基于高效液相色谱—四级杆—飞行时间质谱技术筛查渔业水域环境中抗生素残留方法的建立与应用

Determination of antibiotic residues in fishery water environment by high performance liquid chromatography quadrupole time of flight mass spectrometry and its application

应用高效液相色谱—四级杆—飞行时间质谱（HPLC-Q-TOF-MS）技术建立水中常用的42种抗生素残留快速筛查方法。采用固相萃取富集净化的方法进行样品预处理,目标药物经液相色谱仪C18反相柱分离,1%甲酸乙酸铵水溶液—甲醇溶液为流动相梯度洗脱,利用正离子源全扫描模式进行检测,并将建立的方法应用于浙江省内主要渔业环境水质样品抗生素残留的筛查工作。渔业水域环境中42种抗生素定量限（LOQ,S/N=10）为0.010-0.120μg/L。3个水平加标的平均回收率为60.7%-97.1%,相对标准偏差（RSD）为0.58%-8.01%。该方法快速简便,灵敏度高,对抽取的60批次样品进行检测,共检出磺胺甲鰁唑、磺胺间甲氧基嘧啶、磺胺吡啶、磺胺氯哒嗪、恩诺沙星5种药物,含量为25.6-106.7 ng/L。本实验建立的渔业水质中抗生素药物的高效液相色谱—四级杆串联飞行质谱分析方法,灵敏、准确、定性能力强,可以成功应用于渔业环境水质样品抗生素残留的筛查工作。

Rapid screening method for 42 kinds of commonly used antibiotics residues in fishery water by High performance liquid chromatography combined with quadrupole time-of-flight mass spectrometry （HPLC-Q-TOF- MS） has been developed. Targeted antibiotics was extracted from samples on C18 Solid-phase extraction cartridges. Analytical separation was performed on a C18 reverse phase column by liquid chromatography with 1% acetic acid, formic acid, ammonium salt aqueous methanol solution as mobile phase. Positive ion source full scan patterns were used. The result showed that Limit of Quantity （S/N=10, LOQ） of 42 kinds of antibiotics were 0.010 - 0.120 μg/L. The average recovery for antibiotics was 60.7% - 97.1%. The relative standard deviation （RSDs） was 0.58% - 8.01%. The method is rapid and simple with high sensitivity. 60 fishery water samples were determined and sulfamethoxazole, sulfamonomethoxine, sulfapyridine, sulfachlorpyridazine, enrofloxacin were detected with the concentration from 25.6 to 106.7 ng/L. The method is sensitive, accurate and can be applied to the screening of antibiotic residues in fishery water environment.