Journal of University of Science and Technology of China ›› 2021, Vol. 51 ›› Issue (8): 637-646.DOI: 10.52396/JUST-2021-0106

• Chemistry • Previous Articles    

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

NIU Fanchao1, XIE Wei2, HUANG Chaozhang2, LAN Hongqiao2, HUANG Yanjun2, GAO Miao1, YANG Jun1*   

  1. 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
  • Received:2021-04-11 Revised:2021-05-27 Online:2021-08-31 Published:2022-01-14
  • Contact: *E-mail: yjun8202@ustc.edu.cn

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.

Key words: pectin, dimethyl silicone rubber tubing, solid state 13C CP/MAS NMR, tobacco

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