同位素内标稀释液相色谱-串联质谱法测定鱼贝类组织中残留的环丙氟哌酸

2009年1月January2009色谱ChineseJournalofChromatographyVol.27No.139～433通讯联系人:金米聪,博士,主任技师.Tel:(0574)87274559,E2mail:jmcjc@163.com.基金项目:浙江省医药卫生优秀青年科技人才专项基金(2007QN014).收稿日期:2008206204同位素内标稀释液相色谱2串联质谱法测定鱼贝类组织中残留的环丙氟哌酸陈晓红,王玉飞,姚浔平,金米聪3(宁波市疾病预防控制中心,宁波市毒物研究与控制重点实验室,浙江宁波315010)摘要:建立了不同鱼贝类肌肉组织中以氘代同位素为内标测定环丙氟哌酸残留量的液相色谱2串联质谱(LC2MS/MS)方法。样品加入内标环丙氟哌酸2D8和磷酸盐缓冲溶液(pH710)后进行匀质并用乙腈超声提取,经正己烷脱脂后采用WatersOasisMAX小柱净化,在Cloversil2C18柱上,以乙腈20105%三氟醋酸(体积比为25∶75)为流动相,采用多反应监测(MRM)模式,液相色谱2电喷雾质谱法测定。根据环丙氟哌酸和氘代内标物的定量离子质量色谱图的峰面积比值,采用内标法定量。结果表明,环丙氟哌酸和内标的定量离子峰面积比值与环丙氟哌酸浓度在011～5010μg/kg范围内呈现良好的线性关系,相关系数为019991,方法的定量检测限为011μg/kg,回收率为9215%～9811%,相对标准偏差(RSD)小于413%。将该方法用于市场上10种鱼和贝类样品的检测,结果表明该法具有灵敏、准确的优点,完全满足残留分析的确证检测要求。关键词:固相萃取;液相色谱2串联质谱法;同位素内标;环丙氟哌酸;鱼贝类组织中图分类号:O658文献标识码:A文章编号:100028713(2009)0120039205栏目类别:研究论文Determinationofciprofloxacinresidueinfish/shellfishtissuesusingliquidchromatography2tandemmassspectrometrywithisotopeinternalstandarddilutiontechniqueCHENXiaohong,WANGYufei,YAOXunping,JINMicong3(NingboKeyLaboratoryofPoisonResearchandControl,NingboMunicipalCenterforDiseaseControlandPrevention,Ningbo315010,China)Abstract:Usingisotopeinternalstandarddilutiontechnique,ahighperformanceliquidchro2matography2tandemmassspectrometry(HPLC2MS/MS)methodhasbeendevelopedfortheidentificationandquantitativedeterminationofciprofloxacinresidueinthetissuesofvariousfi2shes/shellfishes.Thehomogenizedtissuesampleaddedwithciprofloxacin2D8andphosphatebuffersolution(pH710)wasextractedwithacetonitrileunderultrasonication,anddegreasedwithhexane.Aftersolid2phaseextraction(SPE)wasperformedonanOasisMAXcartridge,thesamplewasseparatedonaCloversil2C18column(150mm×416mm,5μm)byusingthemobilephaseconsistingofCH3CN20105%CF3COOH(25∶75,v/v).ThedetectionwascarriedoutbyLC2MS/MSusinganelectrosprayionizationinterfaceinmultiplereactionmonitoring(MRM)mode.Thequantificationusingisotope2labelledinternalstandardwasbasedonthepeakarearatioofciprofloxacinanddeuteratedinternalstandardintheMRMmode.Thecali2brationcurvewaslinearwithintherangeof011-5010μg/kgan