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Development of an analysis method for determination of pectin in tobacco by solid state 13C CP/MAS NMR

  • 1.

    Department of Chemistry, University of Science and Technology of China, Hefei 230026, China

  • 2.

    Technology Center, China Tobacco Fujian Industrial Co., Ltd., Xiamen 361001, China

Cite this:
https://doi.org/10.52396/JUST-2021-0106
  • Received Date: 11 April 2021
  • Rev Recd Date: 27 May 2021
  • Publish Date: 31 August 2021
    Abstract

  • Abstract

    A quantitative analysis method was developed for determination of pectin content in tobacco samples by solid state 13C CP/MAS NMR. A 5.5 mm outer diameter of dimethyl silicone rubber tubing was designed and utilized as a reference of intensity, which was packed into a 5.5 mm inner diameter zirconia NMR rotor to construct an NMR sample tubing. The powder samples filled into the sample tubing were detected to obtain 13C CP/MAS NMR spectra. The peak of C-6 at 171 ppm was processed with spectral deconvolution to eliminate interference from overlapping peaks. The calibration curve was established with the area ratios of assigned C-6 peak to intensity reference peak and the mass of the polygalacturonic acid (PGA). This method was used to determine the pectin content in six different tobacco samples. Relative errors were between -4.94% and 3.84% compared with the results measured by the standard method. The recovery of PGA from spiked tobacco samples was ranged from 94.33% to 102.77%, the RSD (n=5) was less than 2.32%. It demonstrates that the 13C CP/MAS NMR method with a novel intensity reference possesses the properties of speediness, accuracy and simplicity, which is suitable for the quantitative analysis of pectin content in tobacco.

    Abstract

    A quantitative analysis method was developed for determination of pectin content in tobacco samples by solid state 13C CP/MAS NMR. A 5.5 mm outer diameter of dimethyl silicone rubber tubing was designed and utilized as a reference of intensity, which was packed into a 5.5 mm inner diameter zirconia NMR rotor to construct an NMR sample tubing. The powder samples filled into the sample tubing were detected to obtain 13C CP/MAS NMR spectra. The peak of C-6 at 171 ppm was processed with spectral deconvolution to eliminate interference from overlapping peaks. The calibration curve was established with the area ratios of assigned C-6 peak to intensity reference peak and the mass of the polygalacturonic acid (PGA). This method was used to determine the pectin content in six different tobacco samples. Relative errors were between -4.94% and 3.84% compared with the results measured by the standard method. The recovery of PGA from spiked tobacco samples was ranged from 94.33% to 102.77%, the RSD (n=5) was less than 2.32%. It demonstrates that the 13C CP/MAS NMR method with a novel intensity reference possesses the properties of speediness, accuracy and simplicity, which is suitable for the quantitative analysis of pectin content in tobacco.
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    • References(50)
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    Huang Y C, Wu H C, Wang Y D, et al. Pectin methylesterase34 contributes to heat tolerance through its role in promoting stomatal movement. Plant Physiol., 2017, 174 (2):748-763.
    [2]
    Baum A, Dominiak M, Vidal-Melgosa S, et al. Prediction of pectin yield and quality by FTIR and carbohydrate microarray analysis. Food Bioprocess Technol., 2017, 10 (1):143-154.
    [3]
    Grassino A N, Barba F J, Brnčić M, et al. Analytical tools used for the identification and quantification of pectin extracted from plant food matrices, wastes and by-products: A review. Food Chem., 2018, 266:47-55.
    [4]
    Lopez-Sanchez P, Martinez-Sanz M, Bonilla M R, et al. Nanostructure and poroviscoelasticity in cell wall materials from onion, carrot and apple: Roles of pectin. Food Hydrocoll., 2020, 98:105253.
    [5]
    Bagherian H, Ashtiani F Z, Fouladitajar A, et al. Comparisons between conventional, microwave- and ultrasound-assisted methods for extraction of pectin from grapefruit. Chem. Eng. Process., 2011, 50 (11/12): 1237-1243.
    [6]
    Naqash F, Masoodi F A, Rather S A, et al. Emerging concepts in the nutraceutical and functional properties of pectin—A Review. Carbohyd. Polym., 2017, 168:227-239.
