This study employed large-volume thermal injection-gas chromatography-mass spectrometry (LVTI-GC-MS) technique to systematically investigate the effects of glycerol addition and heating temperature on the puff-by-puff release of volatile organic compounds (VOCs) in aerosols from heated tobacco products (HTPs). The method, which uses a large injection volume of 100 µL, achieves high sensitivity, good stability, and is simple and convenient, thus meeting the requirements for efficient and stable analysis of the release of trace volatile organic compounds. The results showed that: (1) the puff-by-puff release of volatile organic compounds initially increased and then decreased. The lower the boiling point of the components, the earlier the release peak appears. (2) The total release of most volatile organic compounds significantly increased with higher glycerol concentrations, and the growth rate exceeded that of glycerol itself. The release of some components stabilized when the glycerol addition ratio reached 20%. (3) The release trends of volatile organic compounds compared to glycerol showed significant differences. Pyrazines, methyl cyclopentenones, and cyclopentenones exhibited the greatest divergence, while nicotine showed the smallest difference. (4) As glycerol concentration and heating temperature increased, earlier puffs showed more complete release of volatile organic compounds, while the release ratio in the last two puffs significantly decreased, likely due to limitations on the total release. (5) Compared to high-boiling components, low-boiling components were less stable in terms of puff-by-puff release, and their stability showed a significant negative correlation with glycerol concentration and heating temperature. There were substantial differences in how glycerol addition and heating temperature affected the release and stability of various volatile organic compounds. These findings may help optimize the glycerol content and heating conditions for HTPs.
In the tobacco industry, classification serves as a vital bridge linking the properties of raw tobacco leaves with the quality of end products, playing a key role in ensuring product consistency and enhancing market competitiveness. This review systematically summarizes the latest progress from conventional analytical methods to cutting-edge intelligent systems in tobacco detection and classification. Four critical technological domains are systematically analyzed: (1) For appearance feature recognition, advanced image processing and deep learning technologies have enabled efficient, automated grading; (2) Regarding chemical structure detection, integrating various spectroscopic methods with machine learning has facilitated the precise identification of tobacco components; (3) Thermal reaction analysis coupled with machine learning, captures the distinct heat-release and mass-loss during pyrolysis and combustion, enabling accurate classification of different raw tobacco leaves; (4) The pre- and post-reaction product analysis methods have significantly enhanced both the accuracy and speed of complex component detection. Of particular note is the integration of in-situ hyperspectral detection with machine learning algorithms, which enables real-time, non-destructive classification and identification of tobacco leaves, while simultaneously providing detailed information on their chemical composition, such as nicotine and reducing sugars. The review concludes by forecasting future trends in tobacco classification technology, highlighting that the integration of intelligent, in-situ, and fully automated systems will enhance classification precision, shorten assessment cycles, and contribute to improved standardization in tobacco processing.
Combustible cigarettes remain the dominant tobacco product in China, although use of emerging tobacco/nicotine products such as electronic cigarettes (ECs), heated tobacco products (HTPs), smokeless tobacco and nicotine pouches (NPs) is increasing. However, their addictive potential is not well understood. We conducted an online survey (June-September 2025) among 5,901 adult tobacco/nicotine users in China, assessing dependence using the Autonomy Over Tobacco Scale (AUTOS) and the Fagerström Test for Nicotine Dependence (FTND). General linear regression indicated that EC-only users had the lower AUTOS scores (18.32 ± 6.84), while poly-users, especially cigarette + EC users, showed the higher AUTOS (21.61 ± 6.46) and FTND scores (4.06 ± 2.10), compared with cigarette-only users (AUTOS: 20.41 ± 7.02, FTND: 3.63 ± 2.26). Similarly, individuals using ECs plus HTPs (4.79 ± 2.39), cigarettes plus ECs plus HTPs (4.77 ± 1.70), or other combinations (4.76 ± 2.02) exhibited higher FTND scores than cigarette-only users. Familiarity with tobacco/nicotine products and perceived social facilitation were positively associated with both AUTOS and FTND, while perceptions of addictiveness, quitting difficulty, and health risk were positively related to AUTOS. These findings highlight multidimensional dependence, encompassing psychological and physiological dimensions, and reflect influences of diverse product use and cognitive perceptions.
