A study of bioactive, branched (1→3)-β-d-glucans in dimethylacetamide/LiCl and dimethyl sulphoxide/LiCl using size-exclusion chromatography with multi-angle light scattering detection

•DMAc/LiCl and DMSO/LiCl were evaluated and compared as solvents for SEC-MALLS of β-(1→3)-d-glucans.•A new SEC-MALLS protocol based on DMAc/LiCl as solvent was developed.•A kinetic model for depolymerization upon heat treatment in DMAc/LiCl is provided.•SEC-MALLS in DMSO prone to artefacts and low s...

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Veröffentlicht in:Journal of Chromatography A 2013-08, Vol.1305, p.109-113
Hauptverfasser: Qin, Fen, Kes, Mürşide, Christensen, Bjørn E.
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Christensen, Bjørn E.
description •DMAc/LiCl and DMSO/LiCl were evaluated and compared as solvents for SEC-MALLS of β-(1→3)-d-glucans.•A new SEC-MALLS protocol based on DMAc/LiCl as solvent was developed.•A kinetic model for depolymerization upon heat treatment in DMAc/LiCl is provided.•SEC-MALLS in DMSO prone to artefacts and low sensitivity in MALLS. Water-soluble (1→3)-β-d-glucans with 1,6-linked branches (SBG) isolated from the cell walls of Saccharomyces cerevisiae were studied by size exclusion chromatography (SEC) with multi-angle laser light scattering (MALLS) detector using dimethylacetamide (DMAc) containing 0.5% (0.12M) LiCl, or dimethyl sulphoxide (DMSO) in the absence and presence of 0.25M LiCl, respectively, as eluents. The aggregating glucan could be dispersed as single chains in both solvents, with chain length distributions in reasonable agreement with results obtained previously with carboxymethylated glucans in aqueous solvent. However, DMAc is preferred over DMSO because of higher sensitivity in MALLS, and also because the latter produces SEC anomalies. SBG dissolves slowly in DMAc/LICl at room temperature, but heating accelerates the process. The rate of depolymerisation of SBG in DMAc/LiCl at high temperatures (70–105°C) was determined as a basis for defining dissolution procedures at elevated temperatures with a minimum of degradation. The result of the investigation is a simple and reliable protocol for preparing unaggregated, fully dissolved and undegraded SBG in DMAc/LiCl, which is well suited as a standard analysis of the molecular weight distribution of SBG-like molecules without chemical derivatization.
doi_str_mv 10.1016/j.chroma.2013.07.002
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Water-soluble (1→3)-β-d-glucans with 1,6-linked branches (SBG) isolated from the cell walls of Saccharomyces cerevisiae were studied by size exclusion chromatography (SEC) with multi-angle laser light scattering (MALLS) detector using dimethylacetamide (DMAc) containing 0.5% (0.12M) LiCl, or dimethyl sulphoxide (DMSO) in the absence and presence of 0.25M LiCl, respectively, as eluents. The aggregating glucan could be dispersed as single chains in both solvents, with chain length distributions in reasonable agreement with results obtained previously with carboxymethylated glucans in aqueous solvent. However, DMAc is preferred over DMSO because of higher sensitivity in MALLS, and also because the latter produces SEC anomalies. SBG dissolves slowly in DMAc/LICl at room temperature, but heating accelerates the process. The rate of depolymerisation of SBG in DMAc/LiCl at high temperatures (70–105°C) was determined as a basis for defining dissolution procedures at elevated temperatures with a minimum of degradation. The result of the investigation is a simple and reliable protocol for preparing unaggregated, fully dissolved and undegraded SBG in DMAc/LiCl, which is well suited as a standard analysis of the molecular weight distribution of SBG-like molecules without chemical derivatization.