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.
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)
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)。
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
Ultra-high-performance liquid chromatography-triple quadrupole mass spectrometry
New pollutants
Quinolone antibiotics
Solid-phase extraction
Aquaculture wastewater
