Advancing Quantitative ³¹P NMR Spectroscopy for Reliable Thiol Group Analysis.

ABSTRACT: Accurate thiol quantification is essential for advancing thiol-X-ligation strategies in polymer and materials synthesis. Conventional assays, most notably Ellman's test, are limited in scope, particularly for hydrophobic or multifunctional thiols. Here, we introduce a straightforward and broadly applicable ³¹P NMR spectroscopy method for thiol quantification, using 2-chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane (TMDP) as a phosphitylation reagent. The approach extends established ³¹P NMR protocols for hydroxyl and carboxyl group analysis to thiols, offering high specificity and stability in readout. The method demonstrates applicability across a wide range of substrates, from small organic molecules to polymeric multi thiols with M_n up to 8000 g

SUBMITTER: Walter K 

PROVIDER: S-EPMC12825386 | biostudies-literature | 2026 Jan

REPOSITORIES: biostudies-literature