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    Tyagi V, Sharma P, Malviya R. Pectins and their role in food and pharmaceutical industry: A review. J. Chronother. Drug Deliv., 2015, 6:65-77.
    [8]
    Jafari F, Khodaiyan F, Kiani H, et al. Pectin from carrot pomace: Optimization of extraction and physicochemical properties. Carbohyd. Polym., 2017, 157:1315-1322.
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    Kyomugasho C, Christiaens S, Shpigelman A, et al. FT-IR spectroscopy, a reliable method for routine analysis of the degree of methylesterification of pectin in different fruit- and vegetable-based matrices. Food Chem.,2015, 176:82-90.
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    Rao W, Tuo S, Zhong K, et al. Research progress on extraction and analysis of pectin in tobacco. Guangzhou Chem., 2009, 34 (1):71-77.
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    Zhou S, Xu Y, Wang C, et al. Pyrolysis behavior of pectin under the conditions that simulate cigarette smoking. J. Anal. Appl. Pyrolysis., 2011, 91:232-240.
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    Yang J, Ding H, Yu G, et al. Determination of pectin content in reconstituted tobacco by carbazole colorimetry.Chin. J. Anal. Lab., 2012, 31 (6):100-102.
    [13]
    Xu Z Q, Chen K B, Cai B, et al. Determination of pectin content in tobacco by enzymatic hydrolysis-flow analysis method.Tobacco Sci. Technol., 2005, 9:26-28.
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    Rao W, Tuo S, Zhong K, et al. Determination of pectin in tobacco by enzymatic hydrolysis-ion chromatography. Chem. Res., 2010, 21 (3):72-74.
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    Tinmanee R, Larsen S C, Morris K R, et al. Quantification of gabapentin polymorphs in gabapentin/excipient mixtures using solid state 13C NMR spectroscopy and X-ray powder diffraction. J. Pharm. Biomed. Anal., 2017, 146:29-36.
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    Christiansen S C, Hedin N, Epping J D, et al. Sensitivity considerations in polarization transfer and filtering using dipole-dipole couplings: Implications for biomineral systems. Solid State Nucl. Mag., 2006, 29 :170-182.
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    Hartmann S R, Hahn E L. Nuclear double resonance in the rotating frame. Phys. Rev., 1962, 128 (5):2042-2953.
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    Schaefer J, Stejskal E O. Carbon-13 nuclear magnetic resonance of polymers spinning at the magic angle. J. Am. Chem. Soc., 1976,98 (4):1031-1032.
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    Haslinger S, Hietala S, Hummel M, et al. Solid-state NMR method for the quantification of cellulose and polyester in textile blends. Carbohyd. Polym., 2019, 207:11-16.
    [20]
    Fu L, McCallum S A, Miao J, et al. Rapid and accurate determination of the lignin content of lignocellulosic biomass by solid-state NMR. Fuel, 2015, 141:39-45.
    [21]
    Nurdjanah S, Hook J, Paton J, et al. Galacturonic acid content and degree of esterification of pectin from sweet potato starch residue detected using 13C CP/MAS solid state NMR. Eur. J. Food Res. Rev., 2013, 3(1):16-37.
    [22]
    Zhu X, Liu B, Zheng S, et al. Quantitative and structure analysis of pectin in tobacco by 13C CP/MAS NMR spectroscopy. Anal. Methods, 2014, 6 (16):6407-6413.
    [23]
    Giraudeau P, Tea I, Remaud G S, et al. Reference and normalization methods: Essential tools for the intercomparison of NMR spectra. J. Pharm. Biomed. Anal., 2014, 93:3-16.
    [24]
    Hall R A, Jurkiewicz A, Maciel G E. A bicyclic ketone as a solid-state carbon-13 NMR intensity reference. Anal. Chem., 1993, 65 (5):534-538.
    [25]
    Muntean J V, Stock L M. Bloch decay solid-state carbon-13 NMR spectroscopy of the samarium iodide-treated Argonne Premium coals. Energy Fuels, 1991, 5:765-767.
