Determination of hydroxyl groups in biorefinery resources via quantitative 31P NMR spectroscopy.
Identifieur interne : 000A35 ( Main/Exploration ); précédent : 000A34; suivant : 000A36Determination of hydroxyl groups in biorefinery resources via quantitative 31P NMR spectroscopy.
Auteurs : Xianzhi Meng [États-Unis] ; Claudia Crestini [Italie] ; Haoxi Ben [République populaire de Chine] ; Naijia Hao [États-Unis] ; Yunqiao Pu [États-Unis] ; Arthur J. Ragauskas [États-Unis] ; Dimitris S. Argyropoulos [États-Unis]Source :
- Nature protocols [ 1750-2799 ] ; 2019.
Descripteurs français
- KwdFr :
- MESH :
English descriptors
- KwdEn :
- MESH :
- chemical , analysis : Lignin, Tannins.
- chemical , chemistry : Lignin, Phosphorus, Tannins.
- chemistry : Panicum, Pinus, Populus.
- methods : Magnetic Resonance Spectroscopy.
Abstract
The analysis of chemical structural characteristics of biorefinery product streams (such as lignin and tannin) has advanced substantially over the past decade, with traditional wet-chemical techniques being replaced or supplemented by NMR methodologies. Quantitative 31P NMR spectroscopy is a promising technique for the analysis of hydroxyl groups because of its unique characterization capability and broad potential applicability across the biorefinery research community. This protocol describes procedures for (i) the preparation/solubilization of lignin and tannin, (ii) the phosphitylation of their hydroxyl groups, (iii) NMR acquisition details, and (iv) the ensuing data analyses and means to precisely calculate the content of the different types of hydroxyl groups. Compared with traditional wet-chemical techniques, the technique of quantitative 31P NMR spectroscopy offers unique advantages in measuring hydroxyl groups in a single spectrum with high signal resolution. The method provides complete quantitative information about the hydroxyl groups with small amounts of sample (~30 mg) within a relatively short experimental time (~30-120 min).
DOI: 10.1038/s41596-019-0191-1
PubMed: 31391578
Affiliations:
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Argyropoulos</name><affiliation wicri:level="2"><nlm:affiliation>Departments of Chemistry and Forest Biomaterials, North Carolina State University, Raleigh, NC, USA. dsargyro@ncsu.edu.</nlm:affiliation><country xml:lang="fr">États-Unis</country><wicri:regionArea>Departments of Chemistry and Forest Biomaterials, North Carolina State University, Raleigh, NC</wicri:regionArea><placeName><region type="state">Caroline du Nord</region></placeName></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">PubMed</idno><date when="2019">2019</date><idno type="RBID">pubmed:31391578</idno><idno type="pmid">31391578</idno><idno type="doi">10.1038/s41596-019-0191-1</idno><idno type="wicri:Area/Main/Corpus">000762</idno><idno type="wicri:explorRef" wicri:stream="Main" wicri:step="Corpus" wicri:corpus="PubMed">000762</idno><idno type="wicri:Area/Main/Curation">000762</idno><idno type="wicri:explorRef" wicri:stream="Main" wicri:step="Curation">000762</idno><idno type="wicri:Area/Main/Exploration">000762</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en">Determination of hydroxyl groups in biorefinery resources via quantitative <sup>31</sup>P NMR spectroscopy.</title><author><name sortKey="Meng, Xianzhi" sort="Meng, Xianzhi" uniqKey="Meng X" first="Xianzhi" last="Meng">Xianzhi Meng</name><affiliation wicri:level="2"><nlm:affiliation>Department of Chemical and Biomolecular Engineering, The University of Tennessee, Knoxville, TN, USA.</nlm:affiliation><country xml:lang="fr">États-Unis</country><wicri:regionArea>Department of Chemical and Biomolecular Engineering, The University of Tennessee, Knoxville, TN</wicri:regionArea><placeName><region type="state">Tennessee</region></placeName></affiliation></author><author><name sortKey="Crestini, Claudia" sort="Crestini, Claudia" uniqKey="Crestini C" first="Claudia" last="Crestini">Claudia Crestini</name><affiliation wicri:level="1"><nlm:affiliation>Department of Molecular Science and Nanosystems, Ca' Foscari University of Venice, Venice, Italy. claudia.crestini@unive.it.