摘要
采用优化固相萃取-液相色谱-串联质谱同步检测养猪废水中24种抗生素的.水样用1 mol·L^(-1)盐酸调节p H值至3.5—4.0,流经Oasis HLB固相萃取柱富集后再用甲醇和乙酸乙酯(V∶V=1∶1)进行洗脱.以Agilent eclipse plus C_(18)色谱柱为分离柱,以0.1%甲酸水溶液和乙腈为流动相进行梯度洗脱,采用电喷雾正离子源,多反应监测模式检测.24种抗生素的检出限(S/N=3)在0.03—3.00μg·L^(-1)之间.进一步以不同养猪场废水进行实际样品测定,四环素类、大环内酯类、β-内酰胺类、喹诺酮类、磺胺类等5大类抗生素均有检出,土霉素、替米考星和磺胺甲嘧啶等3种抗生素为主要污染抗生素,最高浓度可达147.10、107.83、100.20μg·L^(-1),磺胺甲噻二唑及去甲基金霉素均未检出.本研究建立了快速准确的同步分析5大类24种抗生素的分析方法.
An optimized method employing solid phase extraction-liquid chromatography-tandem mass spectrometry was established for the simultaneous determination of 24 antibiotics in swine wastewater. After adjusting p H to 3.5—4.0 by using 1 mol·L$Research Center for Eco-Environmental Sciences,Chinese Academy of Sciences!Beijing, 100085,China hydrochloric acid,the samples were concentrated and collected after flowing through an Oasis HLB solid-phase extraction column,and were eluted with methanol and ethyl acetate（ V ∶ V = 1∶1）. The gradient elution was carried out with0.1%（ V ∶ V） formic acid solution and acetonitrile as the mobile phase by using the Agilent eclipse plus C_（18） column,and the detection was performed under the monitoring mode of the electrospray ionization source multiple reaction. The limit of detection（ S/N = 3） of the 24 antibiotics wasbetween 0. 03—3. 00 μg·L$Research Center for Eco-Environmental Sciences,Chinese Academy of Sciences!Beijing, 100085,China. Tetracyclines,macrolides,β-lactams,quinolones and sulfonamides were all detected by this method in the swine wastewater samples. As the three main antibiotics,oxytetracycline,tilmicosin and sulfamethoxazole were found to have a maximum concentration of147.10,107. 83 and 100. 20 μg · L$Research Center for Eco-Environmental Sciences,Chinese Academy of Sciences!Beijing, 100085,China, respectively whereas sulfadoxadiazole and dimethyl chlortetracycline were not detected. The rapid and accurate detection of 24 antibiotics in 5 major classes was established.
作者
柴玉峰
冯玉启
张玉秀
陈梅雪
王瑞
柳蒙蒙
魏源送
CHAI Yufeng FENG Yuqi ZHANG Yuxiu CHEN Meixue WANG Rui LIU Mengmeng WEI Yuansong(School of Chemical ＆ Environmental Engineering, China University of Mining and Technoiogy,Beijing, 100083, China School of Energy ＆ Environmental Engineering, Beijing University of Civil Engineering and Architecture, Beijing, 100044, China Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing, 100085, China)
出处
《环境化学》
CAS
CSCD
北大核心
2017年第10期2147-2154,共8页
Environmental Chemistry
基金
国家自然科学基金(41501513,21577161)
中央高校基本科研业务费专项(2010YH05)
国家科技重大专项参与单位任务(2015ZX07203-007-003)
国家重点研发计划课题(2016YFD0501405)资助~~
