title: 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.
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°C. Samples were prepared by extracting sulfonamides from soil using a solid-liquid extraction method with water:acetonitrile, 1:1v/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 (100-400μL), loading solvent (water and different proportions of water:methanol) and washing volume (0.19-0.66mL). The method produced linear results for all sulfonamides from 0.5 to 12.5ngg(-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 0.5ngg(-1). The SPE column allowed for the analysis of many (more than 2000) samples without decreasing the efficiency.
authors.affiliation: Institute of Chemistry, Department of Analytical Chemistry, University of Campinas, P.O. Box 6154, 13083-970 Campinas, SP, Brazil.
authors.forename: Natália Fernanda
authors.initials: NF
authors.lastname: Tetzner
authors.affiliation: School of Civil Engineering, Architecture and Urban Design, University of Campinas, P.O. Box 6143, 13083-889 Campinas, SP, Brazil.
authors.forename: Milena Guedes
authors.initials: MG
authors.lastname: Maniero
authors.affiliation: Institute of Chemistry, Department of Analytical Chemistry, University of Campinas, P.O. Box 6154, 13083-970 Campinas, SP, Brazil.
authors.forename: Caio
authors.initials: C
authors.lastname: Rodrigues-Silva
authors.affiliation: Institute of Chemistry, Department of Analytical Chemistry, University of Campinas, P.O. Box 6154, 13083-970 Campinas, SP, Brazil. Electronic address: Susanne.rath@gmail.com.
authors.forename: Susanne
authors.initials: S
authors.lastname: Rath
mesh_terms: D000097:Acetonitriles; D002851:Chromatography, High Pressure Liquid; D004350:Drug Residues / Q000032:analysis*; D012987:Soil / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D013449:Sulfonamides / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D019155:Veterinary Drugs / Q000737:chemistry; D014867:Water
chemical_list: D000097:Acetonitriles; D012987:Soil; D013449:Sulfonamides; D019155:Veterinary Drugs; D014867:Water; C032159:acetonitrile
keywords: Antimicrobials in soil; Environmental matrices; On-line SPE-UHPLC–MS/MS; Sulfonamide residues; Veterinary drugs