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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 Title: Development of an UPLC-MS/MS Sulfonamide Multi-residue Method and It's 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: Journal of Chromatography A
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: December 10, 2009
Publication Date: February 12, 2010
Repository URL: http://hdl.handle.net/10113/38966
Citation: Shelver, W.L., Hakk, H., Larsen, G.L., DeSutter, T.M., Casey, F.X.M. 2010. 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. Journal of Chromatography A. 1217:1273-1282. DOI:10.1016/j.chroma.2009.12.034.

Interpretive Summary: This article describes the development of a new, very sensitive and specific analysis of sulfonamides, common veterinary and human antibacterials. It is capable of simultaneously determining 14 different sulfonamides with positive identification of the particular sulfonamide as well as a quantitative measure of how much is present in the sample. This method can be applied to water, soil, and manure slurry. In this study, farm samples were analyzed demonstrating some of the drugs were present in the manure slurry and when the manure slurry were used as liquid fertilizer for soil, the drugs were present in the soil.

Technical Abstract: An analytical method was developed using ultra performance liquid chromatography-triple quadrupole-tandem mass spectrophotometry (UPLC-TQ-MS/MS) to simultaneously analyze 14 sulfonamides (SA) in six minutes. 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, 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 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 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 ' 106 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 (0-15.2 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 45.7 – 61.0 cm.

Last Modified: 12/20/2014
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