Mass spectrometric studies of cellulose ethers

Dane Momcilovic

Mass spectrometric studies of cellulose ethers

Dane Momcilovic

Centrum för analys och syntes

Forskningsoutput: Avhandling › Doktorsavhandling (sammanläggning)

Sammanfattning

Popular Abstract in Swedish
Cellulosa etrar är en grupp ämnen som har många tillämpningar inom olika områden. Det stora antalet tillämpningar ställer höga krav på de teknologiska egenskaperna hos cellulosa etrarna. För att kunna kontrollera de teknologiska egenskaperna är det nödvändigt att utveckla analytiska metoder, med vilka egenskaperna kan korreleras till den kemiska strukturen. Ibland går det inte att förklara variationer i de teknologiska egenskaperna med dagens befintliga analysmetoder och tekniker. Därför är det viktigt att undersöka lämpligheten hos nya analytiska tekniker för kemisk karakterisering av cellulosa etrar.

I den här avhandlingen har matris-assisterad laser desorptions/joniserings masspektrometri (MALDI-MS) och nano-elektrosprej joniserings masspektrometri (nano-ESI-MS) studerats i syfte att analysera cellulosa etrar. Båda teknikerna har visat sig vara utmärkta verktyg för strukturanalys av oligomerfragment utav cellulosa etrar. Nano-ESI-MS har också använts för att studera selektiviteten hos ett cellulosanedbrytande enzym, endoglukanas, på metyl cellulosa (MC). Då oligomerfragmenten derivatiserades med dialkylaminer kunde det konstateras att känsligheten i MALDI-MS och nano-ESI-MS ökade markant. Dessa derivaten förenklade också för strukturanalys med hjälp av tandem masspektrometri. Molmassefördelningen hos partiellt depolymeriserad MC kunde mätas genom att sammankoppa storleksuteslutningskromatografi med MALDI-MS. Vidare demonstrerades det att det med MALDI-MS mycket enkelt och snabbt går att särskilja cellulosa etrar med olika substitutionsgrad.

Originalspråk	engelska
Kvalifikation	Doktor
Tilldelande institution	Centrum för analys och syntes
Handledare	Wahlund, Karl-Gustav, handledare
Tilldelningsdatum	2005 apr. 29
Förlag	Analytical Chemistry, Lund University
ISBN (tryckt)	91-628-6316-9
Status	Published - 2005

Bibliografisk information

Defence details

Date: 2005-04-29
Time: 10:30
Place: Lecture Hall B, Centre for Chemistry and Chemical Engineering, Getingevägen 60, Lund, Sweden.

External reviewer(s)

Name: Mischnick, Petra
Title: Prof. Dr.
Affiliation: Technische Universität Carolo-Wilhelmina zu Braunschweig, Institut für Lebensmittelchemie, Braunschw

---

The information about affiliations in this record was updated in December 2015.
The record was previously connected to the following departments: Analytical Chemistry (S/LTH) (011001004)

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@phdthesis{30e5d7ea867740aeba4761a036e516fd,

title = "Mass spectrometric studies of cellulose ethers",

abstract = "Cellulose based derivatives, such as cellulose ethers, today find many applications in a diverse range of fields. The numerous applications put high demands on the technological performance of the cellulose ethers. In order to be able to control the technological properties it is necessary to develop analytical methods by, which they can be correlated to the chemical structure. In some cases variations in the technological properties cannot be explained by the chemical characterisation methods available today. Thus, it is of high importance to investigate the suitability of new analytical techniques for chemical characterisation of cellulose ethers. In this thesis matrix-assisted laser desorption/ionisation mass spectrometry (MALDI-MS) and nanoelectrospray ionisation (nano-ESI)-MS were studied as analytical techniques for cellulose ethers. Among the results, MALDI tandem mass spectrometry (MS/MS) and nano-ESI-MS/MS were demonstrated as exceptionally useful tools for the structure analysis of cellulose ether oligosaccharides. Nano-ESI-MS/MS was employed to characterise the selectivity of a cellulose depolymerising enzyme, endoglucanase, on methyl cellulose (MC). Novel dialkylamine derivatives of cellulose ether oligosaccharides were shown to increase the sensitivity in both MALDI- and nano-ESI-MS, and to facilitate structure analysis by MS/MS. Studies of the molar mass distribution of partially depolymerised MC were performed by size-exclusion chromatography semi-online to MALDI-MS. The sample preparation method for MALDI was found to have a significant influence on the outcome of the analysis. Furthermore, a simple experiment showed that, the combination of MALDI-MS and partial acidic depolymerisation could be used to distinguish between cellulose ethers of different degrees of substitution.",

keywords = "Polymerteknik, biopolymers, Polymer technology, Analytisk kemi, Analytical chemistry, enzymatic depolymerisation, reductive amination, electrospray ionisation, cellulose ethers, MALDI, mass spectrometry",

