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A Thesis Entitled Detection of Oxidized Lipids by Laser A Thesis Entitled Detection of Oxidized Lipids by Laser Desorption Ionization Time of Flight Mass Spectrometry Using Hydrazine Containing Reagents By Mohammed Abdullah A Alyami Submitted to the Graduate Faculty as partial fulfillment of the requirements for the Master of Science Degree in Pharmaceutical Sciences _________________________________________ Dr. Hermann von Grafenstein, Committee Chair _________________________________________ Dr. Youssef Sari, Committee Member _________________________________________ Dr. Zahoor Shah, Committee Member _________________________________________ Dr. Amanda Bryant-Friedrich, Dean College of Graduate Studies The University of Toledo May-2018 Copyright 2018, Mohammed Abdullah A Alyami This document is copyrighted material. Under copyright law, no parts of this document may be reproduced without the expressed permission of the author. An Abstract of Detection of Oxidized Lipids by Laser Desorption Ionization Time of Flight Mass Spectrometry Using Hydrazine Containing Reagents By Mohammed Abdullah A Alyami Submitted to the Graduate Faculty as partial fulfillment of the requirements for the Master of Science Degree in Pharmaceutical Sciences The University of Toledo May-2018 Since matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) was established, it has been advanced as an analytical technique to detect and identify a large range of molecules. Lipids have been analyzed intensively by MALDI-TOF MS for several years. Because lipids are essential components of the body, any change in their structures can produce dramatic effects, either beneficial or detrimental. Oxidation of phospholipids is one of these types of changes. In the brain, it is found that formation of amyloid fibrils has a strong relationship to production of oxidized phospholipids (OxPLs) such as 1-palmitoyl-2-(9-oxo-nonanoyl)-sn-Glycero-3- phosphocholine (PoxnoPC). Due to addition of an aldehyde group in oxidized lipids, it may be possible to selectivity detect them by using fluorescent reagents containing a hydrazine functional group which was the ability to react with the carbonyl group. In the context of the MALDI-TOF MS analysis technique, 2,4-dinitrophenylhydrazine (DNPH) has been used as a reactive matrix holding the promise that this might allow selective detection oxidized lipids among un-oxidized lipids. However, in these studies unreacted excess DNPH was never removed, preventing definitive conclusions to be made as iii regarding the role of DNPH as a fluorescent tag as opposed to functioning as a matrix. Oxidized phosphatidylcholine is derivatized at its carbonyl group with DNPH to form 2,4-dinitrophenylhydrazone (DNPhydrazone). To evaluate the “reactive matrix” concept implying that DNPhydrazone might be used as a selective detection of the analyte, we removed an excess amount of unreacted DNPH by using glyoxylic acid (GA) and added back different concentrations of DNPH. We found that the signal of DNPhydrazone was directly proportional to the DNPH concentration. Moreover, signals for both 1,2- dipalmitoyl-sn-glycero-3-phosphocholine (DPPC) mixed with DNPH were detected. DNPH functioned as a non-reactive matrix molecule as well as an analyte tag, although DNPhydrazone demonstrated a higher signal than DPPC in all experiments. Utilizing DNPH as a matrix molecule, we examined the difference of laser power required for compared with 2,5-dihydroxybenzoic acid (DHB). In the presence of DNPH, our results showed that DPPC needed lower laser intensity to be recorded. In contrast, DHB required more energy for detection of DPPC. Interestingly, we observed that a complex mixture of lipids influenced the DNPhydrazone and DPPC signals significantly. Further experiments showed that although DNPH did not allow matrix-free detection of oxidized lipids and was not selective in positive ion mode, selective detection of oxidized lipids is possible in negative ion mode. Here, DNPH appears to act as a charge-tagging reagent, adding a negative charge to the hydrazine moiety of DNPH. iv Acknowledgements I believe that words are not always enough to thank and appreciate Dr. Grafenstein. Albeit he has much knowledge, he accepted and welcomed all my objections and debating. In fact, we worked as a team listening to each other's ideas, respectively, so it was more than a professor and student relationship. I am proud that I was one of his students. I would like to thank Kirschbaum and Hanson for all of the support that helped me to finish my thesis. Dr. Kirschbaum fought for all students to have a new instrument, which gave all of us hope to complete our experiments. Dr. Hanson never has hesitated to help me and answered all my questions. I appreciate that Dr. Sari and Shah accepted to be