超高效液相色谱串联质谱法测定渔业水环境中七种氟喹诺酮类药物含量  

Determination of Seven Pieces of Fluoroquinolones Antibiotic Residues in Fishery Water Using Ultra High Performance Liquid Chromatography Coupled With Triple Quadrupole Mass Spectrometry

作　　者：高磊[1,2,3] 王钟强 覃东立 陈中祥[1,2] 吴松 汤施展[1] 黄晓丽 孙承宇[1] 黄丽 郝其睿[1] 白淑艳[1] 杜宁宁 李晨辉[1] 王鹏 GAO Lei;WANG Zhongqiang;QIN Dongli;CHEN Zhongxiang;WU Song;TANG Shizhan;HUANG Xiaoli;SUN Chengyu;HUANG Li;HAO Qirui;BAI Shuyan;DU Ningning;LI Chenhui;WANG Peng(Heilongjiang River Fisheries Research Institute,Chinese Academy of Fishery Sciences,Harbin 150070,China;Supervision,Inspection and Testing Center for Fishery Environment and Aquatic Products(Harbin),Ministry of Agriculture and Rural Affairs,Harbin 150070,China;Key Laboratory of Control of Quality and Safety for Aquatic Products,Ministry of Agriculture and Rural Affairs,Beijing 100041,China;Fisheries Technology Extension Center of Hebei Province,Shijiazhuang 050021,China;Northeast Agricultural University,Harbin 15030,China;Northeast Forestry University,Harbin 150040,China)

机构地区：[1]中国水产科学研究院黑龙江水产研究所,黑龙江哈尔滨150070 [2]农业农村部渔业环境及水产品质量监督检验测试中心(哈尔滨),黑龙江哈尔滨150070 [3]农业农村部水产品质量安全控制重点实验室,北京100141 [4]河北省水产技术推广总站,河北石家庄050021 [5]东北农业大学,黑龙江哈尔滨150030 [6]东北林业大学,黑龙江哈尔滨150006

出　　处：《水产学杂志》2022年第2期59-65,共7页Chinese Journal of Fisheries

基　　金：中央级公益性科研院所基本科研业务费专项(HSY201905Q);国家自然科学基金(32002445);国家重点研发计划(2020YFD0900301);公益性行业(农业)科研专项(201503108);中国水产科学研究院基本科研业务费专项(2019ZD0805);中央级公益性科研院所基本科研业务费专项(HSY2018010Q、HSY201906Q).

摘　　要：本研究建立了磁性固相萃取-超高效液相色谱串联质谱法分析渔业水环境中七种氟喹诺酮类药物残留的检测方法。采用具有磁性的碳纳米管(MCNTs)作为吸附材料,首先在渔业水环境样品中添加MCNTs,经振荡萃取,磁性分离等步骤后,选用甲醇洗脱待测物,再分离洗脱液,置于氮吹仪吹至近干,使用色谱初始流动相定容至1 mL,过有机相滤膜,用超高效液相色谱-串联质谱(UPLC-MS/MS)采集数据,并针对MCNTs质量、洗脱剂种类、萃取时间、回收次数等条件进行优化。结果显示:100 mL水样中加入30 mg吸附材料并萃取20 min,以甲醇作为洗脱剂(1 mL×3次)洗脱,可以达到良好的回收率。诺氟沙星(NFX)、环丙沙星(CFX)、培氟沙星(PEF)、洛美沙星(LOM)、恩诺沙星(EFX)、氧氟沙星(OFX)及氟罗沙星(FLX)七种氟喹诺酮类药物在20~1000 ng/L范围内线性较好,其相关系数均在0.995~1之间,加标回收率范围为76.70%~98.16%,日内、日间相对标准偏差均在2.21%~6.21%之间。在选取的几个渔业水环境样品中发现其中一个样品中检出恩诺沙星和环丙沙星。综上所述,磁性固相萃取具有处理方法简单、重现性好、可批量处理样品、实验成本低等优点,可用于实际检测渔业水域样品中氟喹诺酮类药物的含量。A method was developed for the separation and analysis of seven fluoroquinolones antibiotic residues in fishery water by magnetic solid phase extraction(MSPE)-ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).In the experiment,magnetic carbon nanotubes(MCNTs)were used as adsorbents,and the conditions including amount of MCNTs,eluent and extraction time were optimized.MCNTs were added into the fishery water samples and shaken for extraction,and separated by permanent magnet.Methanol was used to elute the analyzes,and the eluent was separated and placed in a nitrogen gas to dry.The initial mobile phase of the chromatograph was used to re-dissolve the residues.Finally,UPLC-MS/MS was used to analyze the data.The results showed that the optimal adsorption effect were obtained by 30 mg MCNTs in 100 mL water sample for shaking 20 min and eluted by methanol(1 mL×3 times).The seven fluoroquinolone antibiotics(include norfloxacin,ciprofloxacin,pefloxacin,lomefloxacin,enrofloxacin,ofloxacin and fleroxacin)in UPLC-MS/MS have good linearity in the range of 20~1000 ng/L,and the correlation coefficients were all range from 0.995 to 1.The satisfied recoveries(76.70%~98.16%)were obtained and the relative standard deviations within-day and between-days were between 2.21%and 6.21%.The samples have been analyzed,and enrofloxacin and ciprofloxacin were detected in one sample.In summary,M-SPE is featured advantages such as simple handling,good reproducibility,sample batching and low experimental costs.It can be applied to the detection of fluoroquinolones from fishery water.

关 键 词：渔业水环境 磁性固相萃取 超高效液相色谱-串联质谱 氟喹诺酮类药物 

分 类 号：X835[环境科学与工程—环境工程]