On-line solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry as a powerful technique for the determination of sulfonamide residues in soils

Autor(es)

Tetzner, Natalia Fernanda ^[1] ; Maniero, Milena Guedes ^[2] ; Rodrigues-Silva, Caio ^[1] ; Rath, Susanne ^[1]

Afiliação do(s) autor(es)

^[1] Univ Estadual Campinas, Inst Chem, Dept Analyt Chem, POB 6154, BR-13083970 Campinas, SP - Brazil

^[2] Univ Estadual Campinas, Sch Civil Engn Architecture & Urban Design, POB 6143, BR-13083889 Campinas, SP - Brazil

• Tipo de documento: Artigo Científico
• Fonte: Journal of Chromatography A; v. 1452, p. 89-97, JUN 24 2016.
• Citações Web of Science: 28

Resumo

Sulfonamides are antimicrobials used widely as veterinary-drugs, and their residues have been detected in environmental matrices. An analytical method for determining sulfadiazine, sulfathiazole, sulfamethazine, sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline residues in soils employing a solid phase extraction on-line technique coupled with ultra-high performance liquid chromatography and tandem mass spectrometry (SPE-UHPLC-MS/MS) was developed and validated in this study. SPE and chromatographic separation were performed using an Oasis HLB column and an Acquity UPLC BEH C18 analytical column, respectively, at 40 degrees C. Samples were prepared by extracting sulfonamides from soil using a solid-liquid extraction method with water:acetonitrile, 1:1 v/v (recovery of 70.2-99.9%). The following parameters were evaluated to optimize the on-line SPE process: sorbent type (Oasis and C8), sample volume (100-400 mu l), loading solvent (water and different proportions of water:methanol) and washing volume (0.19-0.66 mL). The method produced linear results for all sulfonamides from 0.5 to 12.5 ngg(-1) with a linearity greater than 0.99. The precision of the method was less than 15%, and the matrix effect was -27% to -87%. The accuracy was in the range of 77-112% for all sulfonamides. The limit of quantitation in the two soils (clay and sand) was 0.5 ngg(-1). The SPE column allowed for the analysis of many (more than 2000) samples without decreasing the efficiency. (C) 2016 Elsevier B.V. All rights reserved. (AU)

• Processo FAPESP: 13/07817-2 - Degradação de sulfonamidas e tetraciclinas por UV/H2O2 e O3: avaliação da atividade antimicrobiana e da toxicidade
• Beneficiário: Milena Guedes Maniero Ferreira
• Modalidade de apoio: Bolsas no Brasil - Pós-Doutorado
• Processo FAPESP: 13/09543-7 - Resíduos de medicamentos veterinários no ambiente
• Beneficiário: Susanne Rath
• Modalidade de apoio: Auxílio à Pesquisa - Temático
• Processo FAPESP: 14/16622-3 - Identificação dos intermediários formados durante a degradação de fármacos veterinários por processos oxidativos avançados
• Beneficiário: Caio Alexandre Augusto Rodrigues da Silva
• Modalidade de apoio: Bolsas no Brasil - Pós-Doutorado
• Processo FAPESP: 14/06201-0 - EMU concedido no processo 2013/09543-7- cromatógrafo líquido de ultraeficiência acoplado a detetores de arranjo de fotodiodos e espectrômetro de massas sequencial (UPLC-DAD-MS/MS)
• Beneficiário: Susanne Rath
• Modalidade de apoio: Auxílio à Pesquisa - Programa Equipamentos Multiusuários