members of the committee. They gave helpful comments that I am sure will help me in my future research. Finally, without doubt, I would not be at this level of education and career success career without support from my mother and wife. v Table of Contents Abstract .............................................................................................................................. iii Acknowledgements ..............................................................................................................v Table of Contents ............................................................................................................... vi List of Figures .................................................................................................................. viii List of Abbreviations ...........................................................................................................x 1. Introduction…….. .........................................................................................................1 1.1 Overview ……………………………………………………………………………1 1.2 MALDI ……………………………………………………………………………..2 1.2.1 Ionization Zone ………………………………………………….....................3 1.2.1.1 Hard ionization ……………………………………………………………3 1.2.1.2 Soft ionization …………………………………………………………….4 1.2.1.3 Matrices……………………………………………………………….…..5 1.2.2 Acceleration and flight zone…………………………………………….….…8 1.2.3 Detectors……………………………………………………………….……...8 1.3 Derivatized oxidized lipids ……...………………………………………………...10 1.3.1 Lipid ………………………………………………………………….……...10 1.3.2 DNPH …………………………………………………………………..……11 2. Materials and Method……………………………………………….…………….…12 2.1 Chemicals……………………………………………………...……………...…..12 vi 2.2 Preparations……………………………...……………………………..………....12 2.2.1 Phospholipids…………………………………………………………..…….12 2.2.2 Extracted lipid……………………………………………………………..…13 2.3 MALDI-TOF……………………………………………………………………...13 3. Results and Discussion ……………………………………………………………...14 3.1 Importance of additional amount of DNPH to work as a matrix………………....15 3.2 Comparison DNPH to DHB in consumed laser power………………………...…20 3.3 Effect of the lipid mixture on improving the signal of DNPhydrazone and DPPC…………………………………………………………………………......21 3.4 The possibility of selected oxidized lipids when utilizing DNPhydrazone as a charge tag…………………………………………………………………………23 4. Conclusions…………………………………………………………………………. 24 References ..........................................................................................................................26 Appendix ...………………………………………………………………………………29 vii List of Figures 1-1 MALDI-TOF zones .................................................................................................3 1-2 Hard ionization mechanism .....................................................................................4 1-3 Chemical structure of 2,5-DHB ...............................................................................7 1-4 Chemical structures of PoxnoPC and DNPH.........................................................10 3-1 The mechanism for reaction between DNPH and PoxnoPC .................................15 3-2 Positive ion mode MALDI-TOF of PoxnoPC and DNPhydrazone .......................15 3-3 Peak intensity average of DNPhydrazone in different DNPH concentrations ......16 3-4 Positive ion mode MALDI-TOF spectra of DNPhydrazone ................................17 3-5 Scheme representation steps to remove non-react DNPH ....................................18 3-6 Mass spectra of aqueous and organic phases after adding with GA ......................18 3-7 The mechanism for reaction between DNPH and GA ...........................................18 3-8 Peak intensity average of DPPC and DNPhydrazone after adding GA .................19 3-9 Peak intensity average of DPPC and DNPhydrazone in the separate experiment .19 3-10 Positive ion mode MALDI-TOF spectrum of DPPC mixed with 50mM DNPH ..19 3-11 Different laser power levels needed to detect DPPC ............................................20 3-12 Positive ion mode spectrum of DPPC mixed with different components ...........20 3-13 Effect of the lipid mixture on the signal of the DNPhydrazone ...........................21 3-14 Effect of the lipid mixture on the signal of the DPPC ...........................................22 viii 3-15 MALDI spectra of DPPC and DNPhydrazone in the lipid mixture.......................22 3-16 Negative charge formed in hydrazone moiety after removing H+ ………………23 3-17 Negative ion MALDI-TOF mass spectrum of DNPhydrazone………………….24 3-18 Negative ion MALDI-TOF mass spectrum of DPPC……………………………24 ix List of Abbreviations amu ……………………atomic mass units COX……………………Cyclooxygenases DHB…………………...2,5-Dihydroxybenzoic acid DNPH………………….2,4-dinitrophenylhydrazine DNPhydrazone………...2,4-dinitrophenylhydrazone
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