烟草果胶和纤维素含量13C MultiCP/MAS NMR同时测量
Simultaneous determination of pectin and cellulose in tobacco samples by a 13C MultiCP/MAS NMR method
王鹏 1唐杰 1杨明宇 2朱立军 1汪长国 1陈昆燕 1杨俊2
作者信息
- 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
- 折叠
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 13C 多重交叉极化/魔角旋转核磁共振波谱分析技术(13C 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 13C 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.
Abstract
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.
关键词
果胶/纤维素/13C/MultiCP/MAS/NMR/烟草Key words
pectin/cellulose/13C MCP/MAS NMR/tobacco引用本文复制引用
基金项目
重庆中烟工业有限责任公司科技项目(2020500000300361)
出版年
2024
国家科技期刊平台
NSTL
万方数据