摘要
建立全自动SPE富集、净化作水产养殖用水中的恩诺沙星、环丙沙星、氨苄西林、双氯西林、头孢氨苄和头孢拉定6种抗生素UPLC-MSMS法定性、定量检测的分析方法。随机在水产养殖池塘中采集水产养殖用水,取约5L,去除杂物后调节pH至中性,取调节pH后水样500mL,以流速25mL·min^(-1)的流速,过固相萃取柱富集、净化,净化液氮吹至近干,残渣加1.0mL丙酮溶解,上UPLC-MS/MS定量检测。恩诺沙星、环丙沙星、氨苄西林、双氯西林、头孢氨苄和头孢拉定在浓度0.001~2.0μg·mL^(-1)范围内,线性关系良好;检出限分别为0.021μg·L^(-1)-0.015μg·L、0.036μg·L^(-1)、0.013μg·L^(-1)、0.020μg·L^(-1)和0.009μg·L^(-1);加样回收率范围在86.1~102.1%;重复性RSD分别为1.9%、2.1%、2.4%、2.3%、2.9%、2.7%。实验结果证明,此方法具有操作简单、准确等特点,可以用于水产养殖用水中抗生素的监测。
To establish a method for qualitative and quantitative determination of enrofloxacin,ciprofloxacin,ampicillin,dicloxacillin,cephalexin and cefradine in aquaculture water by UPLC-MS/MS with automatic SPE enrichment and purification.Randomly collect aquaculture water in aquaculture pond,take about 5 L,adjust pH to neutral after removing sundries,take 500 mL of water sample after adjusting pH,enrich and purify it with solid-phase extraction column at the flow rate of 25 mL·min^(-1),blow purified liquid nitrogen to nearly dry,dissolve the residue with 1.O mL acetone,and conduct quantitative detection with UPLC-MS/MS.enrofloxacin,ciprofloxacin,ampicillin,dicloxacillin,cephalexin and cefradine showed good linear relationships in concentration range of 0.001~2.0μg·mL^(-1).The detection limits were 0.021μg·L^(-1)、0.015μg·L^(-1)-0.036μg·L^(-1)、0.013ug·L^(-1)、0.020μg·L^(-1)and 0.009μg·L^(-1).Average recoveries were in the range86.1~102.1%,relative standard deviation(RSD)of repeatability(n=6)was 1.9%、2.1%、2.4%、2.3%、2.9%、2.7%.The experimental results show that this method is simple and accurate,and can be used to monitor antibiotics in aquaculture water.
作者
董飞
于悦
丁可
徐勇
DONG Fei;YU Yue;DING Ke;XU Yong(Shandong Linyi Ecological Environment Monitoring Center,Linyi 276001,China;Feixian Branch of Linyi Ecological Environment Bureau,Linyi 273400,China)
出处
《化学研究与应用》
CAS
北大核心
2024年第5期1148-1153,共6页
Chemical Research and Application