    [26]
    Zhang J, Giotto M V, Wen W Y, et al. An NMR study of the state of ions and diffusion in perfluorosulfonate ionomer. J. Membrane Sci.,2006, 269 (1/2):118-125.
    [27]
    Jurkiewicz A, Maciel G E. 13C NMR spin-lattice relaxation properties and quantitative analytical methodology of 13C NMR spectroscopy for coals. Anal. Chem., 1995, 67(13):2188-2194.
    [28]
    Gao X, Laskar D D, Zeng J, et al. A 13C CP/MAS-based nondegradative method for lignin content analysis. ACS Sustain. Chem. Eng., 2015, 3 (1):153-162.
    [29]
    Hall R A, Wooten J B. Quantitative analysis of cellulose in tobacco by 13C CPMAS NMR.J. Agric. Food Chem., 1998, 46:1423-1427.
    [30]
    Keeler C, Maciel G E. Quantitation in the solid-state 13C NMR analysis of soil and organic soil fractions. Anal. Chem., 2003, 75:2421-2432.
    [31]
    Pang R L, Zhang Q L, Guo L L, et al. Study on the colorimetry determination conditions of pectin in fruits and derived products. J. Fruit Sci., 2012, 29 (1):302-307.
    [32]
    Jarvis M C, Apperley D C. Chain conformation in concentrated pectic gels: Evidence from 13C NMR. Carbohyd. Res., 1995, 275 (1):131-145.
    [33]
    Westerlund E, Aman P, Andersson R E, et al. Investigation of the distribution of methyl ester groups in pectin by high-field 13C NMR. Carbohyd. Polym., 1991, 14:179-187.
    [34]
    Sinitsya A, Copikova J, Pavlikova H. 13C CP/MAS NMR spectroscopy in the analysis of pectins. J. Carbohydr. Chem.,1998, 17 (2):279-292.
    [35]
    Synytsya A, Copikova J, Brus J. 13C CP/MAS NMR spectra of pectins: A peak-fitting analysis in the C-6 region. Czech J. Food Sci., 2003, 21:1-12.
    [36]
    Wang T, Park Y B, Cosgrove D J, et al. Cellulose-pectin spatial contacts are inherent to never-dried arabidopsis primary cell walls: Evidence from solid-state nulear magnetic resonance. Plant Physiol., 2015, 168:871-884.
    [37]
    Phyo P, Wang T, Kiemle S N, et al. Gradients in wall mechanics and polysaccharides along growing inflorescence stems. Plant Physiol., 2017, 175:1593-1607.
    [38]
    Seger M R, Maciel G E. Quantitative 13C NMR analysis of sequence distributions in poly(ethylene-co-1-hexene). Anal. Chem., 2004, 76:5734-5747.
    [39]
    Mao J D, Schmidt-Rohr K. Accurate quantification of aromaticity and nonprotonated aromatic carbon fraction in natural organic matter by 13C solid-state nuclear magnetic resonance. Environ.Sci. Technol., 2004, 38: 2680-2684.
    [40]
    Mao J, Cao X, Olk D C, et al. Advanced solid-state NMR spectroscopy of natural organic matter. Prog. Nucl. Magn. Reson. Spectrosc., 2017, 100:17-51.
    [41]
    Johnson R L, Schmidt-Rohr K. Quantitative solid-state 13C NMR with signal enhancement by multiple cross polarization. J. Magn. Reson.,2014, 239:44-49.
    [42]
    Duan P, Schmidt-Rohr K. Composite-pulse and partially dipolar dephased multiCP for improved quantitative solid-state 13C NMR. J. Magn. Reson., 2017, 285:68-78.
    [43]
    Smernik R J, Oades J M. The use of spin counting for determining quantitation in solid state 13C NMR spectra of natural organic matter: 1. Model systems and the effects of paramagnetic impurities. Geoderma, 2000, 96: 101-129.
    [44]
    Wong S, Hanna J V, King S, et al. Fractionation of natural organic matter in drinking water and characterization by 13C cross-polarization magic-angle spinning NMR spectroscopy and size exclusion chromatography. Environ. Sci. Technol., 2002, 36 (16):3497-3503.
