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On-line hyphenation of solid-phase extraction to chromatographic separation of sulfonamides with fused-core columns in sequential injection chromatography.
Batista, Alex D; Chocholous, Petr; Satínský, Dalibor; Solich, Petr; Rocha, Fábio R P.
Afiliação
  • Batista AD; Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, P.O. Box 96, 13400-970 Piracicaba SP, Brazil.
  • Chocholous P; Department of Analytical Chemistry, Faculty of Pharmacy, Charles University in Prague, Heyrovského 1203, Hradec Králové, Czech Republic. Electronic address: petr.chocholous@faf.cuni.cz.
  • Satínský D; Department of Analytical Chemistry, Faculty of Pharmacy, Charles University in Prague, Heyrovského 1203, Hradec Králové, Czech Republic.
  • Solich P; Department of Analytical Chemistry, Faculty of Pharmacy, Charles University in Prague, Heyrovského 1203, Hradec Králové, Czech Republic.
  • Rocha FR; Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, P.O. Box 96, 13400-970 Piracicaba SP, Brazil.
Talanta ; 133: 142-9, 2015 Feb.
Article em En | MEDLINE | ID: mdl-25435240
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(®) Express RP-Amide, Phenyl-Hexyl, and F5) and two monolithic columns (Chromolith(®) 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 µL 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 µg L(-1), linear response ranges from 30.0 to 1000.0 µg L(-1) (r(2)>0.996) and RSDs of peak heights <2.9% (n=6) at a 100 µg L(-1) level and enabled the screening control of freshwater samples contaminated at the 100 µg 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.
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Texto completo: 1 Coleções: 01-internacional Base de dados: MEDLINE Assunto principal: Sulfonamidas / Poluentes Químicos da Água / Extração em Fase Sólida / Antibacterianos Tipo de estudo: Evaluation_studies Idioma: En Revista: Talanta Ano de publicação: 2015 Tipo de documento: Article País de afiliação: Brasil País de publicação: Holanda

Texto completo: 1 Coleções: 01-internacional Base de dados: MEDLINE Assunto principal: Sulfonamidas / Poluentes Químicos da Água / Extração em Fase Sólida / Antibacterianos Tipo de estudo: Evaluation_studies Idioma: En Revista: Talanta Ano de publicação: 2015 Tipo de documento: Article País de afiliação: Brasil País de publicação: Holanda