本文建立了固相萃取与高效液相色谱-串联质谱联用(HPLC-MS-MS)检测污水中8种氟喹诺酮类(FQs)抗生素残留的分析方法.样品经HLB固相萃取柱富集、净化后,用5%氨水-甲醇(V/V)溶液洗脱,洗脱液经N2浓缩定容后,以Acclaim 120 C18柱分离,高效液相色谱-串联质谱仪多反应监测正离子模式(MRM)定性、定量分析.以去离子水和污水为基质,诺氟沙星-d5为替代物进行回收率评价,8种氟喹诺酮类抗生素在加标浓度为100ng·l^-1和25ng·l^-1时的回收率为73.8%—113%和56.8%—115%,相对标准偏差(RSD)为2.60%—13.2%和3.70%—12.3%(n=4),方法检出限为0.2—1 ng·l^-1.对北京市7大污水处理厂进出口污水中氟喹诺酮类抗生素进行残留分析,结果表明7大污水处理厂进出口污水中均有FQs检出,其中氧氟沙星含量最高.
A method for determination of eight fluoroquinolone antibiotics(FQs) in wastewater samples was developed by high performance liquid chromatography coupled with tandem mass spectrometry.FQs in water samples were enriched and cleaned by HLB solid phase extraction cartridge,and then separated by Acclaim 120 C18 column and analyzed in positive mode using multiple reaction monitoring.Using Nor-d5 as surrogate,the recoveries and relative standard deviations(RSD,n=4) of FQs in deionized water and wastewater samples were 73.8%—113% and 2.60%—13.2% at spiked level of 100ng·l^-1 and 56.8%—115% and 3.70%—12.3% at spiked level of 25ng·l^-1,respectively.The method detection limits ranged in 0.2—1ng·l^-1.Finally,the method was applied to determine the FQs in influent and effluent of seven wastewater treatment plants of Beijing.The results showed that FQs were detected in all samples and the concentration of ofloxacin was the highest.