The study innovatively utilized a combination of smoking machine and Cambridge filter to effectively extract the aroma compounds generated during smoking of cigarettes, and employed three different pretreatment methods to obtain optimal cigarette pretreatment procedures. In addition, the aroma components of different cigarettes were identified by different instruments such as gas chromatography-mass spectrometry. Combined with the calculation of Odor Activity Values (OAV), PCA analysis and sensory evaluation were performed on the five types of cigarettes to reveal differences and similarities in their aroma profiles. ### Competing Interest Statement The authors have declared no competing interest.
An effective complex aroma was obtained using a solvent-assisted flavor evaporation pretreatment method, and volatile flavor substances were obtained by gas chromatography–mass spectrometry (GC–MS). The nine attribute flavor characteristics determined by quantitative descriptive analysis in mainstream cigarette smoke were compared with those determined by GC–MS by odor activity value analysis. The sensory evaluation data and overall impressions of five cigarette samples were processed and analyzed using the social statistics software package. Pearson correlation coefficients between the taste attributes and overall impressions of the cigarette samples were determined, revealing differences in product characteristics between different sensory styles. Heatmap and correlation network analyses demonstrated compound-specific sensory modulation: phthalide and 2,5-dimethylphenol enhanced salty/bitter/sour notes but suppressed sweetness, whereas styrene inversely regulated sweetness and sourness.
This study combined a smoking machine with Cambridge filters to extract cigarette aroma compounds. Three pretreatment methods, namely SPME, SAFE, and SDE, were employed. Through GC-MS, 89, 93, and 77 aroma compounds were detected respectively. PCA indicated that the SAFE method had a better ability to distinguish the aroma components of five types of cigarettes, making it the preferred method. By calculating the OAV, 55 aroma compounds with OAV≥1 were identified. The sensory evaluation of 50 volunteers showed that yk had the highest comfort level (median 68.5), while jy had the lowest (61.5). This study filled the gap in the research on traditional cigarette aroma compounds, clarified the effective extraction and analysis methods, and the development of alternatives, and also laid the foundation for improving smoking comfort in the future.
An efficient and rapid method for the detection of total soluble protein in tobacco leaves, utilizing a smartphone-based colorimetric approach has been developed. The proposed low-cost, immediate, general-purpose, and high-throughput (LIGHt) smartphone colorimetric screening assay integrates commercially available microplates, enabling on-site, high-throughput screening of tobacco leaf quality. The study involves preparing protein standard solutions and constructing standard curves using both spectrophotometric and smartphone-based methods. The LIGHt smartphone colorimetry yielded an average relative standard deviation of 10.6 %, a limit of detection of 2 μg/mL, and an average recovery of 93 %. The results demonstrated a comparable performance between intensities from the blue channel and the absorbance values in reflecting protein concentrations, validating the feasibility of utilizing smartphone colorimetry for protein concentration determination. Our approach demonstrates the potential for practical implementation in the field, providing a cost-effective and user-friendly solution for rapid quality assessment in the tobacco industry. The LIGHt smartphone colorimetry enhances quality control practices in the tobacco sector and offers a promising tool for on-site production quality testing in various industries, such as fruits and vegetables.
为明确不同类型烟叶原料在加热卷烟中的利用价值,以来自全国10个省份的60份烟叶为试验材料,在主成分分析的基础上,利用隶属函数法对不同类型烟叶进行感官质量综合评价,并进行聚类分析.结果表明:①烤烟香气质最好,晒黄烟香气量最足,白肋烟、晒红烟劲头最大,雪茄烟稳定性最好,香料烟杂气、刺激性、干燥感、苦涩感、残留及综合评价得分均最高.②隶属函数综合评价最好的9份烟叶依次为云南增香工艺K326中部、云南明火熏制K326中部、云南降淀粉/蛋白质工艺K326中部、云南增强工艺K326中部、云南打叶复烤云烟87中部、四川糊米处理雪茄德雪3号上部、广东大叶青梗中部、云南红大(高氯)中部、广东大叶青梗上部.③聚类分析结果表明60份烟叶可分为3类,第Ⅲ类包括26份烟叶,除劲头外,其他感官质量指标和综合评价总分均最高,与第Ⅰ类和第Ⅱ类差异显著.
