4.7 Article

Microextraction by packed molecularly imprinted polymer followed by ultra-high performance liquid chromatography for determination of fipronil and fluazuron residues in drinking water and veterinary clinic wastewater

Journal

MICROCHEMICAL JOURNAL
Volume 168, Issue -, Pages -

Publisher

ELSEVIER
DOI: 10.1016/j.microc.2021.106405

Keywords

Molecularly imprinted polymer; Microextraction by packed sorbent; Pesticides; Water samples

Funding

  1. Brazilian agency CNPq (Conselho Nacional de Desenvolvimento Cientifico e Tecnologico)
  2. Brazilian agency FAPEMIG (Fundacao de Amparo `a Pesquisa do Estado de Minas Gerais)
  3. Brazilian agency Coordenacao de Aperfeicoamento de Pessoal de Nivel Superior -Brasil (CAPES) [001]
  4. Rede Mineira de Quimica (RQ-MG) - FAPEMIG [REDE-113/10, CEXRED-0010-14]

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A fast, efficient, and safe method utilizing low-cost lab-microextraction by packed sorbent-device and high ultra-performance liquid chromatography with diode array detection was developed for determining fipronil and fluazuron residues in drinking water and veterinary clinic wastewater. The method demonstrated excellent selectivity, high adsorbent capacity, and high reproducibility with relative recoveries of 98.58 ± 2.64% and 99.92 ± 1.43% for fipronil and fluazuron, respectively, after proper validation.
A fast, efficient and safe method combining a low-cost lab-microextraction by packed sorbent-device and highultra-performance liquid chromatography with diode array detection was developed to determine fipronil and fluazuron residues in drinking water and veterinary clinic wastewater. The prepolymerization complexes of mesoporous molecularly imprinted polymer was studied by density functional theory calculations reaching Delta H = -26.7 kcal mol-1 and Delta G = -8.5 kcal mol-1, in which used fluazuron as template, methacrylic acid as monomer and acetonitrile as porogenic solvent. After, mesoporous molecularly imprinted polymer was properly characterized, demonstrating excellent selectivity to the studied analytes and high adsorbent capacity. After optimization, the better sample preparation conditions were: 75 mu L of ultrapure water as washing solvent, 250 mu L as methanol as eluent, 250 mu L of sample at pH 7, two thaw-eject cycles and two times can be reused. After proper validation, the method was applied in the analysis of fipronil and fluazuron residues in drinking water and veterinary clinic wastewater and showed high reproducibility with relative recoveries of 98.58 +/- 2.64% and 99.92 +/- 1.43% for fipronil and fluazuron, respectively.

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