同位素内标—超高效液相色谱—串联质谱法测定城镇污水处理厂废水中5种四环素类抗生素

采用同位素内标定量,应用超高效液相色谱—串联质谱法建立了城镇污水处理厂废水中5种四环素类抗生素的检测方法。水样经OasisHLB固相萃取小柱富集纯化后,以Thermo Hypersilgold色谱柱(150mm×2.1mm,3.0μm)分离待测物,以0.1%(体积分数)甲酸水溶液和甲醇为流动相进行梯度洗脱,质谱分析采用电喷雾正电离源和多反应监测模式。实验结果表明,5种四环素类抗生素在1~100μg/L间具有良好的线性,取样量为1L时,检出限在0.680~0.859ng/L之间,空白加标回收率为72.5%~124%,精密度为0.7%~13.5%。将该方法应用于2座城镇污水处理厂废水中抗生素的测定,其加标回收率为68.4%~131%。该方法简便、准确、稳定,能满足城镇污水处理厂废水中多种四环素类抗生素的同时测定。

A method based on ultra high performance liquid chromatography-tandem mass spectrometry with isotope internal standard was developed for the determination of 5 tetracycline antibiotics in wastewater from urban sewage treatment plant. The sample was enriched and purified by Oasis HLB solid phase extraction(SPE) column. And the analytes were separated on a thermo Hypersil gold column(150 mm×2.1 mm,3.0 μm), with 0.1%(volume fraction) formic acid solution and methanol as the mobile phase for gradient elution. Electrospray positive ion source and multiple reaction monitoring mode were used in mass spectrometry analysis. Results showed that all 5 tetracycline antibiotics showed good linearity in the range of 1~100 μg/L. The method detection limits(MDLs) of 5 tetracycline antibiotics ranged from 0.680 ng/L to 0.859 ng/L with 1.0 L sampling volume. On the basis of blank sample, the recovery rate were ranged from 72.5%~124%, and the RSD were ranged from 0.7%~13.5%.The method was applied in the determination of antibiotics residues in wastewater from 2 urban sewage treatment plant, with the recovery value ranged from 68.4%~131%.The established method with convenience, accuracy and stability is suitable for determination of simultaneous determination of multiple tetracycline antibiotics in wastewater from urban sewage treatment plant.