液相色谱-质谱法检测渔业养殖水中硝基呋喃及氯霉素药物  

Determination of 4 Nitrofurans and Chloramphenicol in Fisheries Water by Liquid Chromatography Coupled Tandem Mass Spectrometry

作　　者：张立坚[1] 张俊杰[1] 张良滔[1] 蔡春[1] 

机构地区：[1]广东医学院分析中心,广东湛江524023

出　　处：《质谱学报》2011年第4期207-210,共4页Journal of Chinese Mass Spectrometry Society

基　　金：广东省科技计划项目(2009B020316005)资助

摘　　要：建立了同时测定渔业养殖水中呋喃唑酮、呋喃西林、呋喃妥因和呋喃它酮及氯霉素等5种抗生素药物的超高压液相色谱-电喷雾电离串联质谱（UPLC-ESI-MS/MS）分析方法。水样用HLB萃取柱净化、浓缩后,洗脱液经氮气吹干,残渣用V（乙腈）∶V（水）=1∶1混合溶液溶解,以乙腈和0.1%甲酸水溶液为流动相,经ZORBAX SB-C18色谱柱分离后,用串级质谱多反应监测模式做定性定量分析。该方法在0.5μg/L或1~40μg/L浓度范围内具有良好的线性,相关系数均大于0.996,检出限（S/N=3）为0.5~1μg/L,平均回收率为90.3%~104.2%,相对标准偏差为5.4%~10.0%。An ultra high-pressure liquid chromatography coupled electrospray ionization triple-quadruple tandem mass spectrometry（UPLC-ESI MS/MS） was used for the simultaneous determination of furazolidone,nitrofarazone,nitrofarantoin,furaltadone and chloramphenicol in fisheries water.The drugs were extracted and cleaned up by Oasis HLB solid phase extraction cartridge.The extract was evaporated to dryness under nitrogen and reconstituted in solution with V（acetonitrile）∶V（water）=1∶1.The 5 drugs were separated and detected by ZORBAX SB-C18 using 0.1% formic acid（A） and acetonitrile（B） as mobile phase.The target compounds were confirmed and quantified by MS/MS under multiple reactions monitoring（MRM） mode with external standard method.Under the optimal condition,the calibration curves of 5 drugs show good linearity with the correlation coefficients rather than 0.997 in the range of 0.5 μg/L or 1—40 μg/L,the limits of detection（LODs） range from 0.5—1.0 μg/L（S/N=3）,the average recoveries of 5 drugs are in the range of 90.3%—104.2%,and the relative standard deviations（RSDs） are 5.4%—10.0%.

关 键 词：液相色谱-串联质谱(LC-MS/MS) 硝基呋喃 氯霉素 固相萃取 渔业用水 

分 类 号：O657.63[理学—分析化学]