Development of a rapid method for the quantification of cellulose in tobacco by ~(13)C CP/MAS NMR
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- 英文论文题名：Development of a rapid method for the quantification of cellulose in tobacco by ~(13)C CP/MAS NMR
- 论文作者：Jinhui Jiang ; Yonghua Hu ; Zhenfeng Tian ; Kaibo Chen ; Shaolin Ge ; Yingbo Xu ; Dong Tian ; Jun Yang
- 英文论文作者：Jinhui Jiang ; Yonghua Hu ; Zhenfeng Tian ; Kaibo Chen ; Shaolin Ge ; Yingbo Xu ; Dong Tian ; Jun Yang ; Department of Chemistry ; University of Science and Technology of China ; Anhui Key Laboratory of Tobacco Chemistry ; Technology Center ; China Tobacco Anhui Industrial CO. ; LTD
- 年：2016
- 作者机构：Department of Chemistry, University of Science and Technology of China;Anhui Key Laboratory of Tobacco Chemistry, Technology Center, China Tobacco Anhui Industrial CO.,LTD;
- 英文论文关键词：Cellulose ; ~(13) CP/MAS NMR ; Spectral deconvolution ; Tobacco
- 会议召开时间：2016-12-01
- 会议录名称：中国烟草学会2016年度优秀论文汇编——烟草工业主题
- 语种：英文
- 分类号：TS47
- 学会代码：ZGYG
- 学会名称：中国烟草学会
- 页数：18
- 文件大小：864k
- 原文格式：D
摘要
A method was developed for rapid quantitative determination of cellulose in tobacco by utilizing ~(13)C cross polarization magic angle spinning NMR spectroscopy(~(13)C CP/MAS NMR). Sample powder was loaded into NMR rotor, which was customized rotor containing a matched silicon tube as an intensity reference. ~(13)C CP/MAS NMR spectra of tobacco samples were processed with spectral deconvolution to obtain the area of the C-1 resonance at 105.5 ppm and the internal standard at 0 ppm. The ratio between the area of 105.5 ppm and 0 ppm of a set of standard cellulose samples was used to construct a calibration curve. The cellulose content of a tobacco sample was determined by comparison of the ratio between the area of 105.5 ppm and 0 ppm to the calibration curve. Results of this developed method showed good agreement with those obtained from chemical analysis. The proposed method has such advantages of accuracy, quickness and efficiency, and could be an alternative to chemical analyses of cellulose.
A method was developed for rapid quantitative determination of cellulose in tobacco by utilizing ~(13)C cross polarization magic angle spinning NMR spectroscopy(~(13)C CP/MAS NMR). Sample powder was loaded into NMR rotor, which was customized rotor containing a matched silicon tube as an intensity reference. ~(13)C CP/MAS NMR spectra of tobacco samples were processed with spectral deconvolution to obtain the area of the C-1 resonance at 105.5 ppm and the internal standard at 0 ppm. The ratio between the area of 105.5 ppm and 0 ppm of a set of standard cellulose samples was used to construct a calibration curve. The cellulose content of a tobacco sample was determined by comparison of the ratio between the area of 105.5 ppm and 0 ppm to the calibration curve. Results of this developed method showed good agreement with those obtained from chemical analysis. The proposed method has such advantages of accuracy, quickness and efficiency, and could be an alternative to chemical analyses of cellulose.
A method was developed for rapid quantitative determination of cellulose in tobacco by utilizing ~(13)C cross polarization magic angle spinning NMR spectroscopy(~(13)C CP/MAS NMR). Sample powder was loaded into NMR rotor, which was customized rotor containing a matched silicon tube as an intensity reference. ~(13)C CP/MAS NMR spectra of tobacco samples were processed with spectral deconvolution to obtain the area of the C-1 resonance at 105.5 ppm and the internal standard at 0 ppm. The ratio between the area of 105.5 ppm and 0 ppm of a set of standard cellulose samples was used to construct a calibration curve. The cellulose content of a tobacco sample was determined by comparison of the ratio between the area of 105.5 ppm and 0 ppm to the calibration curve. Results of this developed method showed good agreement with those obtained from chemical analysis. The proposed method has such advantages of accuracy, quickness and efficiency, and could be an alternative to chemical analyses of cellulose.
引文
Abidi,N.,Cabrales,L.,&Haigler,C.H.(2014).Changes in the cell wall and cellulose content of developing cotton fibers investigated by FTIR spectroscopy.Carbohydrate polymers,100,9-16.
