Development of an ultra-high-pressure liquid chromatography–tandem mass spectrometry multi-residue sulfonamide method and its application to water, manure slurry, and soils from swine rearing facilities

• Published in: Journal of Chromatography A Vol. 1217; no. 8; pp. 1273 - 1282
• Main Authors: Shelver, Weilin L., Hakk, Heldur, Larsen, Gerald L., DeSutter, Thomas M., Casey, Francis X.M.
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 19.02.2010; Amsterdam; New York: Elsevier; Elsevier
• Subjects: agricultural soils; Agriculture, rearing and food industries wastes; Analysis; Analysis methods; Analytical chemistry; Animals; Applied sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid - methods; drug residues; Exact sciences and technology; groundwater contamination; high performance liquid chromatography; LC-MS/MS; Limit of Detection; Manure - analysis; Manure slurry; mass spectrometry; multiresidue analysis; Natural water pollution; Other chromatographic methods; pig manure; polluted soils; Pollution; slurries; Soil; Soil - analysis; soil pollution; Sulfonamides; Sulfonamides - analysis; surface water; Swine; Tandem Mass Spectrometry - methods; Wastes; Water; Water - analysis; water pollution; Water treatment and pollution; Water; Soil; LC-MS/MS; Manure slurry; Sulfonamides; Analysis; Ultra performance liquid chromatography; Solid phase extraction; Tandem mass spectrometry; Chemical analysis; HPLC chromatography; Soil pollution; Chemical enrichment; Sample preparation; Water well; Antiinfectious; Agricultural waste; Ungulata; Ground water; Sulfonamide; Coupled method; Farmyard manure; Pig; Soils; Vertebrata; Mammalia; Multicomponent analysis; Residue; Animal; Surface water; Water pollution; Artiodactyla
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2009.12.034

An analytical method was developed using ultra-high-pressure liquid chromatography–triple quadrupole-tandem mass spectrometry (UHPLC–TQ-MS/MS) to simultaneously analyze 14 sulfonamides (SA) in 6 min. Despite the rapidity of the assay the system was properly re-equilibrated in this time. No carryover was observed even after high analyte concentrations. The instrumental detection limit based on signal-to-noise ratio (S/N) > 3, was below 1 pg/μL (5 pg on column) for all SAs except sulfachloropyridazine. Surface water, ground water, soil, and slurry manure contained in storage ponds in and around swine [ Sus scrofa domesticus] rearing facilities were analyzed. Sample cleanup for ground water and surface water included using solid phase extraction (SPE) using Oasis ® hydrophilic–lipophilic balance (HLB) cartridges. The soil and slurry manure required tandem strong anion exchange (SAX) and HLB solid phase extraction cartridges for sample cleanup. With few exceptions, the recoveries ranged from 60 to 100% for all matrices. The minimum detectable levels were below 2.0 ng/L for water, 30 ng/L for slurry manure, and 45 ng/kg for soil except for sulfachloropyridazine. The coefficient of variation (CV) was within 20% for most of the compounds analyzed. Using this method, sulfamethazine concentrations of 2250–5060 ng/L, sulfamethoxazole concentrations of 108–1.47 × 10 6 ng/L, and sulfathiazole concentrations of 785–1700 ng/L were found in the slurry manure. Sulfadimethoxine (2.0–32 ng/L), sulfamethazine (2.0–5.1 ng/L), and sulfamethoxazole (20.5–43.0 ng/L) were found in surface water and ground water. In top soil (0–15 cm), sulfamethazine ranged 34.5–663 ng/kg dry weight in those locations that received slurry manure as a nutrient; no SAs were found in the soil depths between 46 and 61 cm. The speed makes the method practical for medium to high throughput applications. The sensitivity and positive analyte identification make the method suitable for the demanding requirements for real world applications.