author = "Dane Momcilovic",

note = "Defence details Date: 2005-04-29 Time: 10:30 Place: Lecture Hall B, Centre for Chemistry and Chemical Engineering, Getingev{\"a}gen 60, Lund, Sweden. External reviewer(s) Name: Mischnick, Petra Title: Prof. Dr. Affiliation: Technische Universit{\"a}t Carolo-Wilhelmina zu Braunschweig, Institut f{\"u}r Lebensmittelchemie, Braunschw --- The information about affiliations in this record was updated in December 2015. The record was previously connected to the following departments: Analytical Chemistry (S/LTH) (011001004)",

year = "2005",

language = "English",

isbn = "91-628-6316-9",

publisher = "Analytical Chemistry, Lund University",

type = "Doctoral Thesis (compilation)",

school = "Centre for Analysis and Synthesis",

}

TY - THES

T1 - Mass spectrometric studies of cellulose ethers

AU - Momcilovic, Dane

N1 - Defence details Date: 2005-04-29 Time: 10:30 Place: Lecture Hall B, Centre for Chemistry and Chemical Engineering, Getingevägen 60, Lund, Sweden. External reviewer(s) Name: Mischnick, Petra Title: Prof. Dr. Affiliation: Technische Universität Carolo-Wilhelmina zu Braunschweig, Institut für Lebensmittelchemie, Braunschw --- The information about affiliations in this record was updated in December 2015. The record was previously connected to the following departments: Analytical Chemistry (S/LTH) (011001004)

PY - 2005

Y1 - 2005

N2 - Cellulose based derivatives, such as cellulose ethers, today find many applications in a diverse range of fields. The numerous applications put high demands on the technological performance of the cellulose ethers. In order to be able to control the technological properties it is necessary to develop analytical methods by, which they can be correlated to the chemical structure. In some cases variations in the technological properties cannot be explained by the chemical characterisation methods available today. Thus, it is of high importance to investigate the suitability of new analytical techniques for chemical characterisation of cellulose ethers. In this thesis matrix-assisted laser desorption/ionisation mass spectrometry (MALDI-MS) and nanoelectrospray ionisation (nano-ESI)-MS were studied as analytical techniques for cellulose ethers. Among the results, MALDI tandem mass spectrometry (MS/MS) and nano-ESI-MS/MS were demonstrated as exceptionally useful tools for the structure analysis of cellulose ether oligosaccharides. Nano-ESI-MS/MS was employed to characterise the selectivity of a cellulose depolymerising enzyme, endoglucanase, on methyl cellulose (MC). Novel dialkylamine derivatives of cellulose ether oligosaccharides were shown to increase the sensitivity in both MALDI- and nano-ESI-MS, and to facilitate structure analysis by MS/MS. Studies of the molar mass distribution of partially depolymerised MC were performed by size-exclusion chromatography semi-online to MALDI-MS. The sample preparation method for MALDI was found to have a significant influence on the outcome of the analysis. Furthermore, a simple experiment showed that, the combination of MALDI-MS and partial acidic depolymerisation could be used to distinguish between cellulose ethers of different degrees of substitution.

AB - Cellulose based derivatives, such as cellulose ethers, today find many applications in a diverse range of fields. The numerous applications put high demands on the technological performance of the cellulose ethers. In order to be able to control the technological properties it is necessary to develop analytical methods by, which they can be correlated to the chemical structure. In some cases variations in the technological properties cannot be explained by the chemical characterisation methods available today. Thus, it is of high importance to investigate the suitability of new analytical techniques for chemical characterisation of cellulose ethers. In this thesis matrix-assisted laser desorption/ionisation mass spectrometry (MALDI-MS) and nanoelectrospray ionisation (nano-ESI)-MS were studied as analytical techniques for cellulose ethers. Among the results, MALDI tandem mass spectrometry (MS/MS) and nano-ESI-MS/MS were demonstrated as exceptionally useful tools for the structure analysis of cellulose ether oligosaccharides. Nano-ESI-MS/MS was employed to characterise the selectivity of a cellulose depolymerising enzyme, endoglucanase, on methyl cellulose (MC). Novel dialkylamine derivatives of cellulose ether oligosaccharides were shown to increase the sensitivity in both MALDI- and nano-ESI-MS, and to facilitate structure analysis by MS/MS. Studies of the molar mass distribution of partially depolymerised MC were performed by size-exclusion chromatography semi-online to MALDI-MS. The sample preparation method for MALDI was found to have a significant influence on the outcome of the analysis. Furthermore, a simple experiment showed that, the combination of MALDI-MS and partial acidic depolymerisation could be used to distinguish between cellulose ethers of different degrees of substitution.

KW - Polymerteknik

KW - biopolymers

KW - Polymer technology

KW - Analytisk kemi

KW - Analytical chemistry

KW - enzymatic depolymerisation

KW - reductive amination

KW - electrospray ionisation

KW - cellulose ethers

KW - MALDI

KW - mass spectrometry

M3 - Doctoral Thesis (compilation)

SN - 91-628-6316-9

PB - Analytical Chemistry, Lund University

ER -

Mass spectrometric studies of cellulose ethers

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