Agarwal,U.P.,Reiner,R.S.,&Ralph,S.A.(2010).Cellulose I crystallinity determination using FT-Raman spectroscopy:univariate and multivariate methods.Cellulose,17(4),721-733.
Alesiani,M.,Proietti,F.,Capuani,S.,Paci,M.,Fioravanti,M.,&Maraviglia,B.(2005).13C CPMASNMR spectroscopic analysis applied to wood characterization.Applied Magnetic Resonance,29(2),177-184.
Atalla,R.H.,Gast,J.C.,Sindorf,D.W.,Bartuska,V.J.,&Maciel,G.E.(1980).Carbon-13 NMRspectra of cellulose polymorphs.Journal of the American Chemical Society,102(9),3249-3251.
Bergbreiter,D.,&Srinivas,B.(1992).PEAKFIT-VERSION 3.01.(Vol.114,pp.7961-7962):AMERCHEMICAL SOC 1155 16TH ST,NW,WASHINGTON,DC 20036.
Bokelman,G.H.,Ryan Jr,W.S.,&Oakley,E.T.(1983).Fractionation of Bright tobacco.Journal of Agricultural and Food Chemistry,31(4),897-901.
Downes,G.M.,Meder,R.,Ebdon,N.,Bond,H.,Evans,R.,Joyce,K.,&Southerton,S.(2010).Radial variation in cellulose content and Kraft pulp yield in Eucalyptus nitens using near-infrared spectral analysis of air-dry wood surfaces.Journal of Near Infrared Spectroscopy,18(2),147.
Foust,T.D.,Aden,A.,Dutta,A.,&Phillips,S.(2009).An economic and environmental comparison of a biochemical and a thermochemical lignocellulosic ethanol conversion processes.Cellulose,16(4),547-565.
Franz,J.,Garcia,R.,Linehan,J.,Love,G.,&Snape,C.(1992).Single-pulse excitation carbon-13 NMRmeasurements on the Argonne premium coal samples.Energy&fuels,6(5),598-602.
French,A.D.,&Cintrón,M.S.(2013).Cellulose polymorphy,crystallite size,and the Segal crystallinity index.Cellulose,20(1),583-588.
Habibi,Y.,Lucia,L.A.,&Rojas,O.J.(2010).Cellulose nanocrystals:chemistry,self-assembly,and applications.Chemical reviews,110(6),3479-3500.
Hall,R.A.,Jurkiewicz,A.,&Maciel,G.E.(1993).A bicyclic ketone as a solid-state carbon-13 NMRintensity reference.Analytical chemistry,65(5),534-538.
Hall,R.A.,&Wooten,J.B.(1998).Quantitative analysis of cellulose in tobacco by 13C CPMAS NMR.Journal of Agricultural and Food Chemistry,46(4),1423-1427.
Hartmann,S.,&Hahn,E.(1962).Nuclear double resonance in the rotating frame.Physical Review,128(5),2042.
He,W.,&Hu,H.(2013).Prediction of hot-water-soluble extractive,pentosan and cellulose content of various wood species using FT-NIR spectroscopy.Bioresource technology,140,299-305.
Henniges,U.,Veigel,S.,Lems,E.-M.,Bauer,A.,Keckes,J.,Pinkl,S.,&Gindl-Altmutter,W.(2014).Microfibrillated cellulose and cellulose nanopaper from Miscanthus biogas production residue.Cellulose,21(3),1601-1610.
Holtman,K.M.,Chen,N.,Chappell,M.A.,Kadla,J.F.,Xu,L.,&Mao,J.(2010).Chemical structure and heterogeneity differences of two lignins from loblolly pine as investigated by advanced solidstate NMR spectroscopy.Journal of Agricultural and Food Chemistry,58(18),9882-9892.
Hou,G.,Deng,F.,Ding,S.,Fu,R.,Yang,J.,&Ye,C.(2006).Quantitative cross-polarization NMRspectroscopy in uniformly 13 C-labeled solids.Chemical physics letters,421(4),356-360.
Jurkiewicz,A.,&Maciel,G.E.(1995).13C NMR spin-lattice relaxation properties and quantitative analytical methodology of 13C NMR spectroscopy for coals.Analytical chemistry,67(13),2188-2194.
Kao,H.-M.,Lee,L.-P.,&Palani,A.(2008).13C CPMAS NMR spectroscopy as a versatile and quantitative tool for determination of mercury adsorption capacity in thiol-functionalized mesoporous silica SBA-1.Analytical chemistry,80(8),3016-3019.
Keeler,C.,&Maciel,G.E.(2003).Quantitation in the solid-state 13C NMR analysis of soil and organic soil fractions.Analytical chemistry,75(10),2421-2432.
