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Normal and slim cigarettes with different filter ventilation and cigarette paper air permeability were rolled. The effects of filter ventilation, cigarette paper ventilation and ventilation distribution on nine phenolic aroma components release from mainstream cigarette smoke were investigated. The results showed the filter ventilation rate, paper ventilation rate negatively correlated to the releases of nine phenolic aroma components in cigarette smoke, and with the increase of ventilation rate, the decrease rate of maltol with caramel flavour and smaller molecular weight was higher, while the decrease rate of eugenol with smoky flavor and larger molecular weight was lower. No matter normal or small cigarettes, the paper and filter ventilation rate have different effects on the decrease of smoke composition, and the paper ventilation rate has greater influence than the filter ventilation rate. The effects of filter ventilation rate, paper ventilation rate and ventilation distribution on the release of nine phenolic aroma components in conventional cigarette smoke were greater than those in slim cigarette smoke. When the total ventilation rate was the same, the release of 9 phenolic aroma components in cigarette smoke with high filter ventilation rate and low paper ventilation rate was higher than that with low filter ventilation rate and high paper ventilation rate. [ABSTRACT FROM AUTHOR]

In order to investigate the effect of different ventilation distribution on organic acid release from mainstream smoke of slim cigarette, the slim cigarette samples with different filter ventilation and cigarette paper air permeability were rolled, and the organic acid in mainstream smoke of samples were analyzed by GC-MS, the prediction models of organic acids release based on both filter and paper ventilation rate were established. The results were as follows: 26 kinds of organic acids were detected. With the increase of filter ventilation rate or paper ventilation rate, the decrease rate of organic acids with smaller molecular weight was higher, while that with larger molecular weight was smaller, and the effect of paper ventilation rate on the release of organic acids in cigarette smoke was greater than that of filter ventilation rate. When the total ventilation rate (V) was constant, the release of organic acids in cigarette smoke with high filter ventilation rate and low paper ventilation rate was higher than that with low filter ventilation rate and high paper ventilation rate. The prediction accuracy of the model of organic acid release was high, and the results further proved that the cigarette organic acid release was higher with the combination of high filter ventilation rate and low paper ventilation rate. [ABSTRACT FROM AUTHOR]

• An AP combination suitable for seven minor tobacco alkaloids analysis was first presented. • AP provides an overall improvement in ME correction for solvents and samples. • The quantitative results of samples are accurate in different experimental scenarios. • This method possessed good accuracy, precision, and long-term robustness. Tobacco alkaloids are important precursors of carcinogenic tobacco-specific nitrosamines. Therefore, accurate quantification of tobacco alkaloids is highly important. This study investigates the compensation effects of novel analyte protectants (APs) for matrix effects (MEs) to determine seven minor tobacco alkaloids (nornicotine, myosmine, anabasine, anatabine, nicotyrine, 2,3′-bipyridine, and cotinine) in mainstream cigarette smoke with high accuracy and robustness. By comparing the heights and shapes of the chromatographic peaks before and after the addition of APs to standard solutions prepared in dichloromethane and cigarette smoke solutions, the compensation effects of 12 APs and their combinations on the MEs of seven minor tobacco alkaloids were evaluated, and the best combination of 2-pyridylethylamine (2 mg/mL)+1,2-decanediol (1 mg/mL) was identified. This AP combination could effectively improve the shapes and increase the heights (by 7–371%) of chromatographic peaks for standard solutions prepared in dichloromethane and cigarette smoke solutions. Before the addition of this AP combination, the slope ratios of the calibration curves for two types of standard solutions of the seven target chemicals were 71.4–159.8%, while they were 87.4–105.6% after the addition, indicating that this AP combination reduced the matrix difference between pure solvent and cigarette smoke solution. After adding the AP combination, the standard curves of solutions prepared in dichloromethane showed good linearity (r 2 ≥ 0.999), the spiked recoveries were between 80.9% and 119.6%, and the inter- and intraday precisions were between 1.5–9.5% and 3.1–8.5%, respectively. Three commercial cigarette samples and one mixed standard solution were also tested under four different instrument working conditions to verify the long-term accuracy and ruggedness of the approach in routine real-world analysis of the method. The results showed that the RSD values were higher (3.5–25.4%) without the AP combination than that (<6.7%) with the AP combination. Because of its high accuracy, precision, and robustness, this method has good practical prospects. [ABSTRACT FROM AUTHOR]

• A GC-MS/MS combining with silylation method was developed to determine 171 hydroxyl flavour additives in cigarette smoke. • Silylation in combination with GC-MS/MS has advantages in terms of high selectivity and sensitivity. • The novel use of a fused silica splitter simplified installation of backflushing system and exhibited better performance. • This method possessed good accuracy, satisfactory sensitivity and long-term robustness. • The developed method was applied to 270 practical cigarette smoke samples and meaningful results of HFAs were obtained. Flavour additives with carboxyl and hydroxyl groups (FACHs), the key ingredients in characteristic flavours, are frequently detected in cigarette smoke. They are attracting increasing attention in regulating the flavour additives used