</nlm:affiliation><country xml:lang="fr">Italie</country><wicri:regionArea>Department of Molecular Science and Nanosystems, Ca' Foscari University of Venice, Venice</wicri:regionArea><wicri:noRegion>Venice</wicri:noRegion></affiliation></author><author><name sortKey="Ben, Haoxi" sort="Ben, Haoxi" uniqKey="Ben H" first="Haoxi" last="Ben">Haoxi Ben</name><affiliation wicri:level="1"><nlm:affiliation>State Key Laboratory of Bio-Fibers and Eco-Textiles, Qingdao University, Qingdao, China.</nlm:affiliation><country xml:lang="fr">République populaire de Chine</country><wicri:regionArea>State Key Laboratory of Bio-Fibers and Eco-Textiles, Qingdao University, Qingdao</wicri:regionArea><wicri:noRegion>Qingdao</wicri:noRegion></affiliation></author><author><name sortKey="Hao, Naijia" sort="Hao, Naijia" uniqKey="Hao N" first="Naijia" last="Hao">Naijia Hao</name><affiliation wicri:level="2"><nlm:affiliation>Department of Chemical and Biomolecular Engineering, The University of Tennessee, Knoxville, TN, USA.</nlm:affiliation><country xml:lang="fr">États-Unis</country><wicri:regionArea>Department of Chemical and Biomolecular Engineering, The University of Tennessee, Knoxville, TN</wicri:regionArea><placeName><region type="state">Tennessee</region></placeName></affiliation></author><author><name sortKey="Pu, Yunqiao" sort="Pu, Yunqiao" uniqKey="Pu Y" first="Yunqiao" last="Pu">Yunqiao Pu</name><affiliation wicri:level="2"><nlm:affiliation>Center for Bioenergy Innovation (CBI), Joint Institute for Biological Sciences, Biosciences Division, Oak Ridge National Laboratory (ORNL), Oak Ridge, TN, USA.</nlm:affiliation><country xml:lang="fr">États-Unis</country><wicri:regionArea>Center for Bioenergy Innovation (CBI), Joint Institute for Biological Sciences, Biosciences Division, Oak Ridge National Laboratory (ORNL), Oak Ridge, TN</wicri:regionArea><placeName><region type="state">Tennessee</region></placeName></affiliation></author><author><name sortKey="Ragauskas, Arthur J" sort="Ragauskas, Arthur J" uniqKey="Ragauskas A" first="Arthur J" last="Ragauskas">Arthur J. Ragauskas</name><affiliation wicri:level="2"><nlm:affiliation>Department of Chemical and Biomolecular Engineering, The University of Tennessee, Knoxville, TN, USA. aragausk@utk.edu.</nlm:affiliation><country xml:lang="fr">États-Unis</country><wicri:regionArea>Department of Chemical and Biomolecular Engineering, The University of Tennessee, Knoxville, TN</wicri:regionArea><placeName><region type="state">Tennessee</region></placeName></affiliation><affiliation wicri:level="2"><nlm:affiliation>Center for Bioenergy Innovation (CBI), Joint Institute for Biological Sciences, Biosciences Division, Oak Ridge National Laboratory (ORNL), Oak Ridge, TN, USA. aragausk@utk.edu.</nlm:affiliation><country xml:lang="fr">États-Unis</country><wicri:regionArea>Center for Bioenergy Innovation (CBI), Joint Institute for Biological Sciences, Biosciences Division, Oak Ridge National Laboratory (ORNL), Oak Ridge, TN</wicri:regionArea><placeName><region type="state">Tennessee</region></placeName></affiliation><affiliation wicri:level="2"><nlm:affiliation>Department of Forestry, Wildlife and Fisheries, Center of Renewable Carbon, The University of Tennessee Institute of Agriculture, Knoxville, TN, USA. aragausk@utk.edu.</nlm:affiliation><country xml:lang="fr">États-Unis</country><wicri:regionArea>Department of Forestry, Wildlife and Fisheries, Center of Renewable Carbon, The University of Tennessee Institute of Agriculture, Knoxville, TN</wicri:regionArea><placeName><region type="state">Tennessee</region></placeName></affiliation></author><author><name sortKey="Argyropoulos, Dimitris S" sort="Argyropoulos, Dimitris S" uniqKey="Argyropoulos D" first="Dimitris S" last="Argyropoulos">Dimitris S. Argyropoulos</name><affiliation wicri:level="2"><nlm:affiliation>Departments of Chemistry and Forest Biomaterials, North Carolina State University, Raleigh, NC, USA. dsargyro@ncsu.edu.