On-line hyphenation of solid-phase extraction to chromatographic separation of sulfonamides with fused-core columns in sequential injection chromatography

Autor(es)

Batista, Alex D. ; Chocholous, Petr ; Satinsky, Dalibor ; Solich, Petr ; Rocha, Fabio R. P.

• Tipo de documento: Artigo Científico
• Fonte: Talanta; v. 133, p. 8-pg., 2015-02-01.

Resumo

On-line sample pretreatment (clean-up and analyte preconcentration) is for the first time coupled to sequential injection chromatography. The approach combines anion-exchange solid-phase extraction and the highly effective pentafluorophenylpropyl (F5) fused-core particle column for separation of eight sulfonamide antibiotics with similar structures (sulfathiazole, sulfanilamide, sulfacetamide, sulfadiazine, sulfamerazine, sulfadimidine, sulfamethoxazole and sulfadimethoxine). The stationary phase was selected after a critical comparison of the performance achieved by three fused-core reversed phase columns (Ascentis (R) Express RP-Amide, Phenyl-Hexyl, and F5) and two monolithic columns (Chromolith (R) High Resolution RP-18 and CN). Acetonitrile and acetate buffer pH 5.0 at 0.60 mL min(-1) were used as mobile phase to perform the separations before spectrophotometric detection. The first mobile phase was successfully used as eluent from SPE column ensuring transfer of a narrow zone to the chromatographic column. Enrichment factors up to 39.2 were achieved with a 500 mu L sample volume. The developed procedure showed analysis time < 10.5 min, resolutions > 1.83 with peak symmetry <= 1.52, LODs between 4.9 and 27 mu g L-1, linear response ranges from 30.0 to 1000.0 mu g L-1 (r(2) > 0.996) and RSDs of peak heights <2.9% (n=6) at a 100 mu g L-1 level and enabled the screening control of freshwater samples contaminated at the 100 mu g L-1 level. The proposed approach expanded the analytical potentiality of SIC and avoided the time-consuming batch sample pretreatment step, thus minimizing risks of sample contamination and analyte losses. (C) 2014 Elsevier B.V. All rights reserved. (AU)

• Processo FAPESP: 11/06437-6 - Sistemas de análises em fluxo aplicados à determinação de poluentes emergentes
• Beneficiário: Alex Domingues Batista
• Modalidade de apoio: Bolsas no Brasil - Doutorado
• Processo FAPESP: 12/14950-8 - Desenvolvimento de procedimento analítico para a determinação de antibióticos em águas utilizando técnicas de microextração e cromatografia por injeção sequencial
• Beneficiário: Alex Domingues Batista
• Modalidade de apoio: Bolsas no Exterior - Estágio de Pesquisa - Doutorado