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Determination of 38 antibiotics in raw and treated wastewater from swine farms using liquid chromatography-mass spectrometry
Authors:Suli Zhi  Jing Zhou  Zulin Zhang  Keqiang Zhang
Institution:1. Innovation Team for Pollution Prevention and Control of Livestock and Poultry Industry, Agro-Environmental Protection Institute, Ministry of Agriculture, Tianjin, P. R. China;2. Technical Development Department, Guangdong VTR Bio-Tech Co., Ltd., Zhuhai, Guangdong, P. R. China;3. Department of Environment and Biochemistry, The James Hutton Institute, Aberdeen, UK
Abstract:The present study firstly aimed at developing a multi-residue method to identify and quantify 38 veterinary antibiotics (belonging to five different classes) not only for raw swine wastewater but also for wastewater differently treated by different units. The proposed method is based on a solid-phase extraction procedure and ultra high performance liquid chromatography with mass spectrometry. For sample preparation, the optimal loading sample volume was selected as 50 mL, the pH of which was adjusted to approximately 3.0 using formic acid. Then 0.1 g/L ethylenediaminetetraacetic acid disodium salt was added. The recovery rates for different types of wastewaters were in the range of 35.94–124.51% and the relative standard deviations were in the range of 0.36–14.62%. All the matrix standard curves exhibited high linearity (0.9956–0.9999). The matrix effects for the target antibiotics ranged from –61.73 to +148.75%. To ensure the practicality of the method, we performed the detection of the actually added concentration to determine method detection limits and quantitation limits. The quantitation limits of most of the target antibiotics were 0.04 μg/L, except for spiramycin (0.1 μg/L) and roxithromycin (0.2 μg/L). This optimized and validated method was applied to analyze antibiotic residues in swine water samples from four swine farms.
Keywords:solid-phase extraction  swine wastewater  veterinary antibiotics
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