Date of Award

5-2024

Document Type

Thesis

Degree Name

Master of Science (MS)

Department

Chemistry

Committee Chair/Advisor

Christopher D Chouinard

Committee Member

Kenneth Marcus

Committee Member

Sourav Saha

Abstract

One of the major problems facing analytical chemistry challenge is the isomers separation, due to their closely related molecular structures and physicochemical properties. Therefore, in this thesis, we have performed the separation of steroid isomers through the use of ion mobility mass spectrometry, using various chemical approaches. Ion mobility is an effective high-resolution separation techniques that utilizes the mobility of ions in the gas-phase environment. A useful tool for isomeric analysis due to the ability to separate different isomeric classes of steroids according to their varied collision cross-sections, which is achieved by taking advantage of differences in ion mobility.

Moreover, the derivatization reactions were employed to introduce distinctive functional structures to the steroid molecules, facilitating enhanced separation through ion mobility spectrometry. In this work, a range of derivatization techniques investigated in order to modify the structure, size and charge of steroid isomers and improve their resolution and detectability. These techniques include the use of “shift reagents” such as 1,1-carbonyldiimidazole, Girard’s Reagent P, dansyl chloride, and 4-(bromomethyl)benzenesulfonyl chloride.

To sum up, this thesis provides insight into the continued development and use of advanced techniques for the analysis of steroids, highlighting the role of ion mobility mass spectrometry and the advantage of derivatization reactions in the identification and separation of isomeric forms. The presented methodologies can be a great scientific interest to a large number of fields working with steroids and requiring accurate identification and quantification of isomeric forms, including but not limited to environmental monitoring and pharmaceutical, clinical, and forensic chemistry.

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