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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

Permanent URL:
http://handle.nal.usda.gov/10113/38966
Abstract:
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 6min. 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 1pg/μL (5pg 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 2.0ng/L for water, 30ng/L for slurry manure, and 45ng/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 2250-5060ng/L, sulfamethoxazole concentrations of 108-1.47×10⁶ ng/L, and sulfathiazole concentrations of 785-1700ng/L were found in the slurry manure. Sulfadimethoxine (2.0-32ng/L), sulfamethazine (2.0-5.1ng/L), and sulfamethoxazole (20.5-43.0ng/L) were found in surface water and ground water. In top soil (0-15cm), sulfamethazine ranged 34.5-663ng/kg dry weight in those locations that received slurry manure as a nutrient; no SAs were found in the soil depths between 46 and 61cm. 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.
Author(s):
Shelver, Weilin L. , Hakk, Heldur , Larsen, Gerald L. , DeSutter, Thomas M. , Casey, Francis X.M.
Subject(s):
pig manure , slurries , drug residues , sulfonamides , multiresidue analysis , high performance liquid chromatography , mass spectrometry , water pollution , surface water , groundwater contamination , agricultural soils , polluted soils , soil pollution
Format:
p. 1273-1282.
Note:
Includes references
Source:
Journal of chromatography. A 2010 Feb. 19, v. 1217, no. 8
Language:
English
Publisher:
Amsterdam; New York: Elsevier
Year:
2010
Collection:
Journal Articles, USDA Authors, Peer-Reviewed
File:
Download [PDF File]
Rights:
Works produced by employees of the U.S. Government as part of their official duties are not copyrighted within the U.S. The content of this document is not copyrighted.