| 摘要: |
| 通过固相萃取-超高效液相色谱-三重四极杆质谱分析系统，对养殖尾水中16种喹诺酮类抗生素进行定性、定量检测。实验结果表明，使用含有0.1%甲酸的甲醇溶液洗脱，0.5%甲酸-5 mmol/L甲酸铵+甲醇溶液（V∶V=95∶5）定容效果最佳，流动相则选择0.5%甲酸-5 mmol/L甲酸铵+甲醇溶液，分离效果最好。此条件下，16种喹诺酮类抗生素均具有较好的线性关系，相关系数为0.998 4～0.999 8，方法检出限为0.03～0.18 ng/L，测定下限为0.14～0.72 ng/L。以休渔期水产养殖排放尾水为基质进行低、中、高质量浓度加标回收实验，回收率为64.9%～107.7%，相对标准偏差为5.4%～14.6%。水产养殖排放尾水实样中16种喹诺酮类抗生素的质量浓度为0～432 ng/L。该方法定性、定量准确，稳定性好，仪器分析时间短，能够满足超痕量分析要求。 |
| 关键词: 超高效液相色谱-三重四极杆质谱 新污染物 喹诺酮类抗生素 固相萃取 养殖尾水 |
| DOI：DOI：10.3969/j.issn.1674-6732.2025.02.009 |
| 分类号:X832 |
| 基金项目:江苏省生态环境监测科研基金项目（2305）；2023年度盐城市基础研究计划指导性项目（YCBK2023071） |
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| Determination of 16 Quinolones in Aquaculture Wastewater by Solid-Phase Extraction-Ultra-High-Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry |
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WANG Ling， LI Haizong*， SHAN Long， ZHAO Xia
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Jiangsu Yancheng Environmental Monitoring Center， Yancheng， Jiangsu 224002， China
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| Abstract: |
| Sixteen quinolone antibiotics in the aquaculture wastewater were qualitatively and quantitatively detected through the comprehensive solid-phase extraction-ultra-high-performance liquid chromatography-triple quadrupole mass spectrometry analysis system. The experimental results showed that polystyrene divinylphenyl-pyrrolidone（HLB） solid-phase extraction column was used for pre-treatment extraction， with elution by methanol solution containing 0.1% formic acid， and a mixture of 0.5% formic acid and 5 mmol/L ammonium formate/methanol solution with 95/5 volume ratio provided the best results. For the mobile phase， 0.5% formic acid and 5 mmol/L ammonium formate solution/methanol provided the best separation. Under this condition， 16 quinolone antibiotics had a good linear relationship， with the correlation coefficient between 0.998 4 and 0.999 8. The method detection limit was 0.03～0.18 ng/L， and the reliable quantitation was 0.14～0.72 ng/L. The discharged wastewater during the fishing moratorium was used as the matrix for low， medium and high concentration spiked recovery experiments， with the recovery rates between 64.9% and 107.7%， and the relative standard deviations between 5.4% and 14.6%. The concentration levels of 16 quinolone antibiotics in the sample analysis were 0～432 ng/L. The method was accurate in qualitative and quantitative analysis， good in stability， and short in instrument analysis time， which could meet the requirements of ultra-trace analysis. |
| Key words: Ultra-high-performance liquid chromatography-triple quadrupole mass spectrometry New pollutants Quinolone antibiotics Solid-phase extraction Aquaculture wastewater |