    [45]
    Alesiani M, Proietti F, Capuani S, et al. 13C CP/MAS NMR spectroscopic analysis applied to wood characterization. Appl. Magn. Reson., 2005, 29 (2):177-184.
    [46]
    Jiang J, Hu Y, Tian Z, et al. Development of a rapid method for the quantification of cellulose in tobacco by 13C CP/MAS NMR. Carbohyd. Polym., 2016, 135:121-127.
    [47]
    Zhang M, Maciel G E. Built-in carbon-13 intensity reference for solid-state analysis by magic-angle-spinning nuclear magnetic resonance spectrometry. Anal. Chem., 1989, 61:2579-2582.
    [48]
    Kintner III P K, Van Buren J P. Carbohydrate interference and its correction in pectin analysis using the m-hydroxydiphenyl method. J. Food Sci., 1982, 47 (3):756-759.
    [49]
    Mazzoni V, Bradesi P, Tomi F, et al. Direct qualitative and quantitative analysis of carbohydrate mixtures using 13C NMR spectroscopy: Application to honey. Magn. Reson. Chem.,1997, 35 (13):81-90.
    [50]
    Tamate J, Bradbury J H. Determination of sugars in tropical root crops using 13C NMR spectroscopy: Comparison with the HPLC method. J. Sci. Food Agric., 1985, 36 (12):1291-1302.
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    [1]
    Huang Y C, Wu H C, Wang Y D, et al. Pectin methylesterase34 contributes to heat tolerance through its role in promoting stomatal movement. Plant Physiol., 2017, 174 (2):748-763.
    [2]
    Baum A, Dominiak M, Vidal-Melgosa S, et al. Prediction of pectin yield and quality by FTIR and carbohydrate microarray analysis. Food Bioprocess Technol., 2017, 10 (1):143-154.
    [3]
    Grassino A N, Barba F J, Brnčić M, et al. Analytical tools used for the identification and quantification of pectin extracted from plant food matrices, wastes and by-products: A review. Food Chem., 2018, 266:47-55.
    [4]
    Lopez-Sanchez P, Martinez-Sanz M, Bonilla M R, et al. Nanostructure and poroviscoelasticity in cell wall materials from onion, carrot and apple: Roles of pectin. Food Hydrocoll., 2020, 98:105253.
    [5]
    Bagherian H, Ashtiani F Z, Fouladitajar A, et al. Comparisons between conventional, microwave- and ultrasound-assisted methods for extraction of pectin from grapefruit. Chem. Eng. Process., 2011, 50 (11/12): 1237-1243.
    [6]
    Naqash F, Masoodi F A, Rather S A, et al. Emerging concepts in the nutraceutical and functional properties of pectin—A Review. Carbohyd. Polym., 2017, 168:227-239.
    [7]
    Tyagi V, Sharma P, Malviya R. Pectins and their role in food and pharmaceutical industry: A review. J. Chronother. Drug Deliv., 2015, 6:65-77.
    [8]
    Jafari F, Khodaiyan F, Kiani H, et al. Pectin from carrot pomace: Optimization of extraction and physicochemical properties. Carbohyd. Polym., 2017, 157:1315-1322.
    [9]
    Kyomugasho C, Christiaens S, Shpigelman A, et al. FT-IR spectroscopy, a reliable method for routine analysis of the degree of methylesterification of pectin in different fruit- and vegetable-based matrices. Food Chem.,2015, 176:82-90.
    [10]
    Rao W, Tuo S, Zhong K, et al. Research progress on extraction and analysis of pectin in tobacco. Guangzhou Chem., 2009, 34 (1):71-77.
    [11]
    Zhou S, Xu Y, Wang C, et al. Pyrolysis behavior of pectin under the conditions that simulate cigarette smoking. J. Anal. Appl. Pyrolysis., 2011, 91:232-240.
    [12]
    Yang J, Ding H, Yu G, et al. Determination of pectin content in reconstituted tobacco by carbazole colorimetry.Chin. J. Anal. Lab., 2012, 31 (6):100-102.
