Thesis-1988-AbdGhani.pdf (2.04 MB)
Derivatisation of amines for electrochemical detection in HPLC
thesis
posted on 2018-05-23, 14:10 authored by Mohmad A. Abd-GhaniThree derivatising reagents have been studied as possible
pre-column derivatisation agents for aliphatic amines for reversed-phase
HPLC with electrochemical detection. O-acetylsalicyloyl chloride, N-succinimidyl-3-(4-hydroxyphenyl)propionate, and methyl
p-hydroxybenzimidate.HCl were examined. O-acetylsalicyloyl chloride
was shown to be a suitable derivatising reagent. Firstly, pure
amine derivatives were prepared using the Schotten-Baumann reaction
conditions and the structure of the compounds were confirmed by
melting point, IR and NMR spectroscopy, and TLC analysis.
Analyses were carried out on an ODS-Hypersil column using as
mobile phase 50:50 methanol-0.025 M phosphate buffer pH 8 and the
derivatives were detected at a glassy carbon electrode set at +0.9 V
vs Ag/AgCl. Results for all amine derivatives have indicated the
suitability of LCEC detection method with good linearity, precision
and sensitivity. Then the amine derivatisation was applied to
in situ determination of amines in dilute aqueous solution to
give 100% yield, and a linear response down to 10-6 M
concentration level. Amine derivatives obtained from
N-succinimidyl-3-(4-hydroxyphenyl)propionate and methyl p-hydroxybenzimidate.HCl can also be detected by LCEC but problems were
observed with these reagents.
Funding
Malaysia, Public Services Department.
History
School
- Science
Department
- Chemistry
Publisher
© M.A. Abd GhaniPublisher statement
This work is made available according to the conditions of the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International (CC BY-NC-ND 4.0) licence. Full details of this licence are available at: https://creativecommons.org/licenses/by-nc-nd/4.0/Publication date
1988Notes
A Master's Thesis. Submitted in partial fulfilment of the requirements for the award of Master of Philosophy at Loughborough University.Language
- en