Two-dimensional liquid chromatography (2D-LC) has gained increased attention because of its high peak capacity for separating complex samples. However, preparative 2D-LC aimed at isolating compounds is significantly different compared with one-dimensional liquid chromatography (1D-LC) in terms of method development and system configuration; thus, it is less developed than its analytical counterpart. The use of 2D-LC in large-scale product preparation has rarely been reported. Hence, a preparative 2D-LC system was developed in this study. The system was composed of one set of preparative LC modules as a separation system, with a dilution pump, switch valves, and trap column array as the interface, to enable the simultaneous isolation of several compounds. Tobacco was used as a sample, and the developed system was applied to isolate nicotine, chlorogenic acid, rutin, and solanesol. The chromatographic conditions were developed by investigating the trapping efficiency of different types of trap column packings, and chromatographic behaviors under different overload conditions. The four compounds were isolated in one 2D-LC run with high purity. The developed system features low cost because it employs medium-pressure isolation, excellent automation owing to its use of an online column switch, high stability, and capability for large-scale production. The isolation of chemicals from tobacco leaves as pharmaceutical raw materials could aid in the development of the tobacco industry and promote the local agricultural economy.
为了掌握丁香酚-β-D-葡萄糖苷在卷烟中的应用情况,对所合成的丁香酚-β-D-葡萄糖苷进行热失重及热裂解-气相色谱-质谱(Py-GC-MS)分析;将丁香酚-β-D-葡萄糖苷添加至卷烟中,考察其加香应用效果,采用GC-MS考察其在卷烟主流烟气中的释放行为.结果表明:①丁香酚-β-D-葡萄糖苷的热稳定性相比丁香酚明显提升.②丁香酚-β-D-葡萄糖苷在约220℃开始发生裂解,热裂解的主要产物为丁香酚,其他产物有糠醛、苯酚和2-甲氧基苯酚等.③添加丁香酚-β-D-葡萄糖苷的卷烟烟气能释放丁香酚,且其释放量随糖苷添加量的增加而增加,具有良好的释香稳定性和均匀性,糖苷在卷烟中应用的添加方式不同可达不同的加香效果.丁香酚-β-D-葡萄糖苷可作为一种稳定的烟用香料前体应用于卷烟加香中.
The active ingredients from tobacco extracts were continuously separated and purified using a homemade free-flow electrophoresis apparatus. A rectangular free flow electrophoresis device was constructed for the continuous separation and preparation, and the operating conditions of the device were optimized. The fractions obtained from the free-flowing component collection unit were then detected by HPLC and GC-MS. The results showed that a 90% methanol-water solution could maximize the extraction of the active components from tobacco. Chlorogenic acid and nicotine were enriched in three and four of 24 fractions, respectively, after free-flow isoelectric focusing electrophoresis. 2-Hydroxy-2-cyclopentene-1-one, 1-(2-methyl-1,3-oxathiolan-2-yl) ethanone, nornicotine, cotinine, and scopolamine were separated and enriched synchronously. Overall, the use of free-flow electrophoresis technology for the separation and purification of the active substances in tobacco can improve the comprehensive utilization rate of tobacco.
为考察不同类型烟叶挥发性成分的差异,采用两步顶空进样-GC-MS法分析烤烟、雪茄烟、白肋烟、香料烟和晒黄烟烟叶的挥发性成分.两步顶空进样是将静态顶空进样器与程序升温进样口耦合,采用大体积的顶空进样环提高灵敏度,同时采用程序升温进样口以避免因进样体积较大引起的色谱峰展宽.结果表明:①采用新方法共从5种类型烟叶中检出121种挥发性成分;②采用主成分分析和系统聚类分析验证了挥发性成分组成与烟叶类型的关系;③晒黄烟与香料烟的挥发性成分组成最为相似,雪茄烟挥发性成分组成明显区别于其他类型烟叶;④雪茄烟挥发性成分组成与产地有关.该分析方法简便、灵敏、可靠,可用于烟叶成分研究及品质评价.
