Chinese Journal of Applied Chemistry ›› 2016, Vol. 33 ›› Issue (2): 229-237.DOI: 10.11944/j.issn.1000-0518.2016.02.150184

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Preparation of p-Hydroxybenzoic Acid-Imprinted Polymer Particulates and Application to Solid Phase Extraction

ZHANG Tielia*(),CHAI Guopinga,HE Caixiaab,WANG Leia   

  1. aDepartment of Chemistry,Tangshan Nomoral College,Tangshan,Hebei 063000,China
    bCollege of Biological Science and Engineering,Hebei University of Science and Technology,Shijiazhuang 050018,China
  • Received:2015-06-02 Accepted:2015-10-29 Published:2016-02-01 Online:2016-02-01
  • Contact: ZHANG Tieli
  • Supported by:
    Supported by the Key Team Project Foundation of Tangshan Normal College(No.2014D07)

Abstract:

p-Hydroxybenzoic acid(p-HBA)-imprinted polymer particulates were prepared using p-HBA as the template, acrylamide(AM) as the functional monomer and ethylene glycol dimethacrylate as the crosslinker in three different amounts of p-HBA and under two different concentrations of pre-polymerization mixtures via precipitation polymerization. Their rebinding performances for p-HBA were characterized by high-performance liquid chromatography. The results reveal that both the amounts of p-HBA and the concentrations of pre-polymerization mixtures exhibit notable influence on the binding performances of p-HBA-imprinted polymers. The p-HBA-imprinted polymer(P2) with high affinity(k'=4.01) and selectivity for p-HBA is obtained when the amount of p-HBA is 1.0 mmol, which is corresponding to the molar ratio of 1:2(p-HBA/AM), in 37.5 mL of acetonitrile solvent. In addition, the imprinted polymer P2 was chosen as the adsorbent to make the molecularly imprinted solid phase extraction(MISPE) column and the MISPE method for the extraction of p-HBA was developed. The MISPE column capacities for p-HBA are 6.91 μg/100 mg and 1.93 μg/100 mg, respectively, which are determined under two different modes of loading samples. The rhizoma gastrodiae samples spiked with three different amounts of p-HBA are extracted and the recoveries of p-HBA range from 76.8% to 86.6%, with the RSD of 3.4%~6.2%(n=3). The results demonstrate that the p-HBA-imprinted polymer particulates prepared using AM as the functional monomer by precipitation polymerization are suitable as the adsorbent of solid phase extraction column for the selective separation and purification of p-HBA in the real sample of rhizoma gastrodiae.

Key words: p-hydroxybenzoic acid, precipitation polymerization, molecular recognition, molecularly imprinted solid phase extraction