    [13]
    Xu Z Q, Chen K B, Cai B, et al. Determination of pectin content in tobacco by enzymatic hydrolysis-flow analysis method.Tobacco Sci. Technol., 2005, 9:26-28.
    [14]
    Rao W, Tuo S, Zhong K, et al. Determination of pectin in tobacco by enzymatic hydrolysis-ion chromatography. Chem. Res., 2010, 21 (3):72-74.
    [15]
    Tinmanee R, Larsen S C, Morris K R, et al. Quantification of gabapentin polymorphs in gabapentin/excipient mixtures using solid state 13C NMR spectroscopy and X-ray powder diffraction. J. Pharm. Biomed. Anal., 2017, 146:29-36.
    [16]
    Christiansen S C, Hedin N, Epping J D, et al. Sensitivity considerations in polarization transfer and filtering using dipole-dipole couplings: Implications for biomineral systems. Solid State Nucl. Mag., 2006, 29 :170-182.
    [17]
    Hartmann S R, Hahn E L. Nuclear double resonance in the rotating frame. Phys. Rev., 1962, 128 (5):2042-2953.
    [18]
    Schaefer J, Stejskal E O. Carbon-13 nuclear magnetic resonance of polymers spinning at the magic angle. J. Am. Chem. Soc., 1976,98 (4):1031-1032.
    [19]
    Haslinger S, Hietala S, Hummel M, et al. Solid-state NMR method for the quantification of cellulose and polyester in textile blends. Carbohyd. Polym., 2019, 207:11-16.
    [20]
    Fu L, McCallum S A, Miao J, et al. Rapid and accurate determination of the lignin content of lignocellulosic biomass by solid-state NMR. Fuel, 2015, 141:39-45.
    [21]
    Nurdjanah S, Hook J, Paton J, et al. Galacturonic acid content and degree of esterification of pectin from sweet potato starch residue detected using 13C CP/MAS solid state NMR. Eur. J. Food Res. Rev., 2013, 3(1):16-37.
    [22]
    Zhu X, Liu B, Zheng S, et al. Quantitative and structure analysis of pectin in tobacco by 13C CP/MAS NMR spectroscopy. Anal. Methods, 2014, 6 (16):6407-6413.
    [23]
    Giraudeau P, Tea I, Remaud G S, et al. Reference and normalization methods: Essential tools for the intercomparison of NMR spectra. J. Pharm. Biomed. Anal., 2014, 93:3-16.
    [24]
    Hall R A, Jurkiewicz A, Maciel G E. A bicyclic ketone as a solid-state carbon-13 NMR intensity reference. Anal. Chem., 1993, 65 (5):534-538.
    [25]
    Muntean J V, Stock L M. Bloch decay solid-state carbon-13 NMR spectroscopy of the samarium iodide-treated Argonne Premium coals. Energy Fuels, 1991, 5:765-767.
    [26]
    Zhang J, Giotto M V, Wen W Y, et al. An NMR study of the state of ions and diffusion in perfluorosulfonate ionomer. J. Membrane Sci.,2006, 269 (1/2):118-125.
    [27]
    Jurkiewicz A, Maciel G E. 13C NMR spin-lattice relaxation properties and quantitative analytical methodology of 13C NMR spectroscopy for coals. Anal. Chem., 1995, 67(13):2188-2194.
    [28]
    Gao X, Laskar D D, Zeng J, et al. A 13C CP/MAS-based nondegradative method for lignin content analysis. ACS Sustain. Chem. Eng., 2015, 3 (1):153-162.
    [29]
    Hall R A, Wooten J B. Quantitative analysis of cellulose in tobacco by 13C CPMAS NMR.J. Agric. Food Chem., 1998, 46:1423-1427.
    [30]
    Keeler C, Maciel G E. Quantitation in the solid-state 13C NMR analysis of soil and organic soil fractions. Anal. Chem., 2003, 75:2421-2432.
    [31]
    Pang R L, Zhang Q L, Guo L L, et al. Study on the colorimetry determination conditions of pectin in fruits and derived products. J. Fruit Sci., 2012, 29 (1):302-307.
    [32]
    Jarvis M C, Apperley D C. Chain conformation in concentrated pectic gels: Evidence from 13C NMR. Carbohyd. Res., 1995, 275 (1):131-145.
