4.5 Article

Development of a selective sorbent for the solid-phase extraction of terbuthylazine in olive oil samples: A molecular imprinting strategy

Journal

JOURNAL OF SEPARATION SCIENCE
Volume 38, Issue 7, Pages 1204-1212

Publisher

WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201401263

Keywords

Molecularly imprinted polymers; Olive oil; Solid-phase extraction; Terbuthylazine

Funding

  1. FEDER
  2. National founds, through the Programa Operacional Regional do Alentejo (InAlentejo) Operation [ALENT-07-0262-FEDER-001871]
  3. FEDER Funds through the Operational Programme for Competitiveness Factors - COMPETE and National Funds through FCT - Foundation for Science and Technology under the Strategic Projects [PEst-C/AGR/UI0115/2011, PEst-OE/QUI/UI0619/2014, PTDC/AGR-ALI/117544/2010]
  4. Fundacao para a Ciencia e a Tecnologia (FCT) [SFRH/BPD/72182/2010]
  5. Fundação para a Ciência e a Tecnologia [PTDC/AGR-ALI/117544/2010] Funding Source: FCT

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Aiming to implement an analytical methodology that is highly selective for the extraction and quantification of terbuthylazine from olive oil, we successfully achieved: (i) the development of a molecularly imprinted polymer by bulk polymerization using terbuthylazine as template molecule, methacrylic acid as functional monomer, ethylene glycol dimethacrylate as cross-linker, and dichloromethane as porogen; (ii) characterization of the imprinting material using Fourier transform infrared spectroscopy, thermogravimetric analysis, nitrogen adsorption at 77 K, and scanning electron microscopy; (iii) their molecular recognition for the template molecule using high-performance liquid chromatography, and (iv) optimization of a solid-phase extraction procedure using as sorbent the synthesized molecularly imprinted polymer for the selective extraction and clean-up of terbuthylazine from spiked organic olive oil and further quantification of the pesticide levels by high-performance liquid chromatography. The suitability of the implemented analytical methodology was demonstrated, as concentrations of terbuthylazine below the tolerated maximum residue limits in the spiked organic olive oil samples could be satisfactorily analyzed with good precision/accuracy with high recovery rates (96%). Overall, the implemented methodology has proven to be reliable and robust and is highly promising in the field of sample preparation, particularly for the isolation/preconcentration of terbuthylazine in complex food samples.

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