加速溶剂萃取-高效液相色谱-串联质谱法同时检测鱼肉中喹诺酮、磺胺与大环内酯类抗生素  

Simultaneous Determination of Quinolones,Sulfonamides and Macrolides in Fish Samples Using Accelerated Solvent Extraction Followed by High Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

作　　者：厉文辉[1] 史亚利[1] 高立红[2] 刘杰民[2] 蔡亚岐[1] 

机构地区：[1]中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室,北京100085 [2]北京科技大学土木与环境工程学院,北京100083

出　　处：《分析测试学报》2010年第10期987-992,共6页Journal of Instrumental Analysis

基　　金：国家自然科学基金重点资助项目(20837003);国家自然科学基金重大资助项目(20890111);国家973项目子课题资助项目(2009CB421605)

摘　　要：建立了加速溶剂萃取(ASE)-高效液相色谱-串联质谱联用法同时检测鱼肉中22种抗生素药物残留的分析方法。样品经ASE提取,HLB固相萃取柱净化后进入高效液相色谱-串联质谱仪分析。对ASE的萃取条件进行优化,并采用XTerraMSC18柱对药物进行分离,以甲醇-乙腈(体积比1∶1)为色谱流动相A,以0.3%(体积分数)甲酸水溶液(含0.1%甲酸铵,pH=2.9)为流动相B。22种喹诺酮、磺胺和大环内酯类抗生素药物在加标水平为20、100μg/L时的回收率分别为72%～120%与66%～114%,相对标准偏差(RSD,n=5)分别为1.9%～16%与0.7%～10%,方法的检出限为0.02～0.6μg/kg。结果显示所建立的方法精密度好,准确度高,可满足同时对鱼肉样品中多种喹诺酮、磺胺和大环内酯类抗生素残留进行定性及定量分析的要求。A method for the simultaneous analysis of 22 antibiotics（quinolones,sulfonamides and macrolides）in fish samples was developed.The target compounds were extracted using accelerated solvent extraction（ASE）and purified by solid phase extraction（SPE）using a hydrophilic-lipophilic balanced（HLB）polymer.The ASE conditions were optimized.The optimum ASE conditions were using methanol as the extraction solvent at temperature of 70 ℃,pressure of 10.34 MPa and extraction time of 15 min.The eluate was collected and concentrated to 1 mL under a gentle stream of nitrogen gas,and then analyzed by HPLC-ESI MS/MS under positive electrospray ionization and multiple reaction monitoring（MRM）mode.The separation of analytes was carried out on a XTerra MS C18 column with methanol-acetonitrile（1∶1,by volume）as mobile phase A and 0.3% formic acid（containing 0.1% ammonium formate,pH=2.9）as mobile phase B.The recoveries of all the compounds from fish muscles at two concentration levels of 20 and 100 μg/L were in the range of 72%-120% and 66%-114%,respectively,with the corresponding relative standard deviations（RSD,n=5）of 1.9%-16% and 0.7%-10%,respectively.The method detection limits ranged from 0.02 μg/kg to 0.6 μg/kg.The method could be applied in the analysis of quinolones,sulfonamides and macrolides in fish muscle samples with good precision and accuracy.

关 键 词：加速溶剂萃取 高效液相色谱-串联质谱 喹诺酮 磺胺 大环内酯 鱼肉 

分 类 号：O657.72[理学—分析化学] TQ460.72[理学—化学]