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http://dx.doi.org/10.5338/KJEA.2017.36.3.22

Development of Simultaneous Analytical Method of Veterinary Antibiotics in Manure using Liquid Chromatography Coupled with Tandem Mass Spectrometry  

Chung, Hyung Suk (Division of Applied Bioscience and Biotechnology, College of Agriculture and Life Sciences, Chonnam National University)
Lee, Young Jun (Kyung Nong Co., Ltd., Central Research Institute)
Lee, Han Sol (Division of Applied Bioscience and Biotechnology, College of Agriculture and Life Sciences, Chonnam National University)
Rahman, Md. Musfiqur (Division of Applied Bioscience and Biotechnology, College of Agriculture and Life Sciences, Chonnam National University)
Kabir, Md. Humayun (Division of Applied Bioscience and Biotechnology, College of Agriculture and Life Sciences, Chonnam National University)
Park, Byung-Jun (Chemical Safety Division, Department of Agro-Food Safety and Crop Protection, National Institute of Agricultural Science)
Kim, Jang-Eok (School of Applied Biosciences, College of Agriculture and Life Sciences, Kyungpook National University)
Shim, Jae-Han (Division of Applied Bioscience and Biotechnology, College of Agriculture and Life Sciences, Chonnam National University)
Publication Information
Korean Journal of Environmental Agriculture / v.36, no.3, 2017 , pp. 201-210 More about this Journal
Abstract
BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.
Keywords
LC-MS/MS; Liquid; Monitoring; Solid manure; Veterinary antibiotics;
Citations & Related Records
Times Cited By KSCI : 4  (Citation Analysis)
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