QTOF 在食品安全的应用

©2010WatersCorporation|COMPANYCONFIDENTIALWaters四级杆－飞行时间质谱（QTof）食品安全领域应用SYNAPTG2XevoG2QTof©2010WatersCorporation|COMPANYCONFIDENTIAL四极杆质谱VSTOF高灵敏度—串联四极杆MRM模式高选择性—特定的MRM通道高线形范围—定量“黄金标准”法规依从性—一个通道定量，一个通道确认灵敏度受检测化合物数量制约—扫描周期和通道数量历史数据无法再处理—对于新的分析物，需要重新再分析低分辨质量未知化合物定性能力弱优势但是…©2010WatersCorporation|COMPANYCONFIDENTIAL内容WatersQTof特点WatersQTof在食品药物残留快速筛查领域的应用©2010WatersCorporation|COMPANYCONFIDENTIAL内容WatersQTof特点WatersQTof在食品药物残留快速筛查领域的应用©2010WatersCorporation|COMPANYCONFIDENTIAL1.分辨率&精确质量四级杆的分辨率不足以将两个化合物分开ToF具有10,000的分辨率,可以清晰的两个峰分开.质量精度2ppm©2010WatersCorporation|COMPANYCONFIDENTIAL精确质量和元素组成ForC0-100H3-74O0-4N0-4Mass118:closestneighborat34ppmMass500:5compoundswithin5ppmMass750:626compoundswithin5ppm(referenceJ.Am.Soc.MassSpectrom.)©2010WatersCorporation|COMPANYCONFIDENTIAL准确的同位素模型609.2809C33H41N2O9©2010WatersCorporation|COMPANYCONFIDENTIAL例：i-FITFiltersOff(5ppm)Atm/z609,with5ppmerroraroundmass,134possiblecombinationsUsingwiderangeofelements:—C500H1000N20O20S10Cl10Br10©2010WatersCorporation|COMPANYCONFIDENTIAL例i-FITFiltersOff(3ppm)Atm/z609,with3ppmerroraroundmass,81possiblecombinationsUsingwiderangeofelements:—C500H1000N20O20S10Cl10Br10©2010WatersCorporation|COMPANYCONFIDENTIAL仅有精确质量是远远不够的！SummaryConclusion•Highmassaccuracy(1ppm)aloneisnotenoughtoexcludefalsepositives•Theuseofisotopicabundancepatternsasanotherfiltercanfurtherremove95%offalsecandidatesFinalQuote….“Assumingthationspeciesarefullyresolved(eitherbychromatographyorbyhighresolutionmassspectrometry),weconcludethatamassspectrometercapableof3ppmmassaccuracyand2%errorforisotopicabundancepatternsoutperformsmassspectrometerswithlessthan1ppmmassaccuracyorevenhypotheticalmassspectrometerswith0.1ppmmassaccuracythatdonotincludeisotopeinformationinthecalculationofmolecularformulae”©2010WatersCorporation|COMPANYCONFIDENTIAL例i-FITFiltersOn(3ppm)Atm/z609,with3ppmerroraroundmass,andiFitfilters,only1possiblecombinationUsingwiderangeofelements:—C500H1000N20O20S10Cl10Br10IsotopeFiltersturnedon—3%instrumenterror—Carbonrange=+/-3©2010WatersCorporation|COMPANYCONFIDENTIAL精确质量测定给出元素组成信息©2010WatersCorporation|COMPANYCONFIDENTIAL2.QuanTof技术XevoG2QTof性能—分辨率:优于20,000FWHM—质量精度:1ppmRMS—线性范围:104,pDRE模式可扩展—领先的灵敏度水平—采集速度-30张谱谱/秒©2010WatersCorporation|COMPANYCONFIDENTIALQuanTof技术，带来一张谱图内的动态线性范围在一张复杂的谱图内获得超过4个数量级的动态线性范围PEGC18H38O10NaObservedMass437.23640.1mDaErrorm/z455.280455.300455.320455.340%010011FEB10_00126(0.890)TOFMSES+2.76e3455.2901m/z300350400450500550600%010011FEB10_00126(0.890)TOFMSES+4.11e7437.2364