Laage,S.,Marchetti,A.,Sein,J.,Pierattelli,R.,Sass,H.J.,Grzesiek,S.,Lesage,A.,Pintacuda,G.,&Emsley,L.(2008).Band-Selective 1H-13C Cross-Polarization in fast magic angle spinning solidstate NMR spectroscopy.Journal of the American Chemical Society,130(51),17216-17217.
Maciel,G.E.(1984).High-resolution nuclear magnetic resonance of solids.Science,226(4672),282-288.
Muntean,J.V.,&Stock,L.M.(1991).Bloch decay solid-state carbon-13 NMR spectroscopy of the samarium iodide-treated Argonne Premium coals.Energy&fuels,5(5),765-767.
Pan,Z.,Sun,D.,Sun,J.,Zhou,Z.,Jia,Y.,Pang,B.,Ma,Z.,&Du,X.(2010).Effects of fiber wax and cellulose content on colored cotton fiber quality.Euphytica,173(2),141-149.
Paoli,M.,Bighelli,A.,Castola,V.,Tomi,F.,&Casanova,J.(2013).Quantification of taxanes in a leaf and twig extract from Taxus baccata L.using 13C NMR spectroscopy.Magnetic Resonance in Chemistry,51(11),756-761.
Schaefer,J.,&Stejskal,E.(1976).Carbon-13 nuclear magnetic resonance of polymers spinning at the magic angle.Journal of the American Chemical Society,98(4),1031-1032.
Sievers,C.,Marzialetti,T.,Hoskins,T.J.,Olarte,M.B.V.,Agrawal,P.K.,&Jones,C.W.(2009).Quantitative solid state NMR analysis of residues from acid hydrolysis of loblolly pine wood.Bioresource technology,100(20),4758-4765.
Smernik,R.J.,&Oades,J.M.(2000).The use of spin counting for determining quantitation in solid state13 C NMR spectra of natural organic matter:1.Model systems and the effects of paramagnetic impurities.Geoderma,96(1),101-129.
Song,J.,Ge,H.,Xu,M.,Chen,Q.,&Zhang,L.(2014).Study on the interaction between urea and cellulose by combining solid-state 13C CP/MAS NMR and extended Hückel charges.Cellulose,21(6),4019-4027.
Stejskal,E.O.,Schaefer,J.,&Waugh,J.S.(1977).Magic-angle spinning and polarization transfer in proton-enhanced NMR.Journal of Magnetic Resonance,28(1),105-112.
Takeda,K.,Noda,Y.,Takegoshi,K.,Lafon,O.,Trébosc,J.,&Amoureux,J.-P.(2012).Quantitative cross-polarization at magic-angle spinning frequency of about 20k Hz.Journal of Magnetic Resonance,214,340-345.
Tan,I.,Flanagan,B.M.,Halley,P.J.,Whittaker,A.K.,&Gidley,M.J.(2007).A method for estimating the nature and relative proportions of amorphous,single,and double-helical components in starch granules by 13C CP/MAS NMR.Biomacromolecules,8(3),885-891.
Van Soest,P.J.,&Robertson,J.(1985).Analysis of forages and fibrous foods.Cornell University.
Virtanen,T.,&Maunu,S.L.(2014).NMR spectroscopic studies on dissolution of softwood pulp with enhanced reactivity.Cellulose,21(1),153-165.
Wang,H.,Gurau,G.,&Rogers,R.D.(2012).Ionic liquid processing of cellulose.Chemical Society Reviews,41(4),1519-1537.
Wickholm,K.,Hult,E.-L.,Larsson,P.T.,Iversen,T.,&Lennholm,H.(2001).Quantification of cellulose forms in complex cellulose materials:a chemometric model.Cellulose,8(2),139-148.
Wickramasinghe,N.P.,&Ishii,Y.(2006).Sensitivity enhancement,assignment,and distance measurement in 13 C solid-state NMR spectroscopy for paramagnetic systems under fast magic angle spinning.Journal of Magnetic Resonance,181(2),233-243.
Xiong,B.,Zhao,P.,Cai,P.,Zhang,L.,Hu,K.,&Cheng,G.(2013).NMR spectroscopic studies on the mechanism of cellulose dissolution in alkali solutions.Cellulose,20(2),613-621.
Zhu,X.,Liu,B.,Zheng,S.,&Gao,Y.(2014).Quantitative and structure analysis of pectin in tobacco by13 C CP/MAS NMR spectroscopy.Analytical Methods,6(16),6407-6413.
