Analysis of Trace Levels of Sulfonamide and Tetracycline Antimicrobials in Groundwater and Surface Water Using Solid-Phase Extraction and Liquid Chromatography/Mass Spectrometry

A method has been developed for the trace analysis of two classes of antimicrobials consisting of six sulfonamides (SAs) and five tetracyclines (TCs), which commonly are used for veterinary purposes and agricultural feed additives and are suspected to leach into ground and surface water. The method...

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Bibliographic Details
Published in:	Analytical chemistry (Washington) 2001-10, Vol.73 (19), p.4640-4646
Main Authors:	Lindsey, Michele E, Meyer, Michael, Thurman, E. M
Format:	Article
Language:	eng
Subjects:	Analysis methods Analytical chemistry antimicrobial agents Applied sciences Chemicals Chemistry Chemistry Techniques, Analytical - methods Chromatographic methods and physical methods associated with chromatography Chromatography Chromatography, Liquid - methods Exact sciences and technology Fresh Water - analysis Groundwater Natural water pollution Other chromatographic methods Pollution Scientific imaging Spectrometry, Mass, Electrospray Ionization - methods Sulfonamides - analysis Tetracycline - analysis Water Pollutants, Chemical - analysis Water treatment and pollution
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Summary:	A method has been developed for the trace analysis of two classes of antimicrobials consisting of six sulfonamides (SAs) and five tetracyclines (TCs), which commonly are used for veterinary purposes and agricultural feed additives and are suspected to leach into ground and surface water. The method used solid-phase extraction and liquid chromatography/mass spectrometry (LC/MS) with positive ion electrospray. The unique combination of a metal chelation agent (Na2EDTA) with a macroporous copolymer resulted in quantitative recoveries by solid-phase extraction (mean recovery, 98 ± 12%) at submicrogram-per-liter concentrations. An ammonium formate/formic acid buffer with a methanol/water gradient was used to separate the antimicrobials and to optimize the signal intensity. Mass spectral fragmentation and ionization characteristics were determined for each class of compounds for unequivocal identification. For all SAs, a characteristic m/z 156 ion representing the sulfanilyl fragment was identified. TCs exhibited neutral losses of 17 amu resulting from the loss of ammonia and 35 amu from the subsequent loss of water. Unusual matrix effects were seen only for TCs in this first survey of groundwater and surface water samples from sites around the United States, requiring that TCs be quantitated using the method of standard additions.
ISSN:	0003-2700 1520-6882