离子液体磁性石墨烯-超高效液相色谱串联质谱法测定水中的磺胺类抗生素
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摘要
建立了离子液体磁性石墨烯(IL@MGO)固相萃取-超高效液相色谱质谱法测定环境水体中的磺胺类抗生素(SAs)。采用一步法制备IL@MGO,通过SEM和TEM等手段对IL@MGO表面结构进行表征,并对磁性固相萃取条件进行优化。利用该法检测6种SAs的检出限为0. 75～1. 47 ng/L,定量限为1. 51～4. 96 ng/L。利用该方法对污水厂的进出水进行分析,加标回收率在86. 4%～103. 4%,相对标准偏差在1. 1%～12. 5%之间。
A method is established to determine sulfonamide antibiotics(SAs) in environmental water by ionic liquid magnetic graphene(IL @ MGO) solid phase extraction-ultra high-performance liquid chromatography-mass spectrometry.IL@ MGO is made via one-step method. The surface structure of IL @ MGO is characterized by means of SEM and TEM,and the conditions for magnetic solid phase extraction are optimized.The detection limit and quantification limit for six kinds of sulfonamide antibiotics is 0. 75-1. 47 ng·L-1 and 1. 51-4. 96 ng·L-1,respectively. When this method is used to detect the influent and effluent water in two sewage treatment plants,the recovery rate is between86. 4% and 103. 4% and the relative standard deviation is between 1. 1% and 12. 5%.
A method is established to determine sulfonamide antibiotics(SAs) in environmental water by ionic liquid magnetic graphene(IL @ MGO) solid phase extraction-ultra high-performance liquid chromatography-mass spectrometry.IL@ MGO is made via one-step method. The surface structure of IL @ MGO is characterized by means of SEM and TEM,and the conditions for magnetic solid phase extraction are optimized.The detection limit and quantification limit for six kinds of sulfonamide antibiotics is 0. 75-1. 47 ng·L-1 and 1. 51-4. 96 ng·L-1,respectively. When this method is used to detect the influent and effluent water in two sewage treatment plants,the recovery rate is between86. 4% and 103. 4% and the relative standard deviation is between 1. 1% and 12. 5%.
引文
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[19]王栋纬,宋燕西,冶晓凡,等.氧化石墨烯对磺胺甲唑和磺胺甲基嘧啶的吸附性能研究[J].分析化学,2018,46(2):211-216.
[20]Zhu Xiaobo,Mo Zunli,Zhang Chun,et al.Preparation of grapheneFe3O4nanocomposites using Fe3+ion-containing magnetic ionic liquid[J].Materials Research Bulletin,2014,59:223-226.
[2]章强,辛琦,朱静敏,等.中国主要水域抗生素污染现状及其生态环境效应研究进展[J].环境化学,2014,33(7):1075-1083.
[3]Ma Y P,Miao L,Wu M,et al. Occurrences and regional distributions of 20 antibiotics in water bodies during groundwater recharge[J]. Science of the Total Environment,2015,518-519:498-506.
[4]Li Y,Wu X,Li Z,et al.Fabrication of CoFe2O4-graphene nanocomposite and its application in the magnetic solid phase extraction of sulfonamides from milk samples[J].Talanta,2015,144(6):1279-1286.
[5]王建凤,杜振霞,王颖,曹沅,等.过滤型固相萃取-超高效液相色谱/质谱法快速测定牛奶中喹诺酮及磺胺类药物[J].分析试验室,2018,37(5):599-603.
[6]赵海香,刘海萍,闫早婴.多壁碳纳米管固相萃取净化-高效液相色谱法测定猪肉和鸡肉中的磺胺多残留[J].色谱,2014,32(3):294-298.
[7]吴小莲,包艳萍,向垒,等.固相萃取-高效液相色谱-串联质谱法同时测定蔬菜中8种磺胺类抗生素[J].环境化学,2013,32(6):1038-1044.
[8]洪蕾洁,石璐,张亚雷,等.固相萃取-高效液相色谱法测定养殖水体中磺胺类抗生素[J].环境科学学报,2012,27(6):493-507.
[9]崔先锋,胡爱军,刘伶俐,等.固相萃取-高效液相色谱法测定养殖水体中磺胺类抗生素[J].湖南农业,2016,4:83-86.
[10]李锋格,苏敏,李晓岩,等.分散固相萃取-超高效液相色谱-串联质谱法测定鸡肝中磺胺类、喹诺酮类和苯并咪唑类药物及其代谢物的残留量[J].色谱,2011,29(2):120-125.
[11]张盈,李晓刚,徐军等.分散固相萃取-超高效液相色谱-串联质谱联用快速检测大豆及土壤中氟磺胺草醚残留[J].环境化学,2012,31(9):1399-1404.
[12]吴翠琴,雷金妹,李韵灵,等.基于离子液体的分散液液微萃取-柱前荧光衍生高效液相色谱法测定水样中8种磺胺类药物[J].色谱,2014,32(12):1362-1367.
[13]张晶,彭敬东,周明琼,等.分散液液微萃取-高效液相色谱法测定水中磺胺类药物残留[J].分析试验室,2014,33(9):993-997.
[14]王慧.动态微波辅助萃取食品和环境样品中有害物质的研究[D].长春:吉林大学,2013.
[15]游辉,于辉,武彦文,等.快速溶剂萃取-基质固相分散-高效液相色谱法测定牛肉中5种磺胺类药物残留[J].分析测试学报,2010,29(10):1087-1090.
[16]Zhao B,He M,Chen B,et al.Novel ion imprinted magnetic mesoporous silica for selective magnetic solid phase extraction of trace Cd followed by graphite furnace atomic absorption spectrometry detection[J].Spectrochimica Acta Part B Atomic Spectroscopy,2015,107:115-124.
[17]Pan S D,Chen X H,Shen H Y,et al.Rapid and effective sample cleanup based ongraphene oxide encapsulated core-shell magnetic microspheres for determination of fifteen trace environmental phenols in seafood by liquid chromatography-tandem mass spectrometry[J].Analytica Chimica Acta,2016,919:34-46.
[18]张利锋,高玉双,张金振,等.离子液体掺杂石墨烯的制备表征及分散性研究[J].陕西科技大学学报,2015,33(4):41-44.
[19]王栋纬,宋燕西,冶晓凡,等.氧化石墨烯对磺胺甲唑和磺胺甲基嘧啶的吸附性能研究[J].分析化学,2018,46(2):211-216.
[20]Zhu Xiaobo,Mo Zunli,Zhang Chun,et al.Preparation of grapheneFe3O4nanocomposites using Fe3+ion-containing magnetic ionic liquid[J].Materials Research Bulletin,2014,59:223-226.