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United States Department of Agriculture

Agricultural Research Service

Research Project: METABOLIC VARIABLES AFFECTING THE EFFICACY, SAFETY, AND FATE OF AGRICULTURAL CHEMICALS

Location: Animal Metabolism-Agricultural Chemicals Research

Title: Development of an UPLC-MS/MS Sulfonamide Multi-residue Method and its Application to Water, Manure Slurry, and Soils from Swine Rearing Facilities

Authors
item Shelver, Weilin
item Hakk, Heldur
item Larsen, Gerald
item Desutter, Thomas -
item Casey, Francis -

Submitted to: Society of Environmental Toxicology and Chemistry Abstracts
Publication Type: Abstract Only
Publication Acceptance Date: January 29, 2010
Publication Date: May 23, 2010
Citation: Shelver, W.L., Hakk, H., Larsen, G.L., Desutter, T.M., Casey, F.X. 2010. Development of an UPLC-MS/MS Sulfonamide Multi-residue Method and its Application to Water, Manure Slurry, and Soils from Swine Rearing Facilities. Society of Environmental Toxicology and Chemistry Abstracts, SETAC Europe: 20th Annual Meeting, 23-27 May 2010, Seville, Spain, "Science and Technology for Environmental Protection" Abstract Book. WE118, p. 325.

Technical Abstract: An analytical method was developed using ultra performance liquid chromatography-triple quadrupole-tandem mass spectrometry (UPLC-TQ-MS/MS) to simultaneously analyze 14 sulfonamides (SA) in six minutes. 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 - 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 – 1470000 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 topsoil (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 at soil depths between 46 – 61 cm. Rapid analysis times makes the method practical for medium to high throughput applications. The sensitivity and specificity make the method suitable for problems with demanding requirements for real world applications.

Last Modified: 8/22/2014
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