Capillary Electrophoresis-Mass Spectrometry: Methods and Protocols (Methods in Molecular Biology, 2531) PDF
Preview Capillary Electrophoresis-Mass Spectrometry: Methods and Protocols (Methods in Molecular Biology, 2531)
Methods in Molecular Biology 2531 Christian Neusüß · Kevin Jooß Editors Capillary Electrophoresis- Mass Spectrometry Methods and Protocols M M B ETHODS IN OLECULAR IO LO GY SeriesEditor JohnM.Walker School of Lifeand MedicalSciences University ofHertfordshire Hatfield, Hertfordshire, UK Forfurther volumes: http://www.springer.com/series/7651 For over 35 years, biological scientists have come to rely on the research protocols and methodologiesinthecriticallyacclaimedMethodsinMolecularBiologyseries.Theserieswas thefirsttointroducethestep-by-stepprotocolsapproachthathasbecomethestandardinall biomedical protocol publishing. Each protocol is provided in readily-reproducible step-by step fashion, opening with an introductory overview, a list of the materials and reagents neededtocompletetheexperiment,andfollowedbyadetailedprocedurethatissupported with a helpful notes section offering tips and tricks of the trade as well as troubleshooting advice. These hallmark features were introduced by series editor Dr. John Walker and constitutethekeyingredientineachandeveryvolumeoftheMethodsinMolecularBiology series. Tested and trusted, comprehensive and reliable, all protocols from the series are indexedinPubMed. Capillary Electrophoresis-Mass Spectrometry Methods and Protocols Edited by Christian Neusüß and Kevin Jooß Aalen University, Aalen, Baden-Württemberg, Germany Editors ChristianNeusu¨ß KevinJooß AalenUniversity AalenUniversity Aalen,Baden-Wu¨rttemberg,Germany Aalen,Baden-Wu¨rttemberg,Germany ISSN1064-3745 ISSN1940-6029 (electronic) MethodsinMolecularBiology ISBN978-1-0716-2492-0 ISBN978-1-0716-2493-7 (eBook) https://doi.org/10.1007/978-1-0716-2493-7 ©SpringerScience+BusinessMedia,LLC,partofSpringerNature2022 Thisworkissubjecttocopyright.AllrightsarereservedbythePublisher,whetherthewholeorpartofthematerialis concerned,specificallytherightsoftranslation,reprinting,reuseofillustrations,recitation,broadcasting,reproduction onmicrofilmsorinanyotherphysicalway,andtransmissionorinformationstorageandretrieval,electronicadaptation, computersoftware,orbysimilarordissimilarmethodologynowknownorhereafterdeveloped. Theuseofgeneraldescriptivenames,registerednames,trademarks,servicemarks,etc.inthispublicationdoesnotimply, evenintheabsenceofaspecificstatement,thatsuchnamesareexemptfromtherelevantprotectivelawsandregulations andthereforefreeforgeneraluse. Thepublisher,theauthorsandtheeditorsaresafetoassumethattheadviceandinformationinthisbookarebelievedto betrueandaccurateatthedateofpublication.Neitherthepublishernortheauthorsortheeditorsgiveawarranty, expressedorimplied,withrespecttothematerialcontainedhereinorforanyerrorsoromissionsthatmayhavebeen made.Thepublisherremainsneutralwithregardtojurisdictionalclaimsinpublishedmapsandinstitutionalaffiliations. ThisHumanaimprintispublishedbytheregisteredcompanySpringerScience+BusinessMedia,LLC,partofSpringer Nature. Theregisteredcompanyaddressis:1NewYorkPlaza,NewYork,NY10004,U.S.A. Preface Capillary electrophoresis-mass spectrometry (CE-MS) is still an underutilized technique compared to the widespread liquid chromatography-mass spectrometry (LC-MS). Never- theless,theselectivitymakesCE-MSanattractivetoolinmanyfieldsofapplicationwhichis oftentimes considered complementary to traditional LC separation. In general, electromi- grativetechniquesseparateionsbasedontheircharge-to-sizeratioand/orisoelectricpoint. Consequently, high separation efficiency can be achieved, ideally resulting in exceptionally sharp peaks under diffusion-limited conditions. In this way, it is possible to resolve closely related species such as isomeric molecules (including enantiomers) or