000276619 001__ 276619 000276619 005__ 20220930130052.0 000276619 0247_ $$2doi$$a10.1371/journal.pone.0139710 000276619 0247_ $$2Handle$$a2128/9540 000276619 0247_ $$2WOS$$aWOS:000362499200055 000276619 0247_ $$2altmetric$$aaltmetric:4589786 000276619 0247_ $$2pmid$$apmid:26436664 000276619 037__ $$aFZJ-2015-06964 000276619 082__ $$a500 000276619 1001_ $$0P:(DE-Juel1)145961$$aDammers, Christina$$b0$$ufzj 000276619 245__ $$aPurification and Characterization of Recombinant N-Terminally Pyroglutamate-Modified Amyloid-β Variants and Structural Analysis by Solution NMR Spectroscopy 000276619 260__ $$aLawrence, Kan.$$bPLoS$$c2015 000276619 3367_ $$0PUB:(DE-HGF)16$$2PUB:(DE-HGF)$$aJournal Article$$bjournal$$mjournal$$s1449666803_32505 000276619 3367_ $$2DataCite$$aOutput Types/Journal article 000276619 3367_ $$00$$2EndNote$$aJournal Article 000276619 3367_ $$2BibTeX$$aARTICLE 000276619 3367_ $$2ORCID$$aJOURNAL_ARTICLE 000276619 3367_ $$2DRIVER$$aarticle 000276619 520__ $$aAlzheimer’s disease (AD) is the leading cause of dementia in the elderly and is characterized by memory loss and cognitive decline. Pathological hallmark of AD brains are intracellular neurofibrillary tangles and extracellular amyloid plaques. The major component of these plaques is the highly heterogeneous amyloid-β (Aβ) peptide, varying in length and modification. In recent years pyroglutamate-modified amyloid-β (pEAβ) peptides have increasingly moved into the focus since they have been described to be the predominant species of all N-terminally truncated Aβ. Compared to unmodified Aβ, pEAβ is known to show increased hydrophobicity, higher toxicity, faster aggregation and β-sheet stabilization and is more resistant to degradation. Nuclear magnetic resonance (NMR) spectroscopy is a particularly powerful method to investigate the conformations of pEAβ isoforms in solution and to study peptide/ligand interactions for drug development. However, biophysical characterization of pEAβ and comparison to its non-modified variant has so far been seriously hampered by the lack of highly pure recombinant and isotope-enriched protein. Here we present, to our knowledge, for the first time a reproducible protocol for the production of pEAβ from a recombinant precursor expressed in E. coli in natural isotope abundance as well as in uniformly [U-15N]- or [U-13C, 15N]-labeled form, with yields of up to 15 mg/l E. coli culture broth. The chemical state of the purified protein was evaluated by RP-HPLC and formation of pyroglutamate was verified by mass spectroscopy. The recombinant pyroglutamate-modified Aβ peptides showed characteristic sigmoidal aggregation kinetics as monitored by thioflavin-T assays. The quality and quantity of produced pEAβ40 and pEAβ42 allowed us to perform heteronuclear multidimensional NMR spectroscopy in solution and to sequence-specifically assign the backbone resonances under near-physiological conditions. Our results suggest that the presented method will be useful in obtaining cost-effective high-quality recombinant pEAβ40 and pEAβ42 for further physiological and biochemical studies. 