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1、2009年3月色谱Vo.l27No.2March2009ChineseJournalofChromatography138~143高效液相色谱2串联质谱法同时测定鳗鱼和虾中残留的33种喹诺酮和磺胺类药物*王志杰,冷凯良,孙伟红,宁劲松,翟毓秀(中国水产科学研究院黄海水产研究所,山东青岛266071)摘要:建立了鳗鱼和虾中33种喹诺酮类(QNs)和磺胺类(SAs)药物残留量的高效液相色谱2串联质谱(HPLC2MS/MS)测定方法。以氘代试剂为内标,样品经酸性乙腈萃取后,用正己烷脱脂,旋转蒸发浓缩,采用L
2、C2MS/MS选择反应监测(SRM)正离子模式测定,同时对鳗鱼和虾中的33种QNs和SAs进行定性和定量。33种QNs和SAs的检出限(S/N=3)为110Lg/kg,定量限(S/N=10)为210Lg/kg;在1010~20010Lg/L时目标物的峰强度与质量浓度的线性关系良好(r>0199);平均回收率为66%~123%。该法简便快捷,降低了分析成本,也在一定程度上实现了药物残留的快速检测。关键词:高效液相色谱2串联质谱;氘代试剂;内标法;喹诺酮类药物;磺胺类药物;多残留;鳗鱼;虾中图分类号:O6
3、58文献标识码:A文章编号:100028713(2009)0220138206栏目类别:研究论文Simultaneousdeterminationof33quinoloneandsulfonamideresiduesineelsandshrimpsbyhighperformanceliquidchromatography2tandemmassspectrometry*WANGZhijie,LENGKailiang,SUNWeihong,NINGJinsong,ZHAIYuxiu(YellowSeaFi
4、sheriesResearchInstitute,ChineseAcademyofFisherySciences,Qingdao266071,China)Abstract:Themethodforthesimultaneousdeterminationof33quinolone(QN)andsulfona2mide(SA)residuesineelsandshrimpswasdevelopedbyhighperformanceliquidchromatog2raphy2tandemmassspectr
5、ometry(HPLC2MS/MS).Thedeuteriumsubstitutedreagentswhichwereusedasinternalstandardswereaddedtothesamplebeforetheextraction.Thesamplewasextractedwithacidifiedacetonitrile,cleaned2upbyhexane,andconcentratedwitharotaryevaporator.Themassspectrometerwasoperat
6、edinthepositiveionmodeusingselectedreac2tionmonitoringforthequalitativeandquantitativeanalysisof33SAsandQNsatthesametime.Thelimitsofdetectionfor33SAsandQNswere110Lg/kg(S/N=3),andthelimitsofquanti2ficationwere210Lg/kg(S/N=10).Thecorrelationcoefficientsof
7、linearcalibrationcurveswereover0199intheconcentrationrangeof1010-20010Lg/L.Theaveragerecoveriesfor33SAsandQNswerebetween66%and123%.Theadvantagesofthemethodaresimpleoperationandlowcost.Themethodrealizedfastroutineanalysis.Keywords:highperformanceliquidch
8、romatography2tandemmassspectrometry(HPLC2MS/MS);deuteriumsubstitutedreagents;internalstandardmethod;quinolones;sulfonamides;multi2residues;eels;shrimps磺胺类(SAs)和喹诺酮类(QNs)药物均为常见成溶血性贫血症,磺胺二甲嘧啶等甚至有引起潜在的合成抗菌剂,因其具有抗菌谱广、高效、低毒、价格致癌性的可能;Q
