固相萃取-超高效液相色谱-三重四极杆质谱法测定养殖尾水中16种喹诺酮类抗生素  

Determination of 16 Quinolones in Aquaculture Wastewater by Solid-Phase Extraction-Ultra-High-Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry

作　　者：王玲 李海宗 单龙 赵霞 WANG Ling;LI Haizong;SHAN Long;ZHAO Xia(Jiangsu Yancheng Environmental Monitoring Center,Yancheng,Jiangsu 224002,China)

机构地区：[1]江苏省盐城环境监测中心,江苏盐城224002

出　　处：《环境监控与预警》2025年第2期68-74,82,共8页Environmental Monitoring and Forewarning

基　　金：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)。

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。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.

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 

分 类 号：X832[环境科学与工程—环境工程]