Analytical and Bioanalytical Chemistry

, Volume 410, Issue 14, pp 3361–3374 | Cite as

Pipette-tip solid-phase extraction using polypyrrole as efficient adsorbent for extraction of avermectins and milbemycins in milk

  • Diego Hernando Ângulo Florez
  • Roseane Andrade Teixeira
  • Ricky Cássio Santos da Silva
  • Bruna Carneiro Pires
  • Flávia Viana Avelar Dutra
  • Keyller Bastos Borges
Research Paper


In this work, we developed a HPLC method for the multidetermination of avermectins (AVM) (abamectin—ABA 1b and ABA 1a, eprinomectin—EPR, and ivermectin—IVM) and milbemycins (moxidectin—MOX) in milk samples using polypyrrole (PPy) as adsorbent material in pipette-tip solid-phase extraction (PT–PPy–SPE). PPy was characterized by scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, and X-ray diffraction and the data agreed with the literature. The sample preparation included the clean-up of the milk by protein precipitation (PP) with acetonitrile and extraction of the analytes by PT–PPy–SPE. The chromatographic method was developed in reverse phase and isocratic mode with flow rate at 1.2 mL min−1 and ultraviolet detection at 250 nm. The mobile phase composition was acetonitrile:methanol:water (55:25:20, v/v/v). The studied parameters and the optimized conditions for the sample preparation were washing solvent (300 μL water), volume and type of eluent (500 μL methanol), volume and pH of sample (1 mL and pH 10), amount of adsorbent material (50 mg PPy), and without addition of salt (NaCl). The method was linear over the concentration range from 20 to 3000 ng mL−1 with coefficients of correlation (r) ≥ 0.99 for all analytes and recoveries around 100%. The method developed and validated was used for the analyses of real milk samples from cow treated with Ivomec® (IVM 3.5%), in which were found 21.51 ± 2.94 ng mL−1 of IVM. Finally, the results proved that PT–PPy–SPE coupled to HPLC–UV was economical, simple, and easy-to-perform technique.

Graphical abstract

Pipette-tip solid phase extraction using polypirrole as adsorbent material for determination of avermectins and milbemycins in milk


Avermectins Milbemycyns Polypyrrole Pipette-tip solid-phase extraction Milk 



The authors would like to thank the Brazilian agencies CNPq (Conselho Nacional de Desenvolvimento Científico e Tecnológico), CAPES (Coordenação de Aperfeiçoamento de Pessoal de Nível Superior), FAPES (Fundação de Amparo à Pesquisa e Inovação do Espírito Santo), and FAPEMIG (Fundação de Amparo à Pesquisa do Estado de Minas Gerais) for financial support. This study is also part of the project involving the Rede Mineira de Química (RQ-MG) supported by FAPEMIG (Project: REDE-113/10; Project: CEX-RED-0010-14).

Compliance with ethical standards

All studies involving animals are reported in accordance with the ARRIVE guidelines and approved by the institutional ethics board committee.

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

216_2018_1031_MOESM1_ESM.pdf (297 kb)
ESM 1 (PDF 296 kb)


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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Diego Hernando Ângulo Florez
    • 1
  • Roseane Andrade Teixeira
    • 1
  • Ricky Cássio Santos da Silva
    • 1
  • Bruna Carneiro Pires
    • 1
  • Flávia Viana Avelar Dutra
    • 1
  • Keyller Bastos Borges
    • 1
  1. 1.Departamento de Ciências NaturaisUniversidade Federal de São João del-ReiSão João del-ReiBrazil

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