    [33]
    Westerlund E, Aman P, Andersson R E, et al. Investigation of the distribution of methyl ester groups in pectin by high-field 13C NMR. Carbohyd. Polym., 1991, 14:179-187.
    [34]
    Sinitsya A, Copikova J, Pavlikova H. 13C CP/MAS NMR spectroscopy in the analysis of pectins. J. Carbohydr. Chem.,1998, 17 (2):279-292.
    [35]
    Synytsya A, Copikova J, Brus J. 13C CP/MAS NMR spectra of pectins: A peak-fitting analysis in the C-6 region. Czech J. Food Sci., 2003, 21:1-12.
    [36]
    Wang T, Park Y B, Cosgrove D J, et al. Cellulose-pectin spatial contacts are inherent to never-dried arabidopsis primary cell walls: Evidence from solid-state nulear magnetic resonance. Plant Physiol., 2015, 168:871-884.
    [37]
    Phyo P, Wang T, Kiemle S N, et al. Gradients in wall mechanics and polysaccharides along growing inflorescence stems. Plant Physiol., 2017, 175:1593-1607.
    [38]
    Seger M R, Maciel G E. Quantitative 13C NMR analysis of sequence distributions in poly(ethylene-co-1-hexene). Anal. Chem., 2004, 76:5734-5747.
    [39]
    Mao J D, Schmidt-Rohr K. Accurate quantification of aromaticity and nonprotonated aromatic carbon fraction in natural organic matter by 13C solid-state nuclear magnetic resonance. Environ.Sci. Technol., 2004, 38: 2680-2684.
    [40]
    Mao J, Cao X, Olk D C, et al. Advanced solid-state NMR spectroscopy of natural organic matter. Prog. Nucl. Magn. Reson. Spectrosc., 2017, 100:17-51.
    [41]
    Johnson R L, Schmidt-Rohr K. Quantitative solid-state 13C NMR with signal enhancement by multiple cross polarization. J. Magn. Reson.,2014, 239:44-49.
    [42]
    Duan P, Schmidt-Rohr K. Composite-pulse and partially dipolar dephased multiCP for improved quantitative solid-state 13C NMR. J. Magn. Reson., 2017, 285:68-78.
    [43]
    Smernik R J, Oades J M. The use of spin counting for determining quantitation in solid state 13C NMR spectra of natural organic matter: 1. Model systems and the effects of paramagnetic impurities. Geoderma, 2000, 96: 101-129.
    [44]
    Wong S, Hanna J V, King S, et al. Fractionation of natural organic matter in drinking water and characterization by 13C cross-polarization magic-angle spinning NMR spectroscopy and size exclusion chromatography. Environ. Sci. Technol., 2002, 36 (16):3497-3503.
    [45]
    Alesiani M, Proietti F, Capuani S, et al. 13C CP/MAS NMR spectroscopic analysis applied to wood characterization. Appl. Magn. Reson., 2005, 29 (2):177-184.
    [46]
    Jiang J, Hu Y, Tian Z, et al. Development of a rapid method for the quantification of cellulose in tobacco by 13C CP/MAS NMR. Carbohyd. Polym., 2016, 135:121-127.
    [47]
    Zhang M, Maciel G E. Built-in carbon-13 intensity reference for solid-state analysis by magic-angle-spinning nuclear magnetic resonance spectrometry. Anal. Chem., 1989, 61:2579-2582.
    [48]
    Kintner III P K, Van Buren J P. Carbohydrate interference and its correction in pectin analysis using the m-hydroxydiphenyl method. J. Food Sci., 1982, 47 (3):756-759.
    [49]
    Mazzoni V, Bradesi P, Tomi F, et al. Direct qualitative and quantitative analysis of carbohydrate mixtures using 13C NMR spectroscopy: Application to honey. Magn. Reson. Chem.,1997, 35 (13):81-90.
    [50]
    Tamate J, Bradbury J H. Determination of sugars in tropical root crops using 13C NMR spectroscopy: Comparison with the HPLC method. J. Sci. Food Agric., 1985, 36 (12):1291-1302.
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