393.2104349.1837481.2628525.2884VerapamilC27H38N2O4ObservedMass455.29010.9mDaError©2010WatersCorporation|COMPANYCONFIDENTIALQuanTof技术,带来精确质量的定量性能Alprazolamspikedintoplasma:Calibrationcurveshowing4ordersoflineardynamicrangeforquantitativestudies.Standardconcentrationsarebetween0.05and500ng/mLCompoundname:AlprazolamCorrelationcoefficient:r=0.999587,r^2=0.999174Calibrationcurve:1.18828*x+-0.0262545Responsetype:InternalStd(Ref1),Area*(ISConc./ISArea)Curvetype:Linear,Origin:Exclude,Weighting:1/x,Axistrans:Noneng/mL050100150200250300350400450500Response0100200300400500600©2010WatersCorporation|COMPANYCONFIDENTIAL一张色谱图内的精确质量稳定性©2010WatersCorporation|COMPANYCONFIDENTIALLockmass：在线的UPLC/MS精确质量采集聪明的途径获得精确质量(EM)LockSpray:3.LockSpray©2010WatersCorporation|COMPANYCONFIDENTIAL仪器的质量校正©2010WatersCorporation|COMPANYCONFIDENTIALLockSprayReferenceAnalyteAnalyticalDataLockSprayData©2010WatersCorporation|COMPANYCONFIDENTIAL4.WatersMSE专利技术Collisioncell0.nsecUPLC/MSEisasimple,patentedmethodofunbiaseddataacquisitionthatcomprehensivelycatalogscomplexsamplesinasingleanalysis.©2010WatersCorporation|COMPANYCONFIDENTIALUPLC/MSE所有数据，所有时间LowCEspectrumHighCEspectrum1.高分离的UPLC数据2.强大的软件解析能力所以，无论您想对目标化合物还是未知化合物进行结构确认–您可以快速、简便地获得高质量的化合物母离子和碎片离子信息©2010WatersCorporation|COMPANYCONFIDENTIALEngineeredSimplicity工程精简1.创新的离子源设计简便的设置灵敏稳定2.IntelliStart:简单的操作所有的仪器校正和系统设置可以自动执行5.EngineeredSimplicity©2010WatersCorporation|COMPANYCONFIDENTIAL创新的离子源设计UniversalsourcearchitectureEnablesthewidestrangeofionizationtechniquestobeutilizedESI,APCI,ESCInanoFlowESI,TRIZAICAPPI,ASAP,APGCCompatiblewiththirdpartysources(DESI,DART,etc)Simpleandtool-freeAllowingyoutochangebetweenionsourceoptionsinminutes.©2010WatersCorporation|COMPANYCONFIDENTIALUniversalSourceTechnology…HighPerformanceandsimplicityofoperationTRIZAIC™SourcewithnanoTileTechnology.Plug&PlaynanoFlowAPGC–AtmosphericPressureGasChromatographyASAP–AtmosphericPressureSolidsAnalysisProbeMALDInanoFlowESIAPCiESCiAPPITRIZAICASAPAPGC‘Game-Changing’…accessesthewidestrangeofcompoundsandapplications5©2010WatersCorporation|COMPANYCONFIDENTIAL内容WatersQTof特点WatersQTof在食品药物残留快速筛查领域的应用©2010WatersCorporation|COMPANYCONFIDENTIALWatersQTof在食品药物残留快速筛查领域的应用FoodScreening目标化合物筛查半目标化合物筛查未知化合物筛查©2010WatersCorporation|COMPANYCONFIDENTIAL目标或半目标化合物筛查目标化合物筛查关注的是那些需要限定含量的特定化合物—目标化合物筛查:化合物在MS采集前设定好范围，范围外那些出现的化合物不会被检测o典型的是那些基于四极杆作为第一质量分析器的方法，比如MRM模式(QqQ)或者子离子扫描（QTOF）—半目标化合物筛查:通用的数据采集，采集后指定需要筛查的化合物o主要是基于全扫描模式的方法，比如TOF非目标化合物筛查在事先不知道任何关于化合物信息或者样品基质组成的情况下寻找“未知化合物”o基于全扫描模式的检测技术o需要功能强