proteoforms varying inonlyoneposttranslationalmodification. CErequirestheapplicationofhighelectricfieldstoperformreasonablyfastandefficient separations, resulting in high electric currents. Consequently, efficient heat dissipation is requiredtoavoidpeakbroadeningandbubbleformationduetoJouleheating.Thisleadsto smallgeometrieswithrelativelyhighsurfaceresultingintotalcapillaryvolumestypicallyin thesingledigitmicroliterrange.Thus,CEisamicrofluidicseparationtechniqueconsidered environmentally friendly due to its low consumption of resources (e.g., solvents). For the samereason,CE-MSisparticularlysuitablefor theanalysisofvaluablesamples,e.g.,ifonly minor amounts are available. However, on the other hand, analytes need to be sufficiently concentrated for sensitive detection. In addition, the handling of small volumes requires specialcareandcanbetechnicallychallenging. Mass Spectrometry (MS) acts as a universal and selective technique for molecule characterization and can be applied in both targeted and nontargeted fashion. In the last decades, enormous progress has been made in MS technology leading to high sensitivity, high speed, increased resolving power, the ability for selective fragmentation of small and largemolecules,andlastbutnotleastimprovedoverallusability.Still,separationtechniques arecrucialduetopossibleinterferenceduringtheionizationprocessandmassspectrometric resolution being limited, which is especially important in the context of complex samples. ElectrosprayIonization(ESI)isthetechniqueofchoiceforon-linecouplingofliquidphase separations, which is particularly true for electromigrative techniques. However, the need for closing the electric circuits for both the CE and the ESI process at the end of the separation capillary requires unique interface designs. Moreover, the selectivity of electro- migrative techniques is substantially influenced by the type and concentration of the com- ponents ofthebackground electrolyte (BGE).ManyCEmethodsarenot compatiblewith ESI-MS in a direct fashion due to nonvolatile constituents, being required for best separa- tionperformance.ThesespecialneedsforCE-MSareaddressedinthisbook. In the first part the handling of modern interfaces is described in detail, including approaches based on (nano)sheath liquid (Chapters 1 and 2), porous tip (Chapter 3), and liquid junction CE-MS interfaces (Chapter 4). The development of novel and increasingly sophisticatedcapillarycoatingsisconsideredanimportantpartofCE-MSmethoddevelop- ment. In this regard, a protocol on an efficient coating for protein analysis is included (see Chapter5).CEtechnologyallowstheintegrationofshortsectionscontainingsolidmaterial (e.g., functionalized beads) for specific and efficient manipulation of analyte molecules. Therefore, one chapter was dedicated to utilizing an immobilized enzyme reactor imple- mented in the CE capillary for tryptic digestion of intact proteins and subsequent peptide v vi Preface level analysis (see Chapter 6). This chapter is followed by a CE-MS-dedicated protocol for the sample preparation and analysis of tryptic peptides (see Chapter 7). Intact protein characterization is another important field of CE-MS applications. In this context, top- down proteomics (TDP) gets increasing attention due to its capability to circumvent the inference problem in proteomics. A general TDP protocol for CE-MS can be found in Chapter 8. As a representative of the field of biotherapeutics the analysis of monoclonal antibodies,rangingfromreducedtointactlevel,issubsequentlydescribed(seeChapter9). ThecomplexityofglycoproteinscanbequitechallengingwithCE-MSbeinghighlysuited toseparateglycoforms.ACE-MSmethoddedicatedtobottom-upanalysisofglycoproteins is presented in Chapter 10. Another protocol is dedicated to the characterization of glycosaminoglycans, more specifically, the chondroitin sulfate and