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Determination of ω -end functionalities in tailored poly(2-alkyl-2-oxazoline)s by liquid chromatography and mass spectrometry.

Determination of ω -end functionalities in tailored poly(2-alkyl-2-oxazoline)s by liquid chromatography and mass spectrometry.

Authors :
Engel N
Dirauf M
Czaplewska JA
Nischang I
Gottschaldt M
Schubert US
Source :
Royal Society open science [R Soc Open Sci] 2024 Feb 07; Vol. 11 (2), pp. 231008. Date of Electronic Publication: 2024 Feb 07 (Print Publication: 2024).
Publication Year :
2024

Abstract

The in-depth analytical characterization of polymers, in particular regarding intended biomedical applications, is becoming increasingly important to elucidate their structure-property relationships. Specifically, end group analysis of e.g. polymers featuring a 'stealth effect' towards the immune system is of particular importance because of their use in coupling reactions to bioactive compounds. Herein, we established a liquid chromatography (LC) protocol to analyse bicyclo[6.1.0]nonyne-functionalized poly(2-alkyl-2-oxazoline)s (POx)s as promising functional polymers that can be applied in strain-promoted click reactions. This work involved the synthesis of poly(2-methyl-2-oxazoline) (PMeOx) and poly(2-ethyl-2-oxazoline) (PEtOx) by living cationic ring-opening polymerization (CROP) with different molar masses ranging from 2 up to 17.5 kDa and, to our knowledge, the first liquid chromatographic analysis of PMeOx. The developed analytical protocol enables the quantitative determination of post-polymerization reaction sequences with respect to the conversion of the ω -end groups. All synthesized polymers were straightforwardly analysed on a C18-derivatized silica monolithic column under reversed-phase chromatographic conditions with a binary mobile phase gradient comprising a mixture of acetonitrile and water. Subsequent mass spectrometry of collected elution fractions enabled the confirmation of the desired ω -end group functionalities and the identification of synthetic by-products.<br />Competing Interests: We declare we have no competing interests.<br /> (© 2024 The Authors.)

Details

Language :
English
ISSN :
2054-5703
Volume :
11
Issue :
2
Database :
MEDLINE
Journal :
Royal Society open science
Publication Type :
Academic Journal
Accession number :
38328565
Full Text :
https://doi.org/10.1098/rsos.231008