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

Author(s)

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

Affiliation

^[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

• Document type: Journal article
• Source: Journal of Chromatography A; v. 1452, p. 89-97, JUN 24 2016.
• Web of Science Citations: 28

Abstract

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)

• FAPESP's process: 13/07817-2 - Degradation of sulfonamides and tetraciclines by UV/H2O2 and O3: evaluation of antimicrobial activity and toxicity
• Grantee: Milena Guedes Maniero Ferreira
• Support Opportunities: Scholarships in Brazil - Post-Doctoral
• FAPESP's process: 13/09543-7 - Residues of veterinary drugs in the environment
• Grantee: Susanne Rath
• Support Opportunities: Research Projects - Thematic Grants
• FAPESP's process: 14/16622-3 - Identification of intermediates formed during degradation of veterinary drugs by advanced oxidation processes
• Grantee: Caio Alexandre Augusto Rodrigues da Silva
• Support Opportunities: Scholarships in Brazil - Post-Doctoral
• FAPESP's process: 14/06201-0 - Multi-equipment aproved in grant 2013/09543-7: ultra high performance liquid chromatograph coupled to a photodiode array detector and tandem mass spectrometer (UPLC-DAD-MS/MS)
• Grantee: Susanne Rath
• Support Opportunities: Multi-user Equipment Program