| 摘要: |
| 采用固相萃取-超高效液相色谱三重四极杆质谱联用法，建立了同时测定养殖废水中9种大环内酯及林可酰胺类抗生素的方法，并对样品pH值、保存时间、洗脱溶剂、上样流速及过滤材质等进行了优化。测定结果表明，pH值为6，过滤材质为聚丙烯（GHP），上样速度为5 mL/min时，9种抗生素的加标回收率最优，为71.4%～126%，相对标准偏差最小，为2.4%～7.1%，标准曲线的线性最好，相关系数为0.998 5～0.999 5,检出限为0.78～1.22 ng/L。该方法灵敏度高、检出限低、测定结果准确，能够广泛应用于养殖废水中大环内酯及林可酰胺类抗生素残留量的监测分析。 |
| 关键词: 大环内酯 固相萃取 液相色谱-串联质谱 抗生素 |
| DOI： |
| 分类号:X703.1 |
| 基金项目:重庆市生态环境局基金科研项目（A21017602） |
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| Simultaneous Determination and Analysis of 9 Macrolide and Lincosamide Antibiotics in Aquaculture Waste Water |
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ZHANG Wen-bin， ZHENG Xuan，ZHAO Jing，LIU Can，WANG Jian
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Ecological and Environmental Monitoring Center of Chongqing, Chongqing 401147, China
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| Abstract: |
| A method was established for the simultaneous determination of 9 macrolides and lincosamides in aquaculture wastewater by solid-phase extraction ultra performance liquid chromatography triple quadrupole mass spectrometry. The pH value and storage time of samples, eluent solvent, sample loading speed and filter material were optimized. The determination results show that when the pH value is 6, the filter material is GHP, and the sample loading speed is 5 mL/min, the standard addition recovery rate of the nine antibiotics is the best, ranging from 71.4% to 126%, and the relative standard deviations are the smallest, ranging from 2.4%～7.1%, the linearity of the standard curves are the best, the correlation coefficients are in the range of 0.998 5～0.999 5, and the detection limits are in the range of 0.78～1.22 ng/L. The method has high sensitivity, low detection limit and accurate determination results, and it can be widely used in monitoring and analysis of macrolide and lincosamide antibiotic residues in aquaculture wastewater. |
| Key words: Macrolide Solid phase extraction Liquid chromatography tandem mass spectrometry Antibiotics |