Agarwal,U.P.,Reiner,R.S.,&Ralph,S.A.(2010).Cellulose I crystallinity determination using FT-Raman spectroscopy:univariate and multivariate methods.Cellulose,17(4),721-733.
Alesiani,M.,Proietti,F.,Capuani,S.,Paci,M.,Fioravanti,M.,&Maraviglia,B.(2005).13C CPMASNMR spectroscopic analysis applied to wood characterization.Applied Magnetic Resonance,29(2),177-184.
Atalla,R.H.,Gast,J.C.,Sindorf,D.W.,Bartuska,V.J.,&Maciel,G.E.(1980).Carbon-13 NMRspectra of cellulose polymorphs.Journal of the American Chemical Society,102(9),3249-3251.
Bergbreiter,D.,&Srinivas,B.(1992).PEAKFIT-VERSION 3.01.(Vol.114,pp.7961-7962):AMERCHEMICAL SOC 1155 16TH ST,NW,WASHINGTON,DC 20036.
Bokelman,G.H.,Ryan Jr,W.S.,&Oakley,E.T.(1983).Fractionation of Bright tobacco.Journal of Agricultural and Food Chemistry,31(4),897-901.
Downes,G.M.,Meder,R.,Ebdon,N.,Bond,H.,Evans,R.,Joyce,K.,&Southerton,S.(2010).Radial variation in cellulose content and Kraft pulp yield in Eucalyptus nitens using near-infrared spectral analysis of air-dry wood surfaces.Journal of Near Infrared Spectroscopy,18(2),147.
Foust,T.D.,Aden,A.,Dutta,A.,&Phillips,S.(2009).An economic and environmental comparison of a biochemical and a thermochemical lignocellulosic ethanol conversion processes.Cellulose,16(4),547-565.
Franz,J.,Garcia,R.,Linehan,J.,Love,G.,&Snape,C.(1992).Single-pulse excitation carbon-13 NMRmeasurements on the Argonne premium coal samples.Energy&fuels,6(5),598-602.
French,A.D.,&Cintrón,M.S.(2013).Cellulose polymorphy,crystallite size,and the Segal crystallinity index.Cellulose,20(1),583-588.
Habibi,Y.,Lucia,L.A.,&Rojas,O.J.(2010).Cellulose nanocrystals:chemistry,self-assembly,and applications.Chemical reviews,110(6),3479-3500.
Hall,R.A.,Jurkiewicz,A.,&Maciel,G.E.(1993).A bicyclic ketone as a solid-state carbon-13 NMRintensity reference.Analytical chemistry,65(5),534-538.
Hall,R.A.,&Wooten,J.B.(1998).Quantitative analysis of cellulose in tobacco by 13C CPMAS NMR.Journal of Agricultural and Food Chemistry,46(4),1423-1427.
Hartmann,S.,&Hahn,E.(1962).Nuclear double resonance in the rotating frame.Physical Review,128(5),2042.
He,W.,&Hu,H.(2013).Prediction of hot-water-soluble extractive,pentosan and cellulose content of various wood species using FT-NIR spectroscopy.Bioresource technology,140,299-305.
Henniges,U.,Veigel,S.,Lems,E.-M.,Bauer,A.,Keckes,J.,Pinkl,S.,&Gindl-Altmutter,W.(2014).Microfibrillated cellulose and cellulose nanopaper from Miscanthus biogas production residue.Cellulose,21(3),1601-1610.
Holtman,K.M.,Chen,N.,Chappell,M.A.,Kadla,J.F.,Xu,L.,&Mao,J.(2010).Chemical structure and heterogeneity differences of two lignins from loblolly pine as investigated by advanced solidstate NMR spectroscopy.Journal of Agricultural and Food Chemistry,58(18),9882-9892.
Hou,G.,Deng,F.,Ding,S.,Fu,R.,Yang,J.,&Ye,C.(2006).Quantitative cross-polarization NMRspectroscopy in uniformly 13 C-labeled solids.Chemical physics letters,421(4),356-360.
Jurkiewicz,A.,&Maciel,G.E.(1995).13C NMR spin-lattice relaxation properties and quantitative analytical methodology of 13C NMR spectroscopy for coals.Analytical chemistry,67(13),2188-2194.
Kao,H.-M.,Lee,L.-P.,&Palani,A.(2008).13C CPMAS NMR spectroscopy as a versatile and quantitative tool for determination of mercury adsorption capacity in thiol-functionalized mesoporous silica SBA-1.Analytical chemistry,80(8),3016-3019.
Keeler,C.,&Maciel,G.E.(2003).Quantitation in the solid-state 13C NMR analysis of soil and organic soil fractions.Analytical chemistry,75(10),2421-2432.