</nlm:affiliation><country xml:lang="fr">États-Unis</country><wicri:regionArea>Departments of Chemistry and Forest Biomaterials, North Carolina State University, Raleigh, NC</wicri:regionArea><placeName><region type="state">Caroline du Nord</region></placeName></affiliation></author></analytic><series><title level="j">Nature protocols</title><idno type="eISSN">1750-2799</idno><imprint><date when="2019" type="published">2019</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass><keywords scheme="KwdEn" xml:lang="en"><term>Lignin (analysis)</term><term>Lignin (chemistry)</term><term>Magnetic Resonance Spectroscopy (methods)</term><term>Panicum (chemistry)</term><term>Phosphorus (chemistry)</term><term>Pinus (chemistry)</term><term>Populus (chemistry)</term><term>Tannins (analysis)</term><term>Tannins (chemistry)</term></keywords><keywords scheme="KwdFr" xml:lang="fr"><term>Lignine (analyse)</term><term>Lignine (composition chimique)</term><term>Panicum (composition chimique)</term><term>Phosphore (composition chimique)</term><term>Pinus (composition chimique)</term><term>Populus (composition chimique)</term><term>Spectroscopie par résonance magnétique (méthodes)</term><term>Tanins (analyse)</term><term>Tanins (composition chimique)</term></keywords><keywords scheme="MESH" type="chemical" qualifier="analysis" xml:lang="en"><term>Lignin</term><term>Tannins</term></keywords><keywords scheme="MESH" type="chemical" qualifier="chemistry" xml:lang="en"><term>Lignin</term><term>Phosphorus</term><term>Tannins</term></keywords><keywords scheme="MESH" qualifier="analyse" xml:lang="fr"><term>Lignine</term><term>Tanins</term></keywords><keywords scheme="MESH" qualifier="chemistry" xml:lang="en"><term>Panicum</term><term>Pinus</term><term>Populus</term></keywords><keywords scheme="MESH" qualifier="composition chimique" xml:lang="fr"><term>Lignine</term><term>Panicum</term><term>Phosphore</term><term>Pinus</term><term>Populus</term><term>Tanins</term></keywords><keywords scheme="MESH" qualifier="methods" xml:lang="en"><term>Magnetic Resonance Spectroscopy</term></keywords><keywords scheme="MESH" qualifier="méthodes" xml:lang="fr"><term>Spectroscopie par résonance magnétique</term></keywords></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">The analysis of chemical structural characteristics of biorefinery product streams (such as lignin and tannin) has advanced substantially over the past decade, with traditional wet-chemical techniques being replaced or supplemented by NMR methodologies. Quantitative <sup>31</sup>P NMR spectroscopy is a promising technique for the analysis of hydroxyl groups because of its unique characterization capability and broad potential applicability across the biorefinery research community. This protocol describes procedures for (i) the preparation/solubilization of lignin and tannin, (ii) the phosphitylation of their hydroxyl groups, (iii) NMR acquisition details, and (iv) the ensuing data analyses and means to precisely calculate the content of the different types of hydroxyl groups. Compared with traditional wet-chemical techniques, the technique of quantitative <sup>31</sup>P NMR spectroscopy offers unique advantages in measuring hydroxyl groups in a single spectrum with high signal resolution. The method provides complete quantitative information about the hydroxyl groups with small amounts of sample (~30 mg) within a relatively short experimental time (~30-120 min).</div></front></TEI><pubmed><MedlineCitation Status="MEDLINE" Owner="NLM"><PMID Version="1">31391578</PMID><DateCompleted><Year>2019</Year><Month>11</Month><Day>25</Day></DateCompleted><DateRevised><Year>2019</Year><Month>11</Month><Day>25</Day></DateRevised><Article PubModel="Print-Electronic"><Journal><ISSN IssnType="Electronic">1750-2799</ISSN><JournalIssue CitedMedium="Internet"><Volume>14</Volume><Issue>9</Issue><PubDate><Year>2019</Year><Month>09</Month></PubDate></JournalIssue><Title>Nature protocols</Title><ISOAbbreviation>Nat Protoc</ISOAbbreviation></Journal><ArticleTitle>Determination of hydroxyl groups in biorefinery resources via quantitative <sup>31</sup>P NMR spectroscopy.