000276619 536__ $$0G:(DE-HGF)POF3-553$$a553 - Physical Basis of Diseases (POF3-553)$$cPOF3-553$$fPOF III$$x0 000276619 588__ $$aDataset connected to CrossRef 000276619 7001_ $$0P:(DE-Juel1)145165$$aGremer, Lothar$$b1$$ufzj 000276619 7001_ $$0P:(DE-Juel1)144510$$aNeudecker, Philipp$$b2$$ufzj 000276619 7001_ $$0P:(DE-HGF)0$$aDemuth, Hans-Ulrich$$b3 000276619 7001_ $$0P:(DE-Juel1)132019$$aSchwarten, Melanie$$b4$$ufzj 000276619 7001_ $$0P:(DE-Juel1)132029$$aWillbold, Dieter$$b5$$eCorresponding author$$ufzj 000276619 773__ $$0PERI:(DE-600)2267670-3$$a10.1371/journal.pone.0139710$$gVol. 10, no. 10, p. e0139710 -$$n10$$pe0139710$$tPLoS one$$v10$$x1932-6203$$y2015 000276619 8564_ $$uhttps://juser.fz-juelich.de/record/276619/files/Purification%20and%20Characterization%20of%20Recombinant%20N-Terminally%20Pyroglutamate-Modified%20Amyloid-%CE%B2%20Variants%20and%20Structural%20Analysis%20by%20Solution%20NMR%20Spectroscopy.pdf$$yOpenAccess 000276619 8564_ $$uhttps://juser.fz-juelich.de/record/276619/files/Purification%20and%20Characterization%20of%20Recombinant%20N-Terminally%20Pyroglutamate-Modified%20Amyloid-%CE%B2%20Variants%20and%20Structural%20Analysis%20by%20Solution%20NMR%20Spectroscopy.pdf?subformat=pdfa$$xpdfa$$yOpenAccess 000276619 8767_ $$92015-09-21$$d2015-09-23$$eAPC$$jZahlung erfolgt$$zUSD 1350,- 000276619 909CO $$ooai:juser.fz-juelich.de:276619$$popenCost$$pVDB$$pdriver$$pOpenAPC$$popen_access$$popenaire$$pdnbdelivery 000276619 9101_ $$0I:(DE-588b)5008462-8$$6P:(DE-Juel1)145961$$aForschungszentrum Jülich GmbH$$b0$$kFZJ 000276619 9101_ $$0I:(DE-588b)5008462-8$$6P:(DE-Juel1)145165$$aForschungszentrum Jülich GmbH$$b1$$kFZJ 000276619 9101_ $$0I:(DE-588b)5008462-8$$6P:(DE-Juel1)144510$$aForschungszentrum Jülich GmbH$$b2$$kFZJ 000276619 9101_ $$0I:(DE-588b)5008462-8$$6P:(DE-Juel1)132019$$aForschungszentrum Jülich GmbH$$b4$$kFZJ 000276619 9101_ $$0I:(DE-588b)5008462-8$$6P:(DE-Juel1)132029$$aForschungszentrum Jülich GmbH$$b5$$kFZJ 000276619 9131_ $$0G:(DE-HGF)POF3-553$$1G:(DE-HGF)POF3-550$$2G:(DE-HGF)POF3-500$$3G:(DE-HGF)POF3$$4G:(DE-HGF)POF$$aDE-HGF$$bKey Technologies$$lBioSoft – Fundamentals for future Technologies in the fields of Soft Matter and Life Sciences$$vPhysical Basis of Diseases$$x0 000276619 9141_ $$y2015 000276619 915__ $$0StatID:(DE-HGF)0200$$2StatID$$aDBCoverage$$bSCOPUS 000276619 915__ $$0StatID:(DE-HGF)1050$$2StatID$$aDBCoverage$$bBIOSIS Previews 000276619 915__ $$0LIC:(DE-HGF)CCBY4$$2HGFVOC$$aCreative Commons Attribution CC BY 4.0 000276619 915__ $$0StatID:(DE-HGF)1040$$2StatID$$aDBCoverage$$bZoological Record 000276619 915__ $$0StatID:(DE-HGF)0100$$2StatID$$aJCR$$bPLOS ONE : 2014 000276619 915__ $$0StatID:(DE-HGF)0500$$2StatID$$aDBCoverage$$bDOAJ 000276619 915__ $$0StatID:(DE-HGF)0111$$2StatID$$aWoS$$bScience Citation Index Expanded 000276619 915__ $$0StatID:(DE-HGF)0150$$2StatID$$aDBCoverage$$bWeb of Science Core Collection 000276619 915__ $$0StatID:(DE-HGF)9900$$2StatID$$aIF < 5 000276619 915__ $$0StatID:(DE-HGF)0510$$2StatID$$aOpenAccess 000276619 915__ $$0StatID:(DE-HGF)0310$$2StatID$$aDBCoverage$$bNCBI Molecular Biology Database 000276619 915__ $$0StatID:(DE-HGF)0300$$2StatID$$aDBCoverage$$bMedline 000276619 915__ $$0StatID:(DE-HGF)0199$$2StatID$$aDBCoverage$$bThomson Reuters Master Journal List 000276619 920__ $$lyes 000276619 9201_ $$0I:(DE-Juel1)ICS-6-20110106$$kICS-6$$lStrukturbiochemie $$x0 000276619 9801_ $$aUNRESTRICTED 000276619 9801_ $$aFullTexts 000276619 980__ $$ajournal 000276619 980__ $$aVDB 000276619 980__ $$aUNRESTRICTED 000276619 980__ $$aI:(DE-Juel1)ICS-6-20110106 000276619 980__ $$aAPC 000276619 981__ $$aI:(DE-Juel1)IBI-7-20200312