Laage,S.,Marchetti,A.,Sein,J.,Pierattelli,R.,Sass,H.J.,Grzesiek,S.,Lesage,A.,Pintacuda,G.,&Emsley,L.(2008).Band-Selective 1H-13C Cross-Polarization in fast magic angle spinning solidstate NMR spectroscopy.Journal of the American Chemical Society,130(51),17216-17217.
Maciel,G.E.(1984).High-resolution nuclear magnetic resonance of solids.Science,226(4672),282-288.
Muntean,J.V.,&Stock,L.M.(1991).Bloch decay solid-state carbon-13 NMR spectroscopy of the samarium iodide-treated Argonne Premium coals.Energy&fuels,5(5),765-767.
Pan,Z.,Sun,D.,Sun,J.,Zhou,Z.,Jia,Y.,Pang,B.,Ma,Z.,&Du,X.(2010).Effects of fiber wax and cellulose content on colored cotton fiber quality.Euphytica,173(2),141-149.
Paoli,M.,Bighelli,A.,Castola,V.,Tomi,F.,&Casanova,J.(2013).Quantification of taxanes in a leaf and twig extract from Taxus baccata L.using 13C NMR spectroscopy.Magnetic Resonance in Chemistry,51(11),756-761.
Schaefer,J.,&Stejskal,E.(1976).Carbon-13 nuclear magnetic resonance of polymers spinning at the magic angle.Journal of the American Chemical Society,98(4),1031-1032.
Sievers,C.,Marzialetti,T.,Hoskins,T.J.,Olarte,M.B.V.,Agrawal,P.K.,&Jones,C.W.(2009).Quantitative solid state NMR analysis of residues from acid hydrolysis of loblolly pine wood.Bioresource technology,100(20),4758-4765.
Smernik,R.J.,&Oades,J.M.(2000).The use of spin counting for determining quantitation in solid state13 C NMR spectra of natural organic matter:1.Model systems and the effects of paramagnetic impurities.Geoderma,96(1),101-129.
Song,J.,Ge,H.,Xu,M.,Chen,Q.,&Zhang,L.(2014).Study on the interaction between urea and cellulose by combining solid-state 13C CP/MAS NMR and extended Hückel charges.Cellulose,21(6),4019-4027.
Stejskal,E.O.,Schaefer,J.,&Waugh,J.S.(1977).Magic-angle spinning and polarization transfer in proton-enhanced NMR.Journal of Magnetic Resonance,28(1),105-112.
Takeda,K.,Noda,Y.,Takegoshi,K.,Lafon,O.,Trébosc,J.,&Amoureux,J.-P.(2012).Quantitative cross-polarization at magic-angle spinning frequency of about 20k Hz.Journal of Magnetic Resonance,214,340-345.
Tan,I.,Flanagan,B.M.,Halley,P.J.,Whittaker,A.K.,&Gidley,M.J.(2007).A method for estimating the nature and relative proportions of amorphous,single,and double-helical components in starch granules by 13C CP/MAS NMR.Biomacromolecules,8(3),885-891.
Van Soest,P.J.,&Robertson,J.(1985).Analysis of forages and fibrous foods.Cornell University.
Virtanen,T.,&Maunu,S.L.(2014).NMR spectroscopic studies on dissolution of softwood pulp with enhanced reactivity.Cellulose,21(1),153-165.
Wang,H.,Gurau,G.,&Rogers,R.D.(2012).Ionic liquid processing of cellulose.Chemical Society Reviews,41(4),1519-1537.
Wickholm,K.,Hult,E.-L.,Larsson,P.T.,Iversen,T.,&Lennholm,H.(2001).Quantification of cellulose forms in complex cellulose materials:a chemometric model.Cellulose,8(2),139-148.
Wickramasinghe,N.P.,&Ishii,Y.(2006).Sensitivity enhancement,assignment,and distance measurement in 13 C solid-state NMR spectroscopy for paramagnetic systems under fast magic angle spinning.Journal of Magnetic Resonance,181(2),233-243.
Xiong,B.,Zhao,P.,Cai,P.,Zhang,L.,Hu,K.,&Cheng,G.(2013).NMR spectroscopic studies on the mechanism of cellulose dissolution in alkali solutions.Cellulose,20(2),613-621.
Zhu,X.,Liu,B.,Zheng,S.,&Gao,Y.(2014).Quantitative and structure analysis of pectin in tobacco by13 C CP/MAS NMR spectroscopy.Analytical Methods,6(16),6407-6413.
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