4.6 Article

Polypyrrole monolithic extraction phase: From conventional to miniaturized sample preparation techniques

Journal

JOURNAL OF CHROMATOGRAPHY A
Volume 1651, Issue -, Pages -

Publisher

ELSEVIER
DOI: 10.1016/j.chroma.2021.462260

Keywords

Monolithic polymer; Polypyrrole; Sample preparation techniques; Liquid chromatography; Agrochemicals; Dexamethasone

Funding

  1. Conselho Nacional de Desenvolvimento Cientifico e Tecnologico (CNPq) [447927/2014-0]
  2. CoordenacAo de Aperfeicoamento de Pessoal de Nivel Superior (CAPES)
  3. FundacAo de Apoio a Pesquisa do Estado de Goias (FAPEG)

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Monolithic polymers modified with polypyrrole are shown to be a feasible alternative extraction phase for miniaturized sample preparation techniques, with high efficiency and absolute recovery values.
Monolithic polymers are described as continuous and highly porous materials. They have been gaining popularity as an effective extracting phase for some sample preparation methods, due to their variety of functionalities, such as wide pH range tolerance, good permeability, and its ability to allow changes into their surface. Polypyrrole represents an interesting alternative for the modification in extraction phases due to its well related ability to perform multiple interactions, such as acid-base, pi -pi, ion exchange, interactions with hydrophobic affinities or polar functional groups. Among the different sample prepara-tion techniques, solid-phase extraction (SPE) is one of the most popular and used; a miniaturized version of SPE is the disposable pipette extraction (DPX). DPX is a recent miniaturized extraction technique that usually employing silica-based sorbents inside a pipette tip (5 or 1 mL). The present study proposes the development of a monolithic extraction phase composed by styrene divinylbenzene (1:1) modified with polypyrrole for SPE and DPX techniques. The efficiency of the material was evaluated in face of the ex-traction of different samples and analytes, triazine herbicides in water and dexamethasone in synthetic synovial liquid by conventional and miniaturized solid-phase extraction techniques. The extractions per -formed by SPE and DPX presented absolute recovery values ranging from 74.8 to 105.0%, inter-day pre-cision ranging from 0.6 to 14.0%, and limit of quantification of 0.5 and 5.0 ng.mL & minus;1, respectively. The DPX miniaturized method exhibited results equivalent to the methods reported in the literature for ex-traction of dexamethasone in synovial fluid samples. Moreover, this technique proved to be quicker and cheaper than SPE, and produced fewer residual volumes, supporting the preference for green chemistry. Monolithic polymers modified with polypyrrole presented to be a feasible alternative extraction phase for miniaturized sample preparation techniques. (C) 2021 Elsevier B.V. All rights reserved.

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