超高效液相色谱-质谱联用分析废水中痕量四环素类抗生素

Hua Wang
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引用次数: 0

摘要

建立了测定废水中四环素、土霉素、金四素和强力霉素的综合方法。该方法以超高效液相色谱-质谱联用(UHPLC-MS)技术为基础,具有专属性强、灵敏度高、精密度高、准确度高等特点。4种抗生素的保留时间和准确的m/z值证实了特异性。所有化合物在5-100 ng/mL范围内均具有良好的线性关系。验证了方法的重复性。日内和日间精度均满足要求。检测限和定量限较低,仅为几ng/mL。在3种浓度水平下,加样回收率在95% ~ 104%之间。在当地养猪场采集的混凝土样品中,土霉素含量为15 ng/mL。该方法可用于水样中四环素类抗生素的常规分析。
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Simultaneous Analysis of Trace Tetracyclines Antibiotics in Wastewater with Ultra-high Performance Liquid Chromatography Coupled with Mass Spectrometry
A comprehensive method was developed for determination of tetracycline, oxytetracycline, chlortetracycline, and doxycycline in wastewater. Based on ultra-high performance liquid chromatography coupled with mass spectrometry (UHPLC–MS), the developed method was specific, sensitive, precise, and accurate. Specificity was confirmed with both retention time and accurate m/z value of four antibiotics. Good linearity was achieved for all compounds in the range 5-100 ng/mL. Repeatability of method was proved. The intra-day and inter-day precision were satisfied. The limit of detection and limit of quantification was low enough at several ng/mL. Recoveries were between 95% and 104% at three concentration levels. The concrete sample collected in local swine farm was determined to containing 15 ng/mL oxytetracycline. The developed method provides a reliable and robust tool that can be used for routine analysis of tetracyclines antibiotics in aqueous samples.
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