</ArticleTitle><Pagination><MedlinePgn>2627-2647</MedlinePgn></Pagination><ELocationID EIdType="doi" ValidYN="Y">10.1038/s41596-019-0191-1</ELocationID><Abstract><AbstractText>The analysis of chemical structural characteristics of biorefinery product streams (such as lignin and tannin) has advanced substantially over the past decade, with traditional wet-chemical techniques being replaced or supplemented by NMR methodologies. Quantitative <sup>31</sup>P NMR spectroscopy is a promising technique for the analysis of hydroxyl groups because of its unique characterization capability and broad potential applicability across the biorefinery research community. This protocol describes procedures for (i) the preparation/solubilization of lignin and tannin, (ii) the phosphitylation of their hydroxyl groups, (iii) NMR acquisition details, and (iv) the ensuing data analyses and means to precisely calculate the content of the different types of hydroxyl groups. Compared with traditional wet-chemical techniques, the technique of quantitative <sup>31</sup>P NMR spectroscopy offers unique advantages in measuring hydroxyl groups in a single spectrum with high signal resolution. The method provides complete quantitative information about the hydroxyl groups with small amounts of sample (~30 mg) within a relatively short experimental time (~30-120 min).</AbstractText></Abstract><AuthorList CompleteYN="Y"><Author ValidYN="Y"><LastName>Meng</LastName><ForeName>Xianzhi</ForeName><Initials>X</Initials><Identifier Source="ORCID">http://orcid.org/0000-0003-4303-3403</Identifier><AffiliationInfo><Affiliation>Department of Chemical and Biomolecular Engineering, The University of Tennessee, Knoxville, TN, USA.</Affiliation></AffiliationInfo></Author><Author ValidYN="Y"><LastName>Crestini</LastName><ForeName>Claudia</ForeName><Initials>C</Initials><Identifier Source="ORCID">http://orcid.org/0000-0001-9903-2675</Identifier><AffiliationInfo><Affiliation>Department of Molecular Science and Nanosystems, Ca' Foscari University of Venice, Venice, Italy. claudia.crestini@unive.it.</Affiliation></AffiliationInfo></Author><Author ValidYN="Y"><LastName>Ben</LastName><ForeName>Haoxi</ForeName><Initials>H</Initials><AffiliationInfo><Affiliation>State Key Laboratory of Bio-Fibers and Eco-Textiles, Qingdao University, Qingdao, China.</Affiliation></AffiliationInfo></Author><Author ValidYN="Y"><LastName>Hao</LastName><ForeName>Naijia</ForeName><Initials>N</Initials><AffiliationInfo><Affiliation>Department of Chemical and Biomolecular Engineering, The University of Tennessee, Knoxville, TN, USA.</Affiliation></AffiliationInfo></Author><Author ValidYN="Y"><LastName>Pu</LastName><ForeName>Yunqiao</ForeName><Initials>Y</Initials><Identifier Source="ORCID">http://orcid.org/0000-0003-2554-1447</Identifier><AffiliationInfo><Affiliation>Center for Bioenergy Innovation (CBI), Joint Institute for Biological Sciences, Biosciences Division, Oak Ridge National Laboratory (ORNL), Oak Ridge, TN, USA.</Affiliation></AffiliationInfo></Author><Author ValidYN="Y"><LastName>Ragauskas</LastName><ForeName>Arthur J</ForeName><Initials>AJ</Initials><Identifier Source="ORCID">http://orcid.org/0000-0002-3536-554X</Identifier><AffiliationInfo><Affiliation>Department of Chemical and Biomolecular Engineering, The University of Tennessee, Knoxville, TN, USA. aragausk@utk.edu.</Affiliation></AffiliationInfo><AffiliationInfo><Affiliation>Center for Bioenergy Innovation (CBI), Joint Institute for Biological Sciences, Biosciences Division, Oak Ridge National Laboratory (ORNL), Oak Ridge, TN, USA. aragausk@utk.edu.</Affiliation></AffiliationInfo><AffiliationInfo><Affiliation>Department of Forestry, Wildlife and Fisheries, Center of Renewable Carbon, The University of Tennessee Institute of Agriculture, Knoxville, TN, USA. aragausk@utk.edu.</Affiliation></AffiliationInfo></Author><Author ValidYN="Y"><LastName>Argyropoulos</LastName><ForeName>Dimitris S</ForeName><Initials>DS</Initials><Identifier Source="ORCID">http://orcid.org/0000-0003-1187-7919</Identifier><AffiliationInfo><Affiliation>Departments of Chemistry and Forest Biomaterials, North Carolina State University, Raleigh, NC, USA. dsargyro@ncsu.edu.