dermatan sulfate, which i.a. play an essential role at the extracellular matrix (see Chapter 11). Two protocols on metaboliteanalysisforcations(seeChapter12)andanions(seeChapter13)showthestellar powerofCE-MSinthisimportantfield.CEinelectrokineticchromatographymodeiswell suited for chiral analysis and described in detail for four different fields of application including pharmaceutical, biomedical, food, and agrochemical analysis (see Chapter 14). Traditionally, CE has been ruled out of many food safety applications, due to the lack of mandatory sensitivity. The inclusion of chromatography-based approaches for sample enrichmenthasbeenthemostsuccessful.Aprotocolutilizingin-linesolidphaseextraction for the detection of quinolone antibiotic residues in chicken meat is presented in Chapter15.AlesscommonsetupisthehyphenationofCEwithinductivelycoupledplasma massspectrometry(ICP-MS).Ithasbeendemonstrated thatthiscombinationisespecially suitableforthecharacterizationofmetalnanoparticles,beingitintraditionalICP-MSmode orevensingleparticle(sp)ICP-MS(seeChapter16). Overall,thisbookisdedicatedtohelpnormalizeCE-MSpracticesandprovideguidance coveringavarietyofdifferentfieldsofapplicationrangingfromsmallmoleculesuptolarge intact proteins. We hope to enhance the CE-MS community and supply a resource for production of reproducible and high-quality data. We thank all authors for their valuable contribution and their patience in the editorial process. We would also like to thank the Methods in Molecular Biology series editor, John Walker, for his guidance and impelling motivationinpreparingthisvolume. Aalen,Baden-Wu¨rttemberg,Germany ChristianNeusu¨ß KevinJooß Contents Preface ..................................................................... v Contributors................................................................. ix 1 EvaluationofPrototypeCE-MSInterfaces................................. 1 SabrinaFerre´,JulienBoccard,SergeRudaz,andVı´ctorGonza´lez-Ruiz 2 CapillaryElectrophoresis–MassSpectrometry(CE-MS)by Sheath–FlowNanosprayInterfaceandItsUsein BiopharmaceuticalApplications........................................... 15 MeiHan,RichardSmith,andDanA.Rock 3 ProtocolforEtchingBare-FusedSilicaCapillariesforSheathless CapillaryElectrophoresis–MassSpectrometryCoupling ..................... 49 ClarisseGosset-Erard,Je´re´mieGiorgetti,MichaelBiacchi, Fre´de´ricAubriet,EmmanuelleLeize-Wagner, PatrickChaimbault,andYannis-NicolasFranc¸ois 4 MicrofabricatedLiquidJunctionCapillaryElectrophoresis–Mass SpectrometryInterface .................................................. 61 JanaKrenkovaandFrantisekForet 5 SuccessiveMultipleIonic-PolymerLayerCoatingsforIntact ProteinAnalysisbyCapillaryZoneElectrophoresis–MassSpectrometry: ApplicationtoHemoglobinAnalysis ...................................... 69 LiesaSalzer,AlexanderStolz,LauraDhellemmes,AlisaH¨ochsmann, LaurentLeclercq,Herve´Cottet,andChristianNeusu¨ß 6 On-lineImmobilizedEnzymeMicroreactorCapillaryZone Electrophoresis–MassSpectrometryforPeptideMapping.................... 77 RogerPero-Gascon,LauraPont,EstelaGime´nez, VictoriaSanz-Nebot,andFernandoBenavente 7 Bottom-UpAnalysisofProteinsbyPeptideMassFingerprinting withtCITP-CZE-ESI-TOFMSAfterTrypticDigest........................ 93 MariusSeglandHannoStutz 8 Top-DownProteomicsbyCapillaryZoneElectrophoresis-Tandem MassSpectrometryforLarge-ScaleCharacterizationofProteoforms inComplexSamples..................................................... 107 ElijahN.McCool,RacheleA.Lubeckyj,DaoyangChen, andLiangliangSun 9 AssessmentofMacro-andMicroheterogeneityofMonoclonal AntibodiesUsingCapillaryZoneElectrophoresisHyphenated withMassSpectrometry ................................................. 