1. Academic Validation
  2. Analysis of pesticide residues in açaí-based food products: an approach using polymeric ionic liquid-based solid-phase microextraction coupled to gas chromatography-mass spectrometry

Analysis of pesticide residues in açaí-based food products: an approach using polymeric ionic liquid-based solid-phase microextraction coupled to gas chromatography-mass spectrometry

  • Food Res Int. 2025 Dec;222(Pt 2):117720. doi: 10.1016/j.foodres.2025.117720.
Luis Eduardo Silva Nascimento 1 Bhawana Thapa 2 Shu-An Hsieh 2 Plínio Ribeiro Rodrigues 3 Marcella Vitória Galindo 4 Wellington da Silva Oliveira 5 Helena Teixeira Godoy 4 Jared L Anderson 6
Affiliations

Affiliations

  • 1 Department of Food Science and Nutrition, School of Food Engineering, University of Campinas (UNICAMP), Rua Monteiro Lobato 80, 13083-862 Campinas, SP, Brazil; Department of Chemistry, Iowa State University, Ames, IA 50011, USA.
  • 2 Department of Chemistry, Iowa State University, Ames, IA 50011, USA.
  • 3 Department of Fundamental Chemistry, Institute of Chemistry, University of São Paulo (USP), Avenida Lineu Prestes 748, 05508-000, Cidade Universitária, Sao Paulo, SP, Brazil; Department of Chemical Engineering, State University of Maringá (UEM), Avenida Colombo, 5790, 87020-900, Jardim Universitário, Maringá, PR, Brazil.
  • 4 Department of Food Science and Nutrition, School of Food Engineering, University of Campinas (UNICAMP), Rua Monteiro Lobato 80, 13083-862 Campinas, SP, Brazil.
  • 5 Reference Laboratory for Physical, Sensory and Statistics Analysis, Science and Food Quality Center, Institute of Food Technology (ITAL), Avenida Brasil 2880, 13070-178 Campinas, SP, Brazil.
  • 6 Department of Chemistry, Iowa State University, Ames, IA 50011, USA. Electronic address: [email protected].
Abstract

The market for açaí-based food products (AFPs) has been growing steadily, particularly within the international sector. The Brazilian Health Regulatory Agency (ANVISA) authorizes the use of certain pesticides in açaí cultivation, which may result in residues in derived products. A solid-phase microextraction (SPME) method based on polymeric ionic liquid (PIL) sorbent coatings coupled with gas chromatography-mass spectrometry (GC-MS) was developed and validated for the determination of pesticide residues in AFPs. A multivariate optimization was performed that focused on the following three variables: extraction temperature, extraction time, and sodium chloride concentration within the extraction solution. The optimized and validated method yielded satisfactory results, with limits of quantification ranging from 1 to 9 μg kg-1, linearity with R2 ≥ 0.987, recoveries between 70 % and 88 %, and precision ranging from 2 % to 12 %. The matrix effect exhibited suppression up to 87 % and enhancement up to 22 %. Furthermore, the method's greenness and practicality were assessed using established metrics. The results demonstrated that the method can be classified as both practical and environmentally-friendly. In the occurrence analysis, S-metolachlor was quantified in four samples at concentrations ranging from 1.1 to 1.3 μg kg-1. Thiabendazole and fluxapyroxad were detected in concentrations below the limit of quantification. In addition, all detected pesticide levels were below their respective acceptable daily intake values. This method demonstrated robust performance for the quantification of pesticides in AFPs and provides important data for regulatory agencies regarding pesticide residues in açaí-derived products.

Keywords

Analytical method; Food analysis; Food contaminant; Gas chromatography–mass spectrometry; Sample preparation.

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