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

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.