125 ChristophGst¨ottner,RobHaselberg,ManfredWuhrer, GovertW.Somsen,andElenaDomı´nguez-Vega 10 High-SensitivityGlycoproteomicAnalysisofBiological SamplesbyCZE-ESI-MS................................................ 143 W.WangandG.S.M.Lageveen-Kammeijer vii viii Contents 11 CapillaryZoneElectrophoresis–ElectrosprayIonizationTandem MassSpectrometryforTotalAnalysisofChondroitin/Dermatan SulfateOligosaccharides ................................................. 163 AlinaD.Zamfir 12 In-SourceFragmentationfor theIdentificationofCompounds byCE-ESI-TOFinHumanPlasma.L-ProlineasCaseStudy ................. 185 MaricruzMamani-Huanca,AnaGradillas, A´ngelesL(cid:1)opez-Gonza´lvez,andCoralBarbas 13 AssessingtheEnergyStatusofLowNumbersofMammalian CellsbyCapillaryElectrophoresis–MassSpectrometry....................... 203 WeiZhangandRawiRamautar 14 ApplicationsofCapillaryElectrophoresis-MassSpectrometry toChiralAnalysis ....................................................... 211 ElenaSa´nchez-L(cid:1)opezandMarı´aLuisaMarina 15 ImprovedSensitivitytoDetermineAntibioticResiduesin ChickenMeatbyIn-LineSolid-PhaseExtractionCoupled toCapillaryElectrophoresis–TandemMassSpectrometry.................... 227 FranciscoJ.LaraandA.M.Garcı´a-Campan˜a 16 CECoupledtoICP-MSandSingleParticleICP-MSfor NanoparticleAnalysis.................................................... 243 DaryaMozhayevaandCarstenEngelhard Index ...................................................................... 259 Contributors FRE´DE´RIC AUBRIET • LaboratoiredeChimieetPhysique-ApprocheMulti-e´chellesdesMilieux Complexes(LCP-A2MC),Universite´deLorraine,Metz,France CORALBARBAS • CentrodeMetabol(cid:1)omicayBioana´lisis(CEMBIO),FacultaddeFarmacia, UniversidadSanPablo-CEU,CEUUniversities,Urbanizaci(cid:1)onMonteprı´ncipe,Madrid, Spain FERNANDOBENAVENTE • DepartmentofChemicalEngineeringandAnalyticalChemistry, InstituteforResearchonNutritionandFoodSafety(INSAlUB),UniversityofBarcelona, Barcelona,Spain MICHAELBIACCHI • LaboratoiredeSpectrome´triedeMassedesInteractionsetdesSyste`mes (LSMIS),UMR7140(Unistra-CNRS),Universite´deStrasbourg,Strasbourg,France JULIENBOCCARD • InstituteofPharmaceuticalSciencesofWesternSwitzerland(ISPSO), UniversityofGeneva,Geneva,Switzerland;SchoolofPharmaceuticalSciences,University ofGeneva,Geneva,Switzerland;SwissCentreforAppliedHumanToxicology,Basel, Switzerland PATRICKCHAIMBAULT • LaboratoiredeChimieetPhysique-ApprocheMulti-e´chellesdes MilieuxComplexes(LCP-A2MC),Universite´deLorraine,Metz,France DAOYANGCHEN • DepartmentofChemistry,MichiganStateUniversity,EastLansing,MI, USA HERVE´ COTTET • InstitutdesBiomole´culesMaxMousseron,UMRCNRS,Universite´de Montpellier,Montpellier,France LAURADHELLEMMES • InstitutdesBiomole´culesMaxMousseron,UMRCNRS,Universite´de Montpellier,Montpellier,France ELENADOMI´NGUEZ-VEGA • Center forProteomicsandMetabolomics,LeidenUniversity MedicalCenter,Leiden,TheNetherlands CARSTENENGELHARD • DepartmentofChemistryandBiology,UniversityofSiegen,Siegen, Germany;ResearchCenterofMicro-andNanochemistryand(Bio)Technology,University ofSiegen,Siegen,Germany SABRINAFERRE´ • InstituteofPharmaceuticalSciencesofWesternSwitzerland(ISPSO), UniversityofGeneva,Geneva,Switzerland;SchoolofPharmaceuticalSciences,University ofGeneva,Geneva,Switzerland FRANTISEKFORET • InstituteofAnalyticalChemistryoftheCzechAcademyofSciences,Brno, CzechRepublic YANNIS-NICOLASFRANC¸OIS • LaboratoiredeSpectrome´triedeMassedesInteractionsetdes Syste`mes(LSMIS),UMR7140(Unistra-CNRS),Universite´deStrasbourg,Strasbourg, France A.M.GARCI´A-CAMPAN˜A • DepartmentofAnalyticalChemistry,FacultyofSciences, UniversityofGranada,Granada,Spain ESTELA GIME´NEZ • DepartmentofChemicalEngineeringandAnalyticalChemistry, InstituteforResearchonNutritionandFoodSafety(INSAlUB),UniversityofBarcelona, Barcelona,Spain JE´RE´MIEGIORGETTI • LaboratoiredeSpectrome´triedeMassedesInteractionsetdesSyste`mes (LSMIS),UMR7140(Unistra-CNRS),Universite´deStrasbourg,Strasbourg,France ix
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