This study reports the utilization of two-step headspace (HS) to profile the volatile compounds of flue-cured tobacco. The relationship between the volatile components and geographic origin was investigated using multivariate data analysis. To avoid the impact of adsorption caused by tobacco on the HS extraction, the tobacco was soaked by saturated NaCl solutions prior to the HS sampling. However, the introduction of water vapor may affect the subsequent gas chromatography-mass spectrometry (GC-MS) analysis. Thus, two-step HS, which is based on the coupling of the programmed temperature vaporizer inlet and HS autosampler, was employed to remove the water vapor while simultaneously preconcentrating the volatile compounds. The repeatability and stability were evaluated, and 80 compounds were identified from 25 flue-cured tobacco samples. Both principal component analysis (PCA) and hierarchical clustering analysis (HCA) revealed that the volatile components of flue-cured tobacco were closely related to the geographic origin. Furthermore, the characteristic volatiles of the flue-cured tobacco from different regions were illustrated using partial least squares discriminant analysis (PLS-DA). The presented work provided a simple and reliable way to profile the volatile components and characterize geographic origin of tobacco and tobacco products.
In this study, we report a portable kit consisting of a portable workstation, gold screen-printed electrode (SPE), 0.45 μm filter membrane, phosphate buffer solution (PBS), and acetic acid (1%) for point-of-use (POU) analysis of nicotine in tobacco. The activated-screen-printed electrode (A-SPE) displayed superior electron transmission efficiency, and the A-SPE without modification was employed for high-performance analysis of nicotine in actual tobacco after simple sample pretreatment. Remarkably, the fabricated nicotine sensor exhibited a broad working range of 10-100 μg g-1, a low limit of detection (LOD) of 6.4 μg mL-1, good stability, selectivity, and practicality under the optimal conditions. The method was applied to the determination of nicotine in (spiked) samples. Satisfactory recovery results demonstrated that the as-prepared portable kit method with outstanding electrocatalysis ability was feasible for analysis of nicotine in tobacco. Moreover, the values obtained using the A-SPE were in good agreement with those determined by gas chromatography-flame ionization detection (GC-FID), which confirms the feasibility and validity of the present method. The results of the as-proposed portable kit provided a new strategy for analyzing nicotine in actual tobacco samples.
以细支卷烟为研究对象,采用气相色谱-三重四极杆质谱联用(GC-MS/MS)法,分析烟丝加香、爆珠加香、香线加香、丝束加香4种加香方式下烟用香精抽吸前滤嘴分布和抽吸后转移情况.结果表明:1)30 d密封保存后,4种加香方式的烟丝与滤嘴中常用香精分布差异明显,烟丝加香方式下沸点较低的烟用香精迁移比例较大;2)爆珠、香线和丝束3种滤嘴加香方式下,烟用香精的主流烟气粒相转移率和滤嘴截留率均较为接近;烟丝加香方式下,烟用香精的主流烟气粒相转移率整体高于其他3种滤嘴加香方式,滤嘴截留率均低于其他3种滤嘴加香方式;对于高沸点烟用香精,烟丝加香与滤嘴加香的差异更加明显;3)爆珠加香方式下,烟用香精的逐口稳定性好于其他3种加香方式;烟丝加香方式下,烟用香精的逐口稳定性受沸点影响较大;丝束加香和香线加香方式下,烟用香精的逐口释放量随口数增加而升高.
为研究吸烟者的唾液成分,改进并优化了闭环回路气提系统,使用咀嚼刺激法以棉球收集吸烟者唾液,建立了吸烟者唾液成分的闭环回路气提-热脱附-气质联用分析方法,采用该方法分析了不同类型卷烟吸烟者的唾液成分.结果表明:①相较于主流烟气,唾液中不同种类化合物的组成以及比例变化明显,其中,变化最为显著的是环戊酮类、吡嗪类和内酯类化合物以及三乙酸甘油酯,唾液中环戊酮类和吡嗪类化合物的色谱峰面积与烟碱的比值提升了10~30倍,内酯类化合物和三乙酸甘油酯的色谱峰面积与烟碱的比值降低了95%以上;②不同类型卷烟吸烟者唾液的主要化合物的色谱峰面积差异明显,差异较大的成分为吡啶类、吡嗪类、环戊烯酮类和呋喃类化合物,英式烤烟型和混合型卷烟吸烟者唾液中吡啶类和吡嗪类化合物的色谱峰面积高于中式烤烟型,中式烤烟型卷烟吸烟者唾液中环戊烯酮类和呋喃类化合物的质量分数则高于英式烤烟和混合型卷烟.
