Date Approved
4-4-2025
Embargo Period
4-7-2027
Document Type
Thesis
Degree Name
Master of Science (M.S.)
Department
Chemistry and Biochemistry
College
College of Science & Mathematics
Advisor
James Grinias, Ph.D.
Committee Member 1
Subash Jonnalagadda, Ph.D.
Committee Member 2
Lark J. Perez, Ph.D.
Keywords
Chemical derivatization;Metabolomics;Method development;Organic acids;Supercritical fluid chromatography
Disciplines
Chemistry | Physical Sciences and Mathematics
Abstract
Organic acid analysis in complex mixtures by LC-MS has been difficult, due in large part to the poor sensitivity of the negative ionization mode needed to detect these native (i.e., underivatized or untagged) compounds. Similar negative ionization-based restrictions have also made it challenging to quantify such compounds using supercritical fluid chromatography (SFC)-MS, a technique that has become more important for metabolomic analysis. In this study, the use of a high proton affinity N-(4-aminophenyl)piperidine derivatization tag was investigated to enhance four organic acids’ (lactic, succinic, malic, and citric acids) detection with varying numbers of carboxylate groups. Upon derivatization with N-(4-aminophenyl)piperidine, detection limits were achieved down to 0.5 ppb, with overall improvements in detection limit ranging from 25- to 2100-fold. The impact of derivatization towards sensitivity, which increased by 200-fold for compounds that were detectable in their native forms, and mass spectrometric detection were also discussed. Preliminary column comparison and modifier effects were further investigated to identify the stationary phase and modifier most suitable for the separation of these four derivatized compounds by SFC. Thus, these results effectively demonstrate the capability of the derivatization technique in improving analysis of organic acids by SFC-MS, particularly for those that are undetectable in their native forms.
Recommended Citation
Saw, Yih Ling, "THE USE OF N-(4-AMINOPHENYL)PIPERIDINE DERIVATIZATION TO IMPROVE ORGANIC ACID DETECTION AND SEPARATION BY SUPERCRITICAL FLUID CHROMATOGRAPHY-MASS SPECTROMETRY" (2025). Theses and Dissertations. 3342.
https://rdw.rowan.edu/etd/3342
