Abstract
An analytical method was developed and tested for four different groups of veterinary antibiotics in both river water and sediment matrices. Solid phase extraction (SPE) was used to enrich and to clean up the aqueous sample. Also, Mcllvaine and ammonium hydroxide buffer solutions were used to extract the compounds from the sediment matrix. High performance liquid chromatography (HPLC) equipped with tandem mass spectrometry (MS/MS) was used to separate and quantify the samples. The range of recoveries (in percent) for tetracyclines (TCs), sulfonamides (SAs), macrolides (MLs), and ionophore polyethers (IPs) in the water matrix were 102.2–124.8, 76.6–124.3, 89.5–114.7, 82.7–117.5 with 1–13 (%) of relative standard deviation respectively with three different concentrations. For sediment, the percent recovery ranges were 32.8–114.8, 62.4–108.9, 53.4–128.4 and 51.3–105.4 for TCs, SAs, MLs and IPs, respectively. The relative standard deviation ranged from 16 – 27 (%) over three different concentrations. The limit of quantification (LOQ) was determined by two different methods and calculated to be in the range of 0.01–0.04 μg/l and 0.3–2.5 μg/kg for TCs, SAs, and MLs in water and sediment, respectively. For IPs, the LOQ was 0.001–0.003 μg/l in river water and 0.4–3.6 μg/kg for sediment. The sediment concentration measured in an agriculture-influenced river was much higher than in the overlying water matrix, indicating a high degree of sediment partitioning for these compounds.
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References
Bruhn ST (2003) J Plant Nutr Soil Sci 166:145–167
Lock CM, Chen L, Volmer DA (1999) Rapid Commun Mass Spectrom 13:1744–1754
Bruno F, Curini R, Corcia AD, Nazzari M, Pallagrosi M (2002) Rapid Commun Mass Spectrom 16:1365–1376
Haller MY, Muller SR, McArdell CS, Alder AC, Suter MJ-F (2002) J Chromatogr A 952:111–120
McArdell CS, Molnar E, Suter MJF, Giger W (2003) Environ Sci Technol 37:5479–5486
Volmer DA, Lock CM (1998) Rapid Commun Mass Spectrom 12:157–164
Animal Health Industry Sales; Animal Health Institute (2002)
Mellon M, Benbrook C, Benbrook KL (2001) Union of Concerned Scientists
Diaz-Cruz MS, Alda MJL, Barcelo D (2003) Trends Anal Chem 22:340–351
Hirsch R, Ternes T, Hanerer K, Kratz KL (1999) Sci Total Environ 225:109–118
Hirsch R, Ternes TA, Haberer K, Mehlich A, Ballwanz F, Kratz KL (1998) J Chromatogr A 815:213–223
Lindsey ME, Meyer M, Thurman EM (2001) Anal Chem 73:4640–4646
Zhu J, Snow DD, Cassada DA, Monson SJ, Spalding RF (2001) J Chromatogr A 928:177–186
Blackwell PA, Lutzhoft HH, Ma HP, Halling-Sorensen B, Boxwell ABA, Kay P (2004) Talanta 64:1058–1064
Jacobsen AM, Halling-Sorensen B, Ingerslev F, Gansen SH (2004) J Chromatogr A 1038:157–170
Jacobsen P, Bergland L (1987) Aquaculture 70:365–370
Bjorklund H, Bondest J, Bylund G (1990) Aquaculture 86:359–367
Cooper AD, Stubbings GWF, Kelly M, Tarbin JA, Farrington WHH, Shcarer G (1998) J Chromatogr A 812:321–326
Hamscher G, Sczesny S, Hoper H, Nau H (2002) Anal Chem 74:1509–1518
Schlusener MP, Bester K, Spiteller M (2003) Anal Bioanal Chem 375:942–947
Wang J (2004) J Agric Food Chem 52:171–181
Loke ML, Jespersen S (2003) J Chromatogr B Analyt Technol Biomed Life Sci 783:11–23
Delepee R, Maume D (2000) J Chromatogr B Analyt Technol Biomed Life Sci 748:369–381
Vinas P, Balsalobre N, Erroz CL, Cordoba MH (2004) J Chromatogr A 1022:125–129
Yang S, Carlson K (2004) J Chromatogr A 1038:141–155
Liang Y, Denton MB, Bates RB (1998) J Chromatogr A 827:45–55
Boxall ABA, Blackwell P, Cavallo R, Kay P, Tolls J (2002) Toxicol Lett 131:19–28
Kim YH, Heinze TM, Kim SJ, Cerniglia CE (2004) J Environ Qual 33:257–264
Thiele-Bruhn S, Seibicke T, Schulten HR, Leinweber P (2004) J Environ Qual 33:1331–1342
Figueroa RA, Leonard A, Mackay AA (2004) Environ Sci Technol 38:476–483
Yang S, Cha J, Carlson KH (2004) Rapid Commun Mass Spectrom 18:2131–2145
Cinquina AL, Longo F, Anastasi G, Giannetti L, Cozzani R (2003) J Chromatogr A 987:227–233
USDA (2003) United States Department of Agriculture Food Safety and Inspection Service
Kolpin DW, Furlong ET, Meyer MT, Thurman EM, Zaugg SD, Barber LB, Buxton HT (2002) Environ Sci Technol 36:1202–1211
Halling-Sorensen B, Jacobsen AM, Jensen J, Sengelov G, Vaclavik E, Ingerslev F (2005) Environ Toxicol Chem 24:802–810
Ferrer I, Furlong ET (2002) Anal Chem 74:1275–1280
Halling-Sorensen B, Sengelov G, Tjornelund J (2002) Arch Environ Contam Toxicol 42:263–271
Acknowledgments
The authors are grateful for the expertise and assistance of Donald Dick in the Department of Chemistry at Colorado State University. This project was funded by the USDA National Integrated Water Quality Program.
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Kim, SC., Carlson, K. Quantification of human and veterinary antibiotics in water and sediment using SPE/LC/MS/MS. Anal Bioanal Chem 387, 1301–1315 (2007). https://doi.org/10.1007/s00216-006-0613-0
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DOI: https://doi.org/10.1007/s00216-006-0613-0