯基苯(PLS)柱相比,MIP柱的选择性更强,回收率更高,纯化效果更好。

关键词: 本体聚合, 分子印迹聚合物, 橄榄醇, 固相萃取

Abstract:

Molecularly imprinted polymer (MIP) was synthesized by bulk polymerization, using olivetol as template molecule, methyl acrylic acid (MAA) as monomer, ethylene glycol dimethacrylate (EDMA) as crosslinker, toluene and dodecanol as solvents. The resulted MIP was characterized by the equilibrium binding experiments, scanning electron microscope (SEM) and Fourier transform infrared spectrometer (FTIR). The polymer was then applied to solid phase extraction (SPE) of olivetol from spiked wheat bran samples. From the equilibrium binding experiments, it was showed that MIP had a better recognizability for the template molecule. Scatchard analysis showed that MIP had specific adsorption to olivetol with two classes of binding sites. The high and low binding sites dissociation constants were 0.021 and 1.002 mmol/L. The corresponding maximum binding capacities were 18.74 and 135.9 μ mol/g, respectively. Under the optimum condition of SPE, the recoveries of olivetol on MIP cartridge were in the range of 97.8%-98.8%. The relative standard deviations (RSDs) were 2.8%-4.2%. The linearity range was between 0.1 and 100 mg/L. The limit of detection (S/N=3) was 0.062 mg/L. MIP cartridge showed stronger selectivity, higher recovery and purified the sample more drastically compared with non-imprinted polymer (NIP) cartridge and commercial poly(styrene/divinylbenzene) (PLS) cartridge.

Key words: bulk polymerization, molecularly imprinted polymer (MIP), olivetol, solid phase extraction

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