Open AccessSolid-state NMR spectroscopy as a tool supporting optimization of MALDI-TOF MS analysis of polylactides
Author(s) -
Anna Sroka-Bartnicka,
Sebastian Olejniczak,
Marek Sochacki,
Tadeusz Biela,
Marek J. Potrzebowski
Publication year - 2009
Publication title -
journal of the american society for mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.961
H-Index - 127
eISSN - 1879-1123
pISSN - 1044-0305
DOI - 10.1016/j.jasms.2008.09.013
Subject(s) - chemistry , crystallinity , magic angle spinning , nuclear magnetic resonance spectroscopy , polymer , solid state nuclear magnetic resonance , benzoic acid , desorption , matrix assisted laser desorption/ionization , spectroscopy , polymer chemistry , analytical chemistry (journal) , crystallography , organic chemistry , nuclear magnetic resonance , physics , adsorption , quantum mechanics
We report systematic structural studies of poly(l-lactide) (PLLA) employing matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) and solid-state NMR spectroscopy. (13)C cross polarization magic angle spinning (CP/MAS) NMR data for 1,8-dihydroxy-9-anthracenone (DT), 2,5-dihydroxybenzoic acid (DHB), 2-(4-hydroxyphenylazo)-benzoic acid (HABA), and trans-3-indoleacrylic acid (IAA), four matrices commonly used in MALDI-TOF analysis of polymers, were analyzed to test the influence of crystallization conditions (solvent, inorganic salt) on sample morphology. (13)C principal elements of chemical shift tensor (CST) and line-shape analyses were employed to study of the nature of hydrogen bonding and to evaluate the crystallinity and amorphicity of the pure polymer. NMR parameters for PLLA were compared with data for polylactide crystallized with the four matrices under different conditions with the addition of two inorganic salts as cationization agents. This study revealed that the semicrystalline structure of the polymer does not change when it is embedded in the matrix.