Data Processing Method for the Determination of Accurate Molecular Weight Distribution of Polymers by SEC/MALDI-MS

Sato, Hiroaki; Ichieda, Nobuyuki; Tao, Hiroaki; Ohtani, Hajime

doi:10.2116/analsci.20.1289

Cited by 24 publications

(11 citation statements)

References 25 publications

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“…[45] However, there has been some promising research at converting MALDI-MS into an accurate tool for molecular weight analysis. [51] An approach at determining band-broadening-free MWD from off-line SEC/MALDI-MS has also been proposed [52] and MALDI has been available now for some time as a molecular weight sensitive detector in SEC. [53] We have recently shown that using online electrospray ionization the individual strengths of both techniques -SEC with concentration detection and ESI-MS -can be successfully combined to derive very accurate MWD of synthetic polymers.…”

Section: Introductionmentioning

confidence: 99%

A Perfect Couple: PLP/SEC/ESI‐MS for the Accurate Determination of Propagation Rate Coefficients in Free Radical Polymerization

Gruendling

Voll

Guilhaus

et al. 2009

Macro Chemistry & Physics

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Pulsed laser polymerization (PLP) in conjunction with online size exclusion chromatography – electrospray ionization mass spectrometry (SEC/ESI‐MS) has successfully been applied for the determination of accurate propagation rate coefficients, kp, in free radical polymerization. SEC/ESI‐MS is used in this context to precisely determine the molecular weight distribution of the polymer produced by the PLP‐experiment. The novel approach allows for a highly accurate internal calibration of the size exclusion system to be obtained from first principles, as the molecular weight of the polymer is determined with ppm accuracy by the mass spectrometer and allows corrections for SEC band broadening effects to be made. Molecular weight measurements can furthermore be performed regardless of the monomer class, as long as the macromolecule is amenable to electrospray ionization. The proposed approach successfully eliminates work‐steps and problems incurred in the analysis of new and poorly characterized monomers, where universal calibration or multi‐detector SEC had to be applied until now and provides an alternative also to PLP/MALDI‐MS. Applicability of the method is demonstrated for the homologous series of methyl‐, ethyl‐ and butyl methacrylate. The experimentally determined kp values were 5–10% higher than the currently available benchmark data. The experimental kp is in agreement with the results of kinetic simulations, assuming a short chain length dependency of kp, in accordance with the empirical model of Smith, Heuts and Russell.magnified image

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Section: Introductionmentioning

confidence: 99%

A Perfect Couple: PLP/SEC/ESI‐MS for the Accurate Determination of Propagation Rate Coefficients in Free Radical Polymerization

Gruendling

Voll

Guilhaus

et al. 2009

Macro Chemistry & Physics

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“…19 The molecular weight distribution of synthetic polymers in MALDI MS can be described approximately by Gaussian distributions in their mass-to-charge ratios. [20][21][22][23][24][25] Because MALDI spectra of polyaddition adducts generally show approximate Gaussian distributions as shown in Fig. 2, the curve fitting method using Origin software was applied to the mass peak patterns obtained from each polymer series.…”

Section: Determining the Relative Contributions Of Polymer Series In mentioning

confidence: 99%

MALDI MS-based Composition Analysis of the Polymerization Reaction of Toluene Diisocyanate (TDI) and Ethylene Glycol (EG)

Ahn

Lee

Kim³

2015

ANAL. SCI.

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This study describes an MS-based analysis method for monitoring changes in polymer composition during the polyaddition polymerization reaction of toluene diisocyanate (TDI) and ethylene glycol (EG). The polymerization was monitored as a function of reaction time using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI TOF MS). The resulting series of polymer adducts terminated with various end-functional groups were precisely identified and the relative compositions of those series were estimated. A new MALDI MS data interpretation method was developed, consisting of a peak-resolving algorithm for overlapping peaks in MALDI MS spectra, a retrosynthetic analysis for the generation of reduced unit mass peaks, and a Gaussian fit-based selection of the most prominent polymer series among the reconstructed unit mass peaks. This method of data interpretation avoids errors originating from side reactions due to the presence of trace water in the reaction mixture or MALDI analysis. Quantitative changes in the relative compositions of the resulting polymer products were monitored as a function of reaction time. These results demonstrate that the mass data interpretation method described herein can be a powerful tool for estimating quantitative changes in the compositions of polymer products arising during a polymerization reaction.

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“…To sequence the peptide, the molecular ion is fragmented by post-source decay (PSD; for peptides <1,500 Da) or ion-source decay (ISD; for peptides >1,500 Da) and the sequence is determined from the mass of fragmented ions (72). Size exclusion chromatography combined with MALDI mass spectrometry (SEC/MALDI) (73) or pulsed gradient spin-echo (PGSE) NMR combined with MALDI can be used to determine molecular weight distribution of macromers and polymers with very high accuracy (74). Accurate determination of macromer molecular weight distribution and sequence distribution of the conjugated peptide is required for relating the chemical/molecular structure to conformation and nanostructure of the selfassembled polymer-peptide conjugate (75).…”

Section: Characterization Of Peptidomimetic Npsmentioning

confidence: 99%

Targeted Delivery with Peptidomimetic Conjugated Self-Assembled Nanoparticles

Jabbari

2008

Pharm Res

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Peptides produce specific nanostructures, making them useful for targeting in biological systems but they have low bioavailability, potential immunogenicity and poor metabolic stability. Peptidomimetic self-assembled NPs can possess biological recognition motifs as well as providing desired engineering properties. Inorganic NPs, coated with self-assembled macromers for stability and anti-fouling, and conjugated with target-specific ligands, are advancing imaging from the anatomy-based level to the molecular level. Ligand conjugated NPs are attractive for cell-selective tumor drug delivery, since this process has high transport capacity as well as ligand dependent cell specificity. Peptidomimetic NPs can provide stronger interaction with surface receptors on tumor cells, resulting in higher uptake and reduced drug resistance. Self-assembled NPs conjugated with peptidomimetic antigens are ideal for sustained presentation of vaccine antigens to dendritic cells and subsequent activation of T cell mediated adaptive immune response. Self-assembled NPs are a viable alternative to encapsulation for sustained delivery of proteins in tissue engineering. Cell penetrating peptides conjugated to NPs are used as intracellular delivery vectors for gene expression and as transfection agents for plasmid delivery. In this work, synthesis, characterization, properties, immunogenicity, and medical applications of peptidomimetic NPs in imaging, tumor delivery, vaccination, tissue engineering, and intracellular delivery are reviewed.

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Data Processing Method for the Determination of Accurate Molecular Weight Distribution of Polymers by SEC/MALDI-MS

Cited by 24 publications

References 25 publications

A Perfect Couple: PLP/SEC/ESI‐MS for the Accurate Determination of Propagation Rate Coefficients in Free Radical Polymerization

A Perfect Couple: PLP/SEC/ESI‐MS for the Accurate Determination of Propagation Rate Coefficients in Free Radical Polymerization

MALDI MS-based Composition Analysis of the Polymerization Reaction of Toluene Diisocyanate (TDI) and Ethylene Glycol (EG)

Targeted Delivery with Peptidomimetic Conjugated Self-Assembled Nanoparticles

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