Time‐of‐Flight Mass Spectrometry for Polymer Characterization

Li, Liang; Whittal, Randy M.

doi:10.1002/9780470567234.ch3

Cited by 4 publications

(5 citation statements)

References 67 publications

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“…The m / z scale was calibrated externally using polystyrene or poly(methyl methacrylate) standards at the molecular weight of interest. Under these conditions, the mass accuracy for polymer analysis is <100 ppm, and our errors fall within this range (all within ∼50 ppm, cf. Figures and and Supporting Information Table S1).…”

Section: Methodssupporting

confidence: 65%

Sequence Analysis of Styrenic Copolymers by Tandem Mass Spectrometry

et al. 2014

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Styrene and smaller molar amounts of either m-dimethylsilylstyrene (m-DMSS) or p-dimethylsilylstyrene (p-DMSS) were copolymerized under living anionic polymerization conditions, and the compositions, architectures, and sequences of the resulting copolymers were characterized by matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and tandem mass spectrometry (MS(2)). MS analysis revealed that linear copolymer chains containing phenyl-Si(CH3)2H pendants were the major product for both DMSS comonomers. In addition, two-armed architectures with phenyl-Si(CH3)2-benzyl branches were detected as minor products. The comonomer sequence in the linear chains was established by MS(2) experiments on lithiated oligomers, based on the DMSS content of fragments generated by backbone C-C bond scissions and with the help of reference MS(2) spectra obtained from a polystyrene homopolymer and polystyrene end-capped with a p-DMSS block. The MS(2) data provided conclusive evidence that copolymerization of styrene/DMSS mixtures leads to chains with a rather random distribution of the silylated comonomer when m-DMSS is used, but to chains with tapered block structures, with the silylated units near the initiator, when p-DMSS is used. Hence, MS(2) fragmentation patterns permit not only differentiation of the sequences generated in the synthesis, but also the determination of specific comonomer locations along the polymer chain.

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Section: Methodssupporting

confidence: 65%

Sequence Analysis of Styrenic Copolymers by Tandem Mass Spectrometry

et al. 2014

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“…Due to the developed technologies and analytical strategies, MALDI-TOF MS has become a normal analytical method for the analysis of synthetic polymers, supplying complete structural information with high sensitivity [17,21]. It has been fruitfully utilized in both characterization and degradation investigations.…”

Section: Maldi Tandem Mass Spectrometry Studiesmentioning

confidence: 99%

“…More recently, several studies have been focused on DDS and pharmacokinetics by MS/MS, thanks to the technological progress and combining ESI with separation techniques. Overall, MS has been more extensively employed in the analyses of biodegradable polymers [14][15][16]19,21,23,25,28,[31][32][33][34][35][36][37]44,128] than tandem MS [38][39][40][41][42][43]45], even if MS/MS is highly informative. This should be reasonably due to the time-consuming step related to the data processing and interpretation in MS/MS [14,15,19,28,39,42], even though tandem MS analysis has provided valuable information on biodegradable polymer architectures, end-group functionalities, bond connectivity, copolymer sequences, etc.…”

Section: Introductionmentioning

confidence: 99%

Matrix-Assisted Laser Desorption and Electrospray Ionization Tandem Mass Spectrometry of Microbial and Synthetic Biodegradable Polymers

Rizzarelli

Rapisarda

2023

Polymers

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The in-depth structural and compositional investigation of biodegradable polymeric materials, neat or partly degraded, is crucial for their successful applications. Obviously, an exhaustive structural analysis of all synthetic macromolecules is essential in polymer chemistry to confirm the accomplishment of a preparation procedure, identify degradation products originating from side reactions, and monitor chemical–physical properties. Advanced mass spectrometry (MS) techniques have been increasingly applied in biodegradable polymer studies with a relevant role in their further development, valuation, and extension of application fields. However, single-stage MS is not always sufficient to identify unambiguously the polymer structure. Thus, tandem mass spectrometry (MS/MS) has more recently been employed for detailed structure characterization and in degradation and drug release monitoring of polymeric samples, among which are biodegradable polymers. This review aims to run through the investigations carried out by the soft ionization technique matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) and electrospray ionization mass spectrometry (ESI-MS) MS/MS in biodegradable polymers and present the resulting information.

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“…34 When pyrolysis is added to GC-MS (Py-GC-MS), the resulting method reveals not only the purity of the polymers but may also enable us to characterize the copolymers. [35][36][37] In turn, matrix-assisted laser desorption ionization-time-of-flight mass spectrometry (MALDI-TOF MS) 38,39 and size exclusion chromatography coupled with various detectors, 40,41 such as evaporative light-scattering detection (SEC-ELS) can be used to assess the molecular weight characteristics of polymers.…”

Section: Introductionmentioning

confidence: 99%