Simultaneous determination of pectin and cellulose in tobacco samples by a 13C MultiCP/MAS NMR method
Pectin and cellulose are important components of tobacco cell wall,and their contents have an important impact on the quality and safety of tobacco.A new method for simultaneous determination of pectin and cellulose in tobacco was developed by solid 13C multi-cross polarization/magic angle rotation NMR(13C Mul-tiCP/MAS NMR)based on optimized NMR sequence conditions.The standard curves of internal standard method were established,using polygalacturonic acid and microcrystalline cellulose as the standard material,respectively,and 3-(Trimethylsilyl)propionic acid-d4 sodium salt(TMSP)as the internal standard material,and the correlation coefficients R2 were 0.999 0 and 0.998 2.The limits of detection(LOD)and quantification(LOQ)were 0.38 and 1.28 mg·g-1 for pectin,the precision(RSD,n=5)was less than 3.05%.The LOD and LOQ were 1.01 and 3.32 mg·g-1 for cellulose,the precision(RSD,n=5)was less than 2.74%.The method was applied to the measurement of the pectin and cellulose contents in different types of samples,such as tobacco stem,reconstituted tobacco and tobacco leaf,and compared with the determination results of the tobacco industry standard methods,the relative error was between-0.95%and 4.51%of pectin content,and between 0.77%and 2.46%of cellulose content,re-spectively.The results showed that the 13C MultiCP/MAS NMR method is fast,accurate and suitable for the de-termination of batch samples,which provides an important technical support for simultaneous quantitative analy-sis of cell wall macromolecules such as pectin and cellulose.
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