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离子色谱指纹图谱分析法在烟用香料质量评价中的应用

[Application of ion chromatographic fingerprint analysis for quality evaluation of tobacco flavors].

作者信息

Xu Gao-Yan, He Xin-Ying, Zhang Li-Na, Liu Chong-Sheng, Gao Yang, Huang Zhong-Ping, Liu Hui-Jun, Wu Zhao-Ming, Zhang Rui-Chao, Shi Hong

机构信息

Technical Center, China Tobacco Zhejiang Industry Co., Ltd., Hangzhou 310008, China.

College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014, China.

出版信息

Se Pu. 2024 Aug;42(8):805-811. doi: 10.3724/SP.J.1123.2023.11008.

Abstract

Tobacco flavor, an important tobacco additive, is an essential raw material in cigarette production that can effectively improve the quality of tobacco products, add aroma and taste, and increase the suction flavor. The quality consistency of tobacco flavors affects the quality stability of branded cigarettes. Therefore, the quality control of tobacco flavors is a major concern for cigarette and flavor manufacturers. Physical and chemical indices, odor similarity, and sensory efficacy are employed to evaluate the quality of tobacco flavors, and the analysis of chemical components in tobacco flavors is usually conducted using gas chromatography (GC) and high performance liquid chromatography (HPLC). However, because the composition of tobacco flavors is complex, their quality cannot be fully reflected using a single component or combination of components. Therefore, establishing an objective analytical method for the quality control of tobacco flavors is of extreme importance. Chromatographic fingerprint analysis is routinely used for the discriminative analysis of tobacco flavors. Chromatographic fingerprints refer to the general characteristics of the concentration profiles of different chemical compounds. In the daily procurement process, fingerprints established by GC and HPLC are effective for the evaluation and identification of tobacco flavors. However, given continuous improvements in aroma-imitation technology, some flavors with high similarity cannot be directly distinguished using existing methods. In this study, a method for the determination of organic acids and inorganic anions in tobacco flavors based on ion chromatography (IC) was developed to ensure the quality consistency of tobacco flavors. A 1.0 g sample of tobacco flavors and 10 mL of deionized water were mixed and vibrated for 30 min. The aqueous sample solution was passed through a 0.45 μm membrane filter and RP pretreatment column in succession to eliminate interferences and then subjected to IC. Standard solutions containing nine organic acids and seven inorganic anions were used to identify the anions in the tobacco flavors, and satisfactory reproducibility was obtained. The relative standard deviations (RSDs) for retention times and peak areas were <0.71% and <6.02%, respectively. The chromatographic fingerprints of four types of tobacco flavors (samples A-D) from five different batches were obtained. Nine tobacco flavor samples from different manufacturers (samples AY1-AY3, BY1-BY2, CY1-CY2, DY1-DY2) were also analyzed to obtain their chromatographic fingerprints. Hierarchical cluster and similarity analyses were used to evaluate the quality of tobacco flavors from different manufacturers. Hierarchical clustering refers to the process of subdividing a group of samples into clusters that exhibit a high degree of intracluster similarity and intercluster dissimilarity. The dendrograms obtained using SPSS 12.0 indicated good quality consistency among the samples in different batches. Samples AY3, BY2, CY2, and DY1 clustered with the batches of standard tobacco flavors. Therefore, hierarchical cluster analysis can effectively distinguish the quality of products from different manufacturers. The Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine (version 2.0) was used to evaluate the similarity between the standard tobacco flavors and products from different manufacturers. Among the samples analyzed, samples AY3, BY2, CY2, and DY1 showed the highest similarity values (>97.7%), which was consistent with the results of the hierarchical cluster analysis. This finding indicates that IC combined with chromatographic fingerprint analysis could accurately determine the quality of tobacco flavors. GC combined with ultrasonic-assisted liquid-liquid extraction was also used to analyze the tobacco flavors and verify the accuracy of the proposed method. Compared with GC coupled with ultrasonic-assisted liquid-liquid extraction, IC demonstrated more significant quality differences among certain tobacco flavors.

摘要

烟草香料作为一种重要的烟草添加剂,是卷烟生产中的关键原料,能够有效提升烟草制品品质,增添香气和口感,增强抽吸风味。烟草香料的质量一致性影响着品牌卷烟的质量稳定性。因此,烟草香料的质量控制是卷烟及香料制造商高度关注的问题。物理化学指标、气味相似度和感官效果被用于评估烟草香料的质量,烟草香料中化学成分的分析通常采用气相色谱法(GC)和高效液相色谱法(HPLC)。然而,由于烟草香料的成分复杂,单一成分或成分组合无法完全反映其质量。因此,建立一种客观的烟草香料质量控制分析方法至关重要。色谱指纹图谱分析常用于烟草香料的鉴别分析。色谱指纹图谱是指不同化合物浓度分布的总体特征。在日常采购过程中,由GC和HPLC建立的指纹图谱对烟草香料的评估和鉴定有效。然而,随着仿香技术的不断进步,一些相似度高的香料无法用现有方法直接区分。本研究建立了一种基于离子色谱(IC)测定烟草香料中有机酸和无机阴离子的方法,以确保烟草香料的质量一致性。取1.0 g烟草香料样品与10 mL去离子水混合并振荡30 min。将水样依次通过0.45 μm滤膜和RP预处理柱以消除干扰,然后进行IC分析。使用含有9种有机酸和7种无机阴离子的标准溶液鉴定烟草香料中的阴离子,获得了良好的重现性。保留时间和峰面积的相对标准偏差(RSD)分别<0.71%和<6.02%。获得了来自五个不同批次的四种烟草香料(样品A - D)的色谱指纹图谱。还分析了来自不同制造商的九个烟草香料样品(样品AY1 - AY3、BY1 - BY2、CY1 - CY2、DY1 - DY2)以获得其色谱指纹图谱。采用层次聚类和相似度分析评估不同制造商的烟草香料质量。层次聚类是指将一组样品细分为簇的过程,同一簇内样品相似度高,不同簇间样品相似度低。使用SPSS 12.0获得的树状图表明不同批次的样品间质量一致性良好。样品AY3、BY2、CY2和DY1与标准烟草香料批次聚类在一起。因此,层次聚类分析能够有效区分不同制造商产品的质量。采用《中药色谱指纹图谱相似度评价系统》(2.0版)评估标准烟草香料与不同制造商产品之间的相似度。在所分析的样品中,样品AY3、BY2、CY2和DY1的相似度值最高(>97.7%),这与层次聚类分析结果一致。这一发现表明IC结合色谱指纹图谱分析能够准确测定烟草香料的质量。还采用GC结合超声辅助液液萃取分析烟草香料并验证所提方法的准确性。与GC联用超声辅助液液萃取相比,IC在某些烟草香料间显示出更显著的质量差异。

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