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Updated: Jun 1, 2026

MALDI-ToF MS Method for the Characterization of Synthetic Polymers with Varying Dispersity and End Groups
Published on: October 3, 2025
Gel permeation chromatography coupled to fourier transform mass spectrometry for polymer characterization
D J Aaserud1, L Prokai, W J Simonsick
1DuPont Marshall R & D Laboratory, Philadelphia, Pennsylvania 19146, and Center for Drug Discovery, College of Pharmacy, University of Florida, Gainesville, Florida 32610.
Abstract:
We report an on-line coupling of gel permeation chromatography (GPC) to Fourier transform mass spectrometry (FTMS) using a modified commercial electrospray ionization (ESI) interface. Selected oligomer profiles for the sodiated (1+ through 5+ charge states) oligomer ions of a narrow-molecular-weight poly(methyl methacrylate) were generated and used for obtaining a calibration curve. Using the MS-generated calibration curve and the refractive index response for quantification, an accurate molecular weight distribution was calculated and showed an excellent agreement with the value specified by the supplier. GPC/ESI/FTMS also allowed for an unequivocal end-group determination and characterization of a secondary distribution due to the formation of cyclic reaction products. We analyzed a glycidyl methacrylate/butyl methacrylate copolymer with a broad molecular weight distribution, where fractionation and high resolving power were required for adequate characterization. Molecular weight distribution data showed the advantage of coupling high-resolution MS and GPC to overcome the difficulty of analyzing polydisperse polymers with MS alone.
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