CAJ | 학술논문

建立了水产品中左氧氟沙星残留的超高效液相色谱串联质谱检测法。采用乙腈对样品中的待测物进行提取,正已烷除脂,浓缩后用固相萃取小柱进行净化,吹氮浓缩后采用超高效液相色谱质谱联用-电喷雾正离子和MRM多反应监测模式进行定性定量分析。检测浓度线性范围为0～100μg/kg,线性相关系数为0.9922,检出限为4.5μg/kg。在鳗鱼、虾和罗非鱼三种不同样品基质中进行添加浓度为10,20,50μg/kg的验证试验,该药物的回收率在72.5%～83.5%内,相对标准偏差（n=6）在7.9～11.4%之间,并对其质谱裂解和基质效应进行了研究。本检测方法快速,高效,灵敏度高,符合检测要求。
건립료수산품중좌양불사성잔류적초고효액상색보천련질보검측법。채용을정대양품중적대측물진행제취,정이완제지,농축후용고상췌취소주진행정화,취담농축후채용초고효액상색보질보련용-전분무정리자화MRM다반응감측모식진행정성정량분석。검측농도선성범위위0～100μg/kg,선성상관계수위0.9922,검출한위4.5μg/kg。재만어、하화라비어삼충불동양품기질중진행첨가농도위10,20,50μg/kg적험증시험,해약물적회수솔재72.5%～83.5%내,상대표준편차（n=6）재7.9～11.4%지간,병대기질보렬해화기질효응진행료연구。본검측방법쾌속,고효,령민도고,부합검측요구。
An analytical method was developed with Ultra Performance Liquid Chromatography Tandem Mass Spectrometry to determine Levofloxacin residues in aquatic products.The compound was extracted with acetonitrile and cleaned with hexane,followed by cleanup with LC-SCX SPE column,and concentrated with N2.Then the reconstituted sample solution was qualitative and quantitative analysis by UPLC-MS/MS under electrospray positive ion mode and multi-reaction monitoring（MRM）.The coefficient correlation of this method was 0.9922 for spiked samples（range from 0 to 100μg/kg）,the limit of quantification were 4.5 μg/kg.The method was validated at 10,20,50μg/kg in eel,shrimp and tilapia fish,the mean recoveries were 72.5%-83.5%,the RSD were 7.9-11.4%,investigated the MS fragmentation mechanism of this compound.The method is effective,fast and high sensitivity,meet the request of detection.