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Comprehensive analysis of cellulose content, crystallinity, and lateral packing in Gossypium hirsutum and Gossypium barbadense cotton fibers using sum frequency generation, infrared and Raman spectroscopy, and X-ray diffraction

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Abstract

The mesoscale packing and crystal structure of cellulose microfibrils as well as temporal changes in cell wall composition and hydration during the development of cotton fibers from two species, Gossypium hirsutum and G. barbadense were studied using vibrational sum frequency generation (SFG), attenuated total refection infrared (ATR-IR), Fourier transform Raman (FT-Raman) spectroscopy and X-ray diffraction (XRD). The developmental stages analyzed (13–60 days post anthesis) included primary wall synthesis, transitional cell wall remodeling, secondary wall thickening via synthesis of nearly pure cellulose, and fiber maturation. ATR-IR and FT-Raman combined with principle component analysis revealed that fibers of both species undergo abrupt changes in the cellulose and matrix polymer contents during the transition to secondary cell wall synthesis. XRD revealed that cellulose crystal size and crystallinity increase similarly over time in both species. SFG analysis of fibers from un-opened bolls, which were stored in water then air dried, showed subtle differences between two species in the mesoscale ordering of cellulose microfibrils in the maturing secondary walls. In the samples of mature fibers dried on the plant after the boll split opened naturally, the difference in SFG spectra between species was negligible. Collectively, the results show that (a) SFG can uniquely reveal differences in cellulose fibril ordering in maturing cotton fibers before boll opening; and (b) illustrate the comparative usefulness of other commonly used spectroscopic analytical methods for cotton fiber analysis.

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Acknowledgments

This work was supported by The Center for Lignocellulose Structure and Formation, an Energy Frontier Research Center funded by the U.S. Department of Energy, Office of Science, and Office of Basic Energy Sciences under Award Number DE-SC0001090.

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Authors and Affiliations

  1. Department of Chemical Engineering and Materials Research Institute, Pennsylvania State University, University Park, PA, 16802, USA

    Christopher M. Lee, Kabindra Kafle, David W. Belias & Seong H. Kim

  2. Department of Biology, Pennsylvania State University, University Park, PA, 16802, USA

    Yong Bum Park

  3. Department of Crop Science, North Carolina State University, Raleigh, NC, 27695-7620, USA

    Richard E. Glick

  4. Department of Crop Science and Department of Plant and Microbial Biology, North Carolina State University, Raleigh, NC, 27695-7620, USA

    Candace H. Haigler

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  1. Christopher M. Lee
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Correspondence to Candace H. Haigler or Seong H. Kim.

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Lee, C.M., Kafle, K., Belias, D.W. et al. Comprehensive analysis of cellulose content, crystallinity, and lateral packing in Gossypium hirsutum and Gossypium barbadense cotton fibers using sum frequency generation, infrared and Raman spectroscopy, and X-ray diffraction. Cellulose 22, 971–989 (2015). https://doi.org/10.1007/s10570-014-0535-5

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