Improved matrix‐assisted laser desorption/ionisation sample preparation of a partially depolymerised cellulose derivative by continuous spray deposition and interfacing with size‐exclusion chromatography

Momcilovic, Dane; Wahlund, Karl-Gustav; Wittgren, Bengt; Brinkmalm, Gunnar

doi:10.1002/rcm.1874

Cited by 8 publications

(11 citation statements)

References 37 publications

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“…The molar-mass distributions (MMD) of the intact and enzymatically hydrolyzed MC (nonacetylated) were calculated from SEC-MALS/RI analysis of nonacetylated MC. The d n /d c for methyl cellulose in aqueous solution was taken to be 0.141 mL/g and was assumed to be constant across the molar-mass and substituent-level distributions . The resulting MMDs are shown in Figure .…”

Section: Resultsmentioning

confidence: 99%

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NMR, Cloud-Point Measurements and Enzymatic Depolymerization: Complementary Tools to Investigate Substituent Patterns in Modified Celluloses

et al. 2006

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The substituent patterns of some chemically modified celluloses were characterized as a function of their size distribution, using size-exclusion chromatography coupled to both nuclear magnetic resonance spectroscopy (NMR) and cloud-point measurements. Intact and enzymatically hydrolyzed methyl cellulose (MC) was fractionated according to size, and the level of substitution of the fractions was measured off-line using NMR. Clouding behavior was also measured as a function of size. Clear differences between hydrolyzed and nonhydrolyzed samples were observed using both techniques. For samples that had been selectively hydrolyzed using cellulose-degrading enzymes, NMR data showed a direct link between the degree of degradation and the level of substitution. Differences in the clouding behavior highlighted changes in substituent levels and substituent patterns across the size distribution. The techniques gave valuable and somewhat complementary information on the substituent distributions of the samples before and after enzymatic hydrolysis.

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Section: Resultsmentioning

confidence: 99%

“…The dn/dc for methyl cellulose in aqueous solution was taken to be 0.141 mL/g and was assumed to be constant across the molar-mass and substituent-level distributions. 27 The resulting MMDs are shown in Figure 2.…”

Section: Secmentioning

confidence: 99%

NMR, Cloud-Point Measurements and Enzymatic Depolymerization: Complementary Tools to Investigate Substituent Patterns in Modified Celluloses

et al. 2006

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“…Acidic De polymerization. Partial acidic depolymerization was performed according to Momcilovic et al…”

Section: Methodsmentioning

confidence: 99%

Improved Chemical Analysis of Cellulose Ethers Using Dialkylamine Derivatization and Mass Spectrometry

et al. 2005

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Oligosaccharides of hydroxypropylmethyl cellulose, hydroxypropyl cellulose, and methyl cellulose were investigated by matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). The cellulose ether oligosaccharides were produced either by enzymatic depolymerization utilizing the purified family 5 endoglucanase from Bacillus agaradhaerens or by partial acidic depolymerization. To lower the limit of detection in MALDI-MS three dilakylamines, dimethyl-, diethyl-, and dipropylamine were studied as reagents for reductive amination of the oligosaccharides. All three amines contributed to a significant increase in sensitivity in MALDI-MS, especially for oligosaccharides with a degree of polymerization (DP) < 3. These reagents were also attractive due to their high volatility, which facilitated the purification of the reaction mixtures. It was established that low-mass discrimination in MALDI-MS in the DP range 1-7 was substantially reduced with dialkylamine derivatization. Hence, dialkylamine derivatization of cellulose ether oligosaccharides obtained by endoglucanase depolymerization increased the number of detected analyte components. Dimethylamine was concluded to be the preferred reagent of those evaluated.

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“…Continuous spray deposition of aqueous solutions of partially depolymerized methyl cellulose (30) from an HPLC column has been reported to improve sensitivity of detection by up to an order of magnitude compared with standard preparation techniques (Momcilovic et al, 2005b). Furthermore, the analyte was more evenly distributed over the target surface, resulting in higher reproducibility.…”

Section: A Polysaccharidesmentioning

confidence: 99%

Analysis of carbohydrates and glycoconjugates by matrix‐assisted laser desorption/ionization mass spectrometry: An update for the period 2005–2006

Harvey

2010

Mass Spectrometry Reviews

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This review is the fourth update of the original review, published in 1999, on the application of MALDI mass spectrometry to the analysis of carbohydrates and glycoconjugates and brings coverage of the literature to the end of 2006. The review covers fundamental studies, fragmentation of carbohydrate ions, method developments, and applications of the technique to the analysis of different types of carbohydrate. Specific compound classes that are covered include carbohydrate polymers from plants, N- and O-linked glycans from glycoproteins, glycated proteins, glycolipids from bacteria, glycosides, and various other natural products. There is a short section on the use of MALDI-TOF mass spectrometry for the study of enzymes involved in glycan processing, a section on industrial processes, particularly the development of biopharmaceuticals and a section on the use of MALDI-MS to monitor products of chemical synthesis of carbohydrates. Large carbohydrate-protein complexes and glycodendrimers are highlighted in this final section.

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Improved matrix‐assisted laser desorption/ionisation sample preparation of a partially depolymerised cellulose derivative by continuous spray deposition and interfacing with size‐exclusion chromatography

Cited by 8 publications

References 37 publications

NMR, Cloud-Point Measurements and Enzymatic Depolymerization: Complementary Tools to Investigate Substituent Patterns in Modified Celluloses

NMR, Cloud-Point Measurements and Enzymatic Depolymerization: Complementary Tools to Investigate Substituent Patterns in Modified Celluloses

Improved Chemical Analysis of Cellulose Ethers Using Dialkylamine Derivatization and Mass Spectrometry

Analysis of carbohydrates and glycoconjugates by matrix‐assisted laser desorption/ionization mass spectrometry: An update for the period 2005–2006

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