为了研究卷烟烟气中香味成分逐口释放规律,采用烟气香味成分GC-MS/MS测定方法,分析了烟气中醇类、醛类、酮类、酯类等不同种类香味成分在4种加香方式(烟丝加香、丝束加香、香线加香和爆珠加香)下主流烟气中的逐口释放规律.结果表明:①丝束加香和香线加香之间相似度最高,烟丝加香与其他3种加香方式相似度最低.②香味成分加香部位、结合方式和沸点是影响逐口释放的主要因素.③烟丝加香受蒸馏段高温影响,不同沸点香味成分逐口释放有较大差异,不同沸点的同类香味成分逐口释放占比也明显不同.④爆珠加香受爆珠香精溶剂和滤嘴温度影响,香味成分逐口释放最为稳定,沸点对同类香味成分的释放量无明显影响.⑤丝束加香和香线加香方式下香味成分逐口释放随口数增加而升高,沸点对同类香味成分的释放量无明显影响.
[目的]研究薄板滚筒干燥(KLD)、气流干燥(HDT)两种烘丝模式对烟丝挥发性成分的影响规律.[方法]采用吹扫捕集-多模式进样口-气质联用(P&T-MMI-GC/MS)法鉴定烟丝挥发性成分.[结果](1)主成分分析表明不同烘丝模式对烟丝挥发性成分的影响具有规律性差异.(2)相较烘前,KLD及HDT烘后烟丝中大部分挥发性成分含量降低,明显散失,挥发性成分的散失幅度都与其沸点相关,沸点越低,散失幅度越大;HDT加工烟丝中挥发性成分的散失幅度明显大于KLD.(3)不同类别挥发性成分散失幅度也有差异.脂肪酸降解产物、挥发性有机酸及酚类,烘后散失幅度相对较大;类胡萝卜素降解产物等散失幅度相对较小.
为解决分析卷烟烟气多环芳烃(PAHs)暴露的生物标志物——羟基多环芳烃(OHPAHs)时基质干扰较大、前处理复杂等问题,建立了中心切割二维液相色谱-串联质谱(2DLC-MS/MS)同时测定人尿液中10种OHPAHs的方法.尿液样品仅需酶解过滤后直接上机,第一维色谱以水-甲醇体系为流动相,C18色谱柱分离除杂;第二维色谱以水-乙腈体系为流动相,PAH色谱柱梯度洗脱,多反应监测模式(MRM)下进行MS/MS分析;两维间通过在线稀释将目标流份切割至捕集柱保留.结果表明:①10种OHPAHs均达到基线分离.②方法的检出限和定量限分别为0.001~0.021、0.005~0.070ng/mL,回收率为87.9%~129.1%,日内和日间RSD在5%以内.③该方法成功应用于6名吸烟者和6名非吸烟者的尿液分析.该方法前处理简单便捷,仪器全自动,有效解决了 5种羟基菲同分异构体准确定量的难题,可为烟气PAHs暴露标志物测定提供更为高效、准确的技术手段.
In this work, the sweet aroma components in cigarette smoke from Yunnan Honghe region were analyzed. The watersoluble components were separated from the particulate matter of cigarette smoke by gel permeation chromatography(GPC).The sweet aroma characteristic components were identified by the sensory taste and electronic tongue evaluations and were analyzed by gas chromatography mass spectrometry(GC/MS). The results showed that pyranones, furans, furanones and cyclopentenones were directly contributed to sweet aroma.This method is helpful to identify the key sweet aroma ingredients of cigarette smoke and this work can provide some reference for improving the sensory comfort of cigarette.