Simultaneous determination of three classes of antibiotics in the suspended solids of swine wastewater by ultrasonic extraction, solid-phase extraction and liquid chromatography-mass spectrometry.
Simultaneous determination of three classes of antibiotics in the suspended solids of swine wastewater by ultrasonic extraction, solid-phase extraction and liquid chromatography-mass spectrometry.
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DOI：
10.1016/s1001-0742(10)60590-6
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发表时间：
2011-10
影响因子：
6.9
通讯作者：
X. Pan;Z. Qiang;Weiwei Ben;Meixue Chen
中科院分区：
文献类型：
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作者：
X. Pan;Z. Qiang;Weiwei Ben;Meixue Chen
本工作描述了一个系统的方法来发展的方法，同时测定三个类别的兽用抗生素在悬浮固体（SS）的猪废水，包括五个磺胺类，四环素类和大环内酯类（泰妙菌素）。对样品前处理、超声提取、固相萃取、液相色谱-质谱联用等方法进行了研究和优化。磺胺类药物、四环素类药物和泰妙菌素的回收率分别为76%~ 104%、81%~ 112%和51%~ 64%。以相对标准偏差（RSD）表示的日内和日间精密度均低于17%。方法检测限（MDLs）在0.14和7.14 μg/kg之间，取决于研究的特定抗生素。该方法应用于北京、上海和山东三个猪场的现场样品检测。所有被调查的抗生素检测到SS和液相的猪废水，分配系数（logKd）范围从0.49至2.30。本研究表明，在测定猪场废水中抗生素浓度时，SS的影响不容忽视。
This work describes a systematic approach to the development of a method for simultaneous determination of three classes of veterinary antibiotics in the suspended solids (SS) of swine wastewater, including five sulfonamides, three tetracyclines and one macrolide (tiamulin). The entire procedures for sample pretreatment, ultrasonic extraction (USE), solid-phase extraction (SPE), and liquid chromatography-mass spectrometry (LC-MS) quantification were examined and optimized. The recovery efficiencies were found to be 76%-104% for sulfonamides, 81%—112% for tetracyclines, and 51%-64% for tiamulin at three spiking levels. The intra-day and inter-day precisions, as expressed by the relative standard deviation (RSD), were below 17%. The method detection limits (MDLs) were between 0.14 and 7.14 μg/kg, depending on a specific antibiotic studied. The developed method was applied to field samples collected from three concentrated swine feeding plants located in Beijing, Shanghai and Shandong province of China. All the investigated antibiotics were detected in both SS and liquid phase of swine wastewater, with partition coefficients (logKd) ranging from 0.49 to 2.30. This study demonstrates that the SS can not be ignored when determining the concentrations of antibiotics in swine wastewater.