烟草果胶和纤维素含量^(13)C MultiCP/MAS NMR同时测量  

Simultaneous determination of pectin and cellulose in tobacco samplesby a ^(13)C MultiCP / MAS NMR method

作　　者：王鹏 唐杰 杨明宇 朱立军 汪长国 陈昆燕 王鹏[2] 杨俊 WANG Peng;TANG Jie;YANG Mingyu;ZHU Lijun;WANG Changguo;CHEN Kunyan;WANG Peng;YANG Jun(Technology Center of China Tobacco Chongqing Industrial Co.,Ltd.,Chongqing 400060;Research Center of Tobacco and Health,University of Science and Technology of China,Hefei 230052)

机构地区：[1]重庆中烟工业有限责任公司技术中心,重庆400060 [2]中国科学技术大学烟草与健康研究中心,合肥230052

出　　处：《安徽农业大学学报》2024年第3期516-522,共7页Journal of Anhui Agricultural University

基　　金：重庆中烟工业有限责任公司科技项目(2020500000300361)资助。

摘　　要：果胶和纤维素是烟草细胞壁的重要组成成分,其含量对烟草品质与安全性产生重要影响。传统分析方法难以实现果胶和纤维素的同时定量。本文在优化核磁共振波谱序列条件的基础上,采用固体^(13)C多重交叉极化/魔角旋转核磁共振波谱分析技术(^(13)C MultiCP/MAS NMR)建立了烟草果胶和纤维素含量的同时测量新方法。方法以聚半乳糖醛酸和微晶纤维素为标准物质,以3-(三甲基甲硅烷基)丙酸-d4钠盐(TMSP)做为内标物质,分别建立内标法标准曲线,相关系数R2为0.999 0和0.998 2。果胶测量的检出限和定量限分别为0.38和1.28 mg·g^(–1),精密度(RSD,n=5)小于3.05%。纤维素测量的检出限和定量限为1.01和3.32 mg·g^(–1),精密度(RSD,n=5)小于2.74%。应用本方法测量烟梗、烟草薄片和烟叶等不同类型样品中的果胶和纤维素含量,并对比烟草行业标准方法的测量结果,果胶含量的相对误差在-0.95%至4.51%之间,纤维素含量的相对误差在0.77%至2.46%之间。表明^(13)C MultiCP/MAS NMR方法快速,准确,适合批量样品的分析测量,为果胶和纤维素等细胞壁类大分子的同时定量分析提供重要技术支持。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 ^(13)C multi-cross polarization/magic angle rotation NMR(^(13)C MultiCP/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-d_(4) sodium salt(TMSP)as the internal standard material,and the correlation coefficients R^(2) were 0.9990 and 0.9982.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,respectively.The results showed that the ^(13)C MultiCP/MAS NMR method is fast,accurate and suitable for the determination of batch samples,which provides an important technical support for simultaneous quantitative analysis of cell wall macromolecules such as pectin and cellulose.

关 键 词：果胶 纤维素 ^(13)C MultiCP/MAS NMR 烟草 

分 类 号：TS411[农业科学—烟草工业]