</Affiliation></AffiliationInfo></Author></AuthorList><Language>eng</Language><PublicationTypeList><PublicationType UI="D016428">Journal Article</PublicationType><PublicationType UI="D013485">Research Support, Non-U.S. Gov't</PublicationType><PublicationType UI="D013486">Research Support, U.S. Gov't, Non-P.H.S.</PublicationType></PublicationTypeList><ArticleDate DateType="Electronic"><Year>2019</Year><Month>08</Month><Day>07</Day></ArticleDate></Article><MedlineJournalInfo><Country>England</Country><MedlineTA>Nat Protoc</MedlineTA><NlmUniqueID>101284307</NlmUniqueID><ISSNLinking>1750-2799</ISSNLinking></MedlineJournalInfo><ChemicalList><Chemical><RegistryNumber>0</RegistryNumber><NameOfSubstance UI="D013634">Tannins</NameOfSubstance></Chemical><Chemical><RegistryNumber>27YLU75U4W</RegistryNumber><NameOfSubstance UI="D010758">Phosphorus</NameOfSubstance></Chemical><Chemical><RegistryNumber>9005-53-2</RegistryNumber><NameOfSubstance UI="D008031">Lignin</NameOfSubstance></Chemical></ChemicalList><CitationSubset>IM</CitationSubset><MeshHeadingList><MeshHeading><DescriptorName UI="D008031" MajorTopicYN="N">Lignin</DescriptorName><QualifierName UI="Q000032" MajorTopicYN="Y">analysis</QualifierName><QualifierName UI="Q000737" MajorTopicYN="Y">chemistry</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D009682" MajorTopicYN="N">Magnetic Resonance Spectroscopy</DescriptorName><QualifierName UI="Q000379" MajorTopicYN="Y">methods</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D008897" MajorTopicYN="N">Panicum</DescriptorName><QualifierName UI="Q000737" MajorTopicYN="N">chemistry</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D010758" MajorTopicYN="N">Phosphorus</DescriptorName><QualifierName UI="Q000737" MajorTopicYN="N">chemistry</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D028223" MajorTopicYN="N">Pinus</DescriptorName><QualifierName UI="Q000737" MajorTopicYN="N">chemistry</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D032107" MajorTopicYN="N">Populus</DescriptorName><QualifierName UI="Q000737" MajorTopicYN="N">chemistry</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D013634" MajorTopicYN="N">Tannins</DescriptorName><QualifierName UI="Q000032" MajorTopicYN="N">analysis</QualifierName><QualifierName UI="Q000737" MajorTopicYN="N">chemistry</QualifierName></MeshHeading></MeshHeadingList></MedlineCitation><PubmedData><History><PubMedPubDate PubStatus="received"><Year>2019</Year><Month>02</Month><Day>04</Day></PubMedPubDate><PubMedPubDate PubStatus="accepted"><Year>2019</Year><Month>05</Month><Day>09</Day></PubMedPubDate><PubMedPubDate 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Meng</name></region><name sortKey="Argyropoulos, Dimitris S" sort="Argyropoulos, Dimitris S" uniqKey="Argyropoulos D" first="Dimitris S" last="Argyropoulos">Dimitris S. Argyropoulos</name><name sortKey="Hao, Naijia" sort="Hao, Naijia" uniqKey="Hao N" first="Naijia" last="Hao">Naijia Hao</name><name sortKey="Pu, Yunqiao" sort="Pu, Yunqiao" uniqKey="Pu Y" first="Yunqiao" last="Pu">Yunqiao Pu</name><name sortKey="Ragauskas, Arthur J" sort="Ragauskas, Arthur J" uniqKey="Ragauskas A" first="Arthur J" last="Ragauskas">Arthur J. Ragauskas</name><name sortKey="Ragauskas, Arthur J" sort="Ragauskas, Arthur J" uniqKey="Ragauskas A" first="Arthur J" last="Ragauskas">Arthur J. Ragauskas</name><name sortKey="Ragauskas, Arthur J" sort="Ragauskas, Arthur J" uniqKey="Ragauskas A" first="Arthur J" last="Ragauskas">Arthur J. Ragauskas</name></country><country name="Italie"><noRegion><name sortKey="Crestini, Claudia" sort="Crestini, Claudia" uniqKey="Crestini C" first="Claudia" last="Crestini">Claudia Crestini</name></noRegion></country><country name="République populaire de Chine"><noRegion><name sortKey="Ben, Haoxi" sort="Ben, Haoxi" uniqKey="Ben H" first="Haoxi" last="Ben">Haoxi Ben</name></noRegion></country></tree></affiliations></record>Pour manipuler ce document sous Unix (Dilib)
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