</description><identifier>ISSN: 0021-9673</identifier><identifier>EISSN: 1873-3778</identifier><identifier>DOI: 10.1016/j.chroma.2013.07.002</identifier><identifier>PMID: 23891208</identifier><identifier>CODEN: JOCRAM</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>(1 → 3)-β-d-Glucan ; Acetamides - chemistry ; Analytical, structural and metabolic biochemistry ; Applied sciences ; bioactive properties ; Biological and medical sciences ; Carbohydrates ; cell walls ; Chromatography ; Chromatography, Gel - methods ; depolymerization ; derivatization ; Detectors ; Dimethyl sulfoxide ; Dimethyl Sulfoxide - chemistry ; Dimethyl sulphoxide (DMSO) ; Dimethylacetamide (DMAc) ; Dissolution ; Exact sciences and technology ; Fundamental and applied biological sciences. Psychology ; gel chromatography ; Glucan ; glucans ; Glucans - analysis ; heat ; Heating ; Light ; Light scattering ; lithium chloride ; Lithium Chloride - chemistry ; Miscellaneous ; molecular weight ; Organic polymers ; Other biological molecules ; Physicochemistry of polymers ; Properties and characterization ; Refractive index increment ; Saccharomyces cerevisiae ; Scattering, Radiation ; SEC-MALLS ; Solubility ; Solvents ; Structure, morphology and analysis ; temperature</subject><ispartof>Journal of Chromatography A, 2013-08, Vol.1305, p.109-113</ispartof><rights>2013 Elsevier B.V.</rights><rights>2014 INIST-CNRS</rights><rights>Copyright © 2013 Elsevier B.V. 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Water-soluble (1→3)-β-d-glucans with 1,6-linked branches (SBG) isolated from the cell walls of Saccharomyces cerevisiae were studied by size exclusion chromatography (SEC) with multi-angle laser light scattering (MALLS) detector using dimethylacetamide (DMAc) containing 0.5% (0.12M) LiCl, or dimethyl sulphoxide (DMSO) in the absence and presence of 0.25M LiCl, respectively, as eluents. The aggregating glucan could be dispersed as single chains in both solvents, with chain length distributions in reasonable agreement with results obtained previously with carboxymethylated glucans in aqueous solvent. However, DMAc is preferred over DMSO because of higher sensitivity in MALLS, and also because the latter produces SEC anomalies. SBG dissolves slowly in DMAc/LICl at room temperature, but heating accelerates the process. The rate of depolymerisation of SBG in DMAc/LiCl at high temperatures (70–105°C) was determined as a basis for defining dissolution procedures at elevated temperatures with a minimum of degradation. The result of the investigation is a simple and reliable protocol for preparing unaggregated, fully dissolved and undegraded SBG in DMAc/LiCl, which is well suited as a standard analysis of the molecular weight distribution of SBG-like molecules without chemical derivatization.</description><subject>(1 → 3)-β-d-Glucan</subject><subject>Acetamides - chemistry</subject><subject>Analytical, structural and metabolic biochemistry</subject><subject>Applied sciences</subject><subject>bioactive properties</subject><subject>Biological and medical sciences</subject><subject>Carbohydrates</subject><subject>cell walls</subject><subject>Chromatography</subject><subject>Chromatography, Gel - methods</subject><subject>depolymerization</subject><subject>derivatization</subject><subject>Detectors</subject><subject>Dimethyl sulfoxide</subject><subject>Dimethyl Sulfoxide - chemistry</subject><subject>Dimethyl sulphoxide (DMSO)</subject><subject>Dimethylacetamide (DMAc)</subject><subject>Dissolution</subject><subject>Exact sciences and technology</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>gel chromatography</subject><subject>Glucan</subject><subject>glucans</subject><subject>Glucans - analysis</subject><subject>heat</subject><subject>Heating</subject><subject>Light</subject><subject>Light scattering</subject><subject>lithium chloride</subject><subject>Lithium Chloride - chemistry</subject><subject>Miscellaneous</subject><subject>molecular weight</subject><subject>Organic polymers</subject><subject>Other biological molecules</subject><subject>Physicochemistry of polymers</subject><subject>Properties and characterization</subject><subject>Refractive index increment</subject><subject>Saccharomyces cerevisiae</subject><subject>Scattering, Radiation</subject><subject>SEC-MALLS</subject><subject>Solubility</subject><subject>Solvents</subject><subject>Structure, morphology and analysis</subject><subject>temperature</subject><issn>0021-9673</issn><issn>1873-3778</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2013</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkk1u1DAYhiMEoqVwAwTeIBWJTP2TieNNpWrEnzQSC-jacuwviUdJPNhO6XAADsBRWHIIDsFJ8JBh2MHKsr_n-3tfZ9ljghcEk_Jis9Cdd4NaUEzYAvMFxvROdkoqznLGeXU3O00vJBclZyfZgxA2GBOOOb2fnVBWCUJxdZp9v0IhTmaHXINq65SO9gZeoNqrUXdg0Dn5-eUre57_-JabvO0nrcaA7IiMHSB2u15piGqwBi7WdtUjNZpjCIWp33bu9hicgh1bFOxnyOFW9-nqRjQvEV3r1bbboU82dmiY-mhzNbY9oN62XURBqxjB7_MNREhTuvFhdq9RfYBHh_Msu3718sPqTb5-9_rt6mqd66KiMSeKgCBYkYolPYSqQdAa67LWgtOmqDXlXClqlmXJTFVzbZaFFgagwarAy4qdZedz3a13HycIUQ42aOh7NYKbgiQVxgUtWSH-j5ZsiSkTdF-1mFHtXQgeGrn1dlB-JwmWe4PlRs7ayL3BEnOZxk9pTw4dpnoAc0z642gCnh0AlUTrm72RNvzleFkIKsrEPZ25RjmpWp-Y6_ep0zL9EkGK33tfzgQkcW8seBm0hVGDsT45II2z_571F1rT09E</recordid><startdate>20130830</startdate><enddate>20130830</enddate><creator>Qin, Fen</creator><creator>Kes, Mürşide</creator><creator>Christensen, Bjørn E.</creator><general>Elsevier B.V</general><general>Elsevier</general><scope>FBQ</scope><scope>IQODW</scope><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7QH</scope><scope>7UA</scope><scope>C1K</scope><scope>F1W</scope><scope>H97</scope><scope>L.G</scope><scope>7U5</scope><scope>8FD</scope><scope>L7M</scope></search><sort><creationdate>20130830</creationdate><title>A study of bioactive, branched (1→3)-β-d-glucans in dimethylacetamide/LiCl and dimethyl sulphoxide/LiCl using size-exclusion chromatography with multi-angle light scattering detection</title><author>Qin, Fen ; Kes, Mürşide ; Christensen, Bjørn E.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c482t-1a1e910a1830029abe92b0c6bc972f4bc277aa2d5663d8b7cd54c9deef0a40583</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2013</creationdate><topic>(1 → 3)-β-d-Glucan</topic><topic>Acetamides - chemistry</topic><topic>Analytical, structural and metabolic biochemistry</topic><topic>Applied sciences</topic><topic>bioactive properties</topic><topic>Biological and medical sciences</topic><topic>Carbohydrates</topic><topic>cell walls</topic><topic>Chromatography</topic><topic>Chromatography, Gel - methods</topic><topic>depolymerization</topic><topic>derivatization</topic><topic>Detectors</topic><topic>Dimethyl sulfoxide</topic><topic>Dimethyl Sulfoxide - chemistry</topic><topic>Dimethyl sulphoxide (DMSO)</topic><topic>Dimethylacetamide (DMAc)</topic><topic>Dissolution</topic><topic>Exact sciences and technology</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>gel chromatography</topic><topic>Glucan</topic><topic>glucans</topic><topic>Glucans - analysis</topic><topic>heat</topic><topic>Heating</topic><topic>Light</topic><topic>Light scattering</topic><topic>lithium chloride</topic><topic>Lithium Chloride - chemistry</topic><topic>Miscellaneous</topic><topic>molecular weight</topic><topic>Organic polymers</topic><topic>Other biological molecules</topic><topic>Physicochemistry of polymers</topic><topic>Properties and characterization</topic><topic>Refractive index increment</topic><topic>Saccharomyces cerevisiae</topic><topic>Scattering, Radiation</topic><topic>SEC-MALLS</topic><topic>Solubility</topic><topic>Solvents</topic><topic>Structure, morphology and analysis</topic><topic>temperature</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Qin, Fen</creatorcontrib><creatorcontrib>Kes, Mürşide</creatorcontrib><creatorcontrib>Christensen, Bjørn E.</creatorcontrib><collection>AGRIS</collection><collection>Pascal-Francis</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>Aqualine</collection><collection>Water Resources Abstracts</collection><collection>Environmental Sciences and Pollution Management</collection><collection>ASFA: Aquatic Sciences and Fisheries Abstracts</collection><collection>Aquatic Science &amp; Fisheries Abstracts (ASFA) 3: Aquatic Pollution &amp; Environmental Quality</collection><collection>Aquatic Science &amp; Fisheries Abstracts (ASFA) Professional</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>Technology Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><jtitle>Journal of Chromatography A</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Qin, Fen</au><au>Kes, Mürşide</au><au>Christensen, Bjørn E.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>A study of bioactive, branched (1→3)-β-d-glucans in dimethylacetamide/LiCl and dimethyl sulphoxide/LiCl using size-exclusion chromatography with multi-angle light scattering detection</atitle><jtitle>Journal of Chromatography A</jtitle><addtitle>J Chromatogr A</addtitle><date>2013-08-30</date><risdate>2013</risdate><volume>1305</volume><spage>109</spage><epage>113</epage><pages>109-113</pages><issn>0021-9673</issn><eissn>1873-3778</eissn><coden>JOCRAM</coden><abstract>•DMAc/LiCl and DMSO/LiCl were evaluated and compared as solvents for SEC-MALLS of β-(1→3)-d-glucans.•A new SEC-MALLS protocol based on DMAc/LiCl as solvent was developed.•A kinetic model for depolymerization upon heat treatment in DMAc/LiCl is provided.•SEC-MALLS in DMSO prone to artefacts and low sensitivity in MALLS. Water-soluble (1→3)-β-d-glucans with 1,6-linked branches (SBG) isolated from the cell walls of Saccharomyces cerevisiae were studied by size exclusion chromatography (SEC) with multi-angle laser light scattering (MALLS) detector using dimethylacetamide (DMAc) containing 0.5% (0.12M) LiCl, or dimethyl sulphoxide (DMSO) in the absence and presence of 0.25M LiCl, respectively, as eluents. The aggregating glucan could be dispersed as single chains in both solvents, with chain length distributions in reasonable agreement with results obtained previously with carboxymethylated glucans in aqueous solvent. However, DMAc is preferred over DMSO because of higher sensitivity in MALLS, and also because the latter produces SEC anomalies. SBG dissolves slowly in DMAc/LICl at room temperature, but heating accelerates the process. The rate of depolymerisation of SBG in DMAc/LiCl at high temperatures (70–105°C) was determined as a basis for defining dissolution procedures at elevated temperatures with a minimum of degradation. The result of the investigation is a simple and reliable protocol for preparing unaggregated, fully dissolved and undegraded SBG in DMAc/LiCl, which is well suited as a standard analysis of the molecular weight distribution of SBG-like molecules without chemical derivatization.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>23891208</pmid><doi>10.1016/j.chroma.2013.07.002</doi><tpages>5</tpages></addata></record>
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subjects (1 → 3)-β-d-Glucan
Acetamides - chemistry
Analytical, structural and metabolic biochemistry
Applied sciences
bioactive properties
Biological and medical sciences
Carbohydrates
cell walls
Chromatography
Chromatography, Gel - methods
depolymerization
derivatization
Detectors
Dimethyl sulfoxide
Dimethyl Sulfoxide - chemistry
Dimethyl sulphoxide (DMSO)
Dimethylacetamide (DMAc)
Dissolution
Exact sciences and technology
Fundamental and applied biological sciences. Psychology
gel chromatography
Glucan
glucans
Glucans - analysis
heat
Heating
Light
Light scattering
lithium chloride
Lithium Chloride - chemistry
Miscellaneous
molecular weight
Organic polymers
Other biological molecules
Physicochemistry of polymers
Properties and characterization
Refractive index increment
Saccharomyces cerevisiae
Scattering, Radiation
SEC-MALLS
Solubility
Solvents
Structure, morphology and analysis
temperature
title A study of bioactive, branched (1→3)-β-d-glucans in dimethylacetamide/LiCl and dimethyl sulphoxide/LiCl using size-exclusion chromatography with multi-angle light scattering detection
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