鱼肉中兽药残留的UPLC-MS/MS同时检测方法

Establishment of UPLC-MS/MS Simultaneous Detection Method for Veterinary Drug Residues in Fish and Methodological Evaluation

为快速筛查鱼肉中的兽药残留,本文通过样品提取和检测条件优化,建立了可同时检测鱼肉样品中氟苯尼考(FF)、氟苯尼考胺(FFA)、盐酸土霉素(OTC)、磺胺甲恶唑(SMZ)的UPLCMS/MS检测方法,并依据欧盟2002/657/EC进行了方法学评价。结果显示,该方法各项分析检测条件和方法学评价指标均符合欧盟2002/657/EC要求,对4种兽药残留具有良好的线性范围,检出限为0.25~5μg/kg,定量限为0.5~10μg/kg,决定限度为102.8~129μg/kg,检测容量为108.2~170μg/kg,回收率为89.7%~106.5%,日内日间CV≤10.8%。运用该方法对成都市新都区采集的88个鱼肉样品进行检测,数据表明该区域采集的鱼肉样品中主要的抗生素残留为氟苯尼考,且残留量均低于国标规定的最大残留限量值。

In order to rapidly detect veterinary drug residued in fish,a UPLC-MS/MS detection method for simultaneous detection of fluorobenzicol(FF),fluorobenzicolamine(FFA),oxytetracycin hydrochloride(OTC)and sulfamethoxazole(SMZ)in fish fish samples was established through sample extraction and detection condition optimization,and a methodology evaluation was conducted according to the European Union 2002/657/EC.The results show that all the analysis and testing conditions and methodological evaluation indicators of this method meet the requirements of EU 2002/657/EC.This method has good linearity for 4 veterinary drugs.The detection limit is 0.25~5μg/kg and the limit of quantification is 0.5~10μg/kg.The determination limit is 102.8~129μg/kg.Detection capacity is 108.2~170μg/kg;recovery rate is 89.7%~106.5%;CV≤10.8%during the day.This method was used to detect 88 fish samples collected in Xindu District of Chengdu.The data showed that the main antibiotic residue in the fish collected in this area was florfenicol,and the residual amounts were lower than the maximum residue limit value specified by the national standard.