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Entwicklung Und Optimierung Einer Methode Zur Entwicklung und Optimierung einer Methode zur Charakterisierung un- bekannter Substanzen mittels Gas- chromatographie - ultra-hochauflö- sender Massenspektrometrie und chemischer Ionisierung unter Atmo- sphärendruck Kumulative Dissertation zur Erlangung des akademischen Grades doctor rerum naturalium (Dr. rer. nat.) der Mathematisch-Naturwissenschaftlichen Fakultät der Universität Rostock eingereicht von Theo Schwemer, geb. am 04.10.1983 in Rostock, https://doi.org/10.18453/rosdok_id00002681 Rostock, 30.11.2019 Die vorliegende Arbeit wurde in der Zeit von November 2012 bis Dezember 2016 am Institut für Chemie der Universität Rostock am Lehrstuhl für Analytische Chemie in der Arbeitsgruppe von Prof. Dr. Ralf Zimmermann angefertigt. Gutachter: Zweitgutachter Prof. Dr. Ralf Zimmermann Prof. Dr. Andreas Römpp Universität Rostock Universität Bayreuth 18059 Rostock 95326 Kulmbach Datum der Einreichung: 31.10.2019 Datum der Verteidigung: 28.01.2020 - III "Wenn man das Unmögliche ausgeschlossen hat, muss das, was übrig bleibt, die Wahrheit sein, so unwahrscheinlich sie auch klingen mag." The Adventure of the Beryl Coronet / Sherlock Holmes ARTHUR CONAN DOYLE - IV Erklärung Ich versichere hiermit an Eides statt, dass ich die vorliegende Arbeit selbstständig angefertigt und ohne fremde Hilfe verfasst habe. Dazu habe ich keine außer den von mir angegebenen Hilfsmitteln und Quellen verwendet und die den benutzten Werken inhaltlich und wörtlich entnommenen Stellen habe ich als solche kenntlich gemacht. Rostock, 30.11.2019 ………………………. Theo Schwemer - V Erklärung zur Abfassung der Manuskripte zur ku- mulativen Dissertation Folgende Manuskripte wurden von Theo Schwemer als Haupt- bzw. Co-Autor in wissen- schaftlichen Fachzeitschriften (peer-reviewed) publiziert. Sie stellen die Grundlage für die vorliegende kumulative Dissertation dar. Der Anteil von Theo Schwemer an den Arbeiten ist jeweils kurz dargestellt. 1. Theo Schwemer, Christopher P. Rüger, Martin Sklorz, and Ralf Zimmermann; Gas Chromatography coupled to atmospheric pressure chemical ionization FT-ICR mass spectrometry for improvement of data reliability; Analytical chemistry 87.24 (2015): 11957-11961. DOI: 10.1021/acs.analchem.5b02114 Theo Schwemer war für den Aufbau des Messgerätes und der Messmethode verantwortlich, plante und führte die Messungen aus. Er führte die Datenanalyse durch und schrieb das Manuskript. 2. Theo Schwemer, Thorsten Rössler, Björn Ahrens, Marion Schäffer, Alexandra Hassel- bach-Minor, Michael Pütz, Martin Sklorz, Thomas Gröger, Ralf Zimmermann, et al. "Characterization of a heroin manufacturing process based on acidic extracts by com- bining complementary information from two-dimensional gas chromatography and high resolution mass spectrometry.” Forensic Chemistry 4 (2017): 9-18. DOI: 10.1016/j.forc.2017.02.006 Theo Schwemer führte Messungen durch, übernahm einen Teil der Datenauswertung und arbeitete am Manuskript und Erstellung der Graphiken. 3. Theo Schwemer, Uwe Käfer, Christopher P. Rüger, Martin Sklorz, Ralf Zimmermann, Application of gas chromatography coupled to ultra-high resolution mass spectrometry for the analysis of bitumen aging Theo Schwemer plante und führte die Messungen aus. Er war für die Datenanalyse verant- wortlich und schrieb das Manuskript. 4. Christopher P. Rüger, Toni Miersch, Theo Schwemer, Martin Sklorz, and Ralf Zimmer- mann, "Hyphenation of thermal analysis to ultrahigh-resolution mass spectrometry (Fou- rier transform ion cyclotron resonance mass spectrometry) using atmospheric pressure - VI chemical ionization for studying composition and thermal degradation of complex mate- rials." Analytical chemistry 87.13 (2015): 6493-6499. DOI: 10.1021/acs.anal- chem.5b00785 Theo Schwemer führte einen Teil der Messungen und die Datenauswertung durch. 5. Rüger, Christopher P., Martin Sklorz, Theo Schwemer, Ralf Zimmermann, "Character- isation of ship diesel primary particulate matter at the molecular level by means of ultra- high-resolution mass spectrometry coupled to laser desorption ionisation—comparison of feed fuel, filter extracts and direct particle measurements." Analytical and bioanalytical chemistry 407.20 (2015): 5923-5937. DOI 10.1007/s00216-014-8408-1 Theo Schwemer führte einen Teil der Messungen und die Datenauswertung durch. 6. Oeder, Sebastian, et al. "Particulate matter from both heavy fuel oil and diesel fuel ship- ping emissions show strong biological effects on human lung cells at realistic and com- parable in vitro exposure conditions." PloS one 10.6 (2015): e0126536. DOI: 10.1371/journal.pone.0126536 Theo Schwemer führte einen Teil der Messungen und die Datenauswertung durch. 7. Streibel, Thorsten, et al. "Aerosol emissions of a ship diesel engine operated with diesel fuel or heavy fuel oil." Environmental Science and Pollution Research 24.12 (2017): 10976-10991. DOI 10.1007/s11356-016-6724-z Theo Schwemer führte einen Teil der Messungen und die Datenauswertung durch. 8. Rüger, Christopher P., Theo Schwemer, Martin Sklorz, Peter B O’Connor, Mark P Bar- row and Ralf Zimmermann, "Comprehensive chemical comparison of fuel composition and aerosol particles emitted from a ship diesel engine by gas chromatography atmos- pheric pressure chemical ionisation ultra-high resolution mass spectrometry with im- proved data processing routines." European Journal of Mass Spectrometry 23.1 (2017): 28-39. DOI: 10.1177/1469066717694286 Theo Schwemer führte einen Teil der Messungen und die Datenauswertung durch. - VII Danksagung Besonders möchte ich mich bei Herrn Prof. Dr. R. Zimmermann dafür bedanken, dass ich in dieser Arbeitsgruppe die Möglichkeit bekommen habe, meine Dissertation anfertigen zu dür- fen. Durch die freundliche und engagierte Betreuung, durch Dr. M. Sklorz und Dr. T. Streibel, hat mir diese Arbeit viel Freude bereitet. Sie standen mir jederzeit mit Rat und Tat zur Seite. Danken möchte ich der gesamten Arbeitsgruppe, die mir jederzeit bei Fragen hilfreich zur Seite stand. Im Besonderen möchte ich Christopher Rüger danken, der mich während mei- ner Promotion immer unterstützt hat und bei Fragen und Problemen hilfreich zur Seite stand. Auch meiner langjährigen Kommilitonin Sabrina Radischat möchte ich meinen Dank aus- sprechen. Sie war mir immer eine verlässliche Praktikumspartnerin und Freundin. Ich danke außerdem meinen Eltern und meiner gesamten Familie, die mich in allen Lebens- lagen unterstützen. Nicht zuletzt gilt ein besonderer Dank meiner Frau Karoline und meinen Kindern. Sie geben mir stetig Kraft, unterstützen mich und spornen mich an, stets mein Bestes zu geben. Ihr habt immer an mich geglaubt und ohne euch wäre mein Leben um vieles ärmer. - VIII Zusammenfassung Die Charakterisierung von hochkomplexen Probengemischen aus mehreren tausenden Substanzen stellt eine Herausforderung für die analytische Chemie dar und bedarf leistungs- fähiger Techniken. Die Massenspektrometrie, insbesondere die hochauflösende Massen- spektrometrie, ist eine Methode, die schon in vielen Forschungsgebieten einen substanziel- len Beitrag zur Beschreibung komplizierter Gemische auf molekularer Ebene geleistet hat. Trotz einfacherer und schnellerer Probenaufgabe ohne weiteres Kopplungssystem, birgt die Verwendung einer chromatographischen Trennung als Einlasssystem für das Massenspek- trometer einige Vorteile für die Separierung und Identifizierung von unbekannten Substan- zen. Zum einen ermöglicht die Gaschromatographie die Auftrennung isomerer Verbindun- gen, zum anderen den Vergleich der Elutionszeiten und anderer Molekülinformationen mit Datenbanken. Daher wurde zunächst eine Kopplung aus ultra-hochauflösendem Massen- spektrometer (Fourier Tranformation Ionen Zyklotron Resonanz Massenspektrometer) und Gaschromatograph entwickelt. Im Anschluss musste sowohl eine funktionierende Methode entwickelt, getestet und evaluiert werden. Da existierende Programme bei der Datenaus- wertung nur unzureichend oder gar nicht mit den kombinierten chromatographischen und hoch aufgelösten Massenspektren zurechtkamen, wurde eine Methode entwickelt, die es ermöglicht, verschiedene existierende Ansätze gewinnbringend zu kombinieren. Dabei fiel auf, dass das Evaluieren der Daten ein entscheidender und zeitaufwendiger Faktor ist. Da- her wurde im Rahmen der Verbesserung der Datenauswertung, eine automatisierte Me- thode zur -evaluierung entwickelt. Zum Testen des Systems, einschließlich der entwickelten Datenauswertung, wurden verschiedene komplexe Proben, z.B. Diesel, Schweröl, Bitumen, Verbrennungsaerosole und Drogenmischungen untersucht. Dadurch konnte gezeigt wer- den, dass die Methode die ausgewählten Proben auf molekularer Ebene adäquat beschrei- ben und bei fragmentierungsarmer Ionisierung gleichzeitig ein weites Spektrum an Substan- zen ionisieren kann. Zusätzlich vermag die Kopplung isobare und isomere Verbindungen aus komplexen Gemischen voneinander zu trennen und diese sogar teilweise zu identifizie- ren, was die Charakterisierung der Proben verbessert. - IX Summary The analysis of complex samples with thousands of compounds is an analytical challenge that needed powerful techniques. Mass spectrometry and especially high-resolution mass spectrometry meets that requirements and contributed to the characterization of samples on a molecular level on many research areas. Despite of a more simple and faster sample in- jection, the hyphenation of a mass spectrometer to chromatographic techniques has some advantages for the separation and identification of unknown substances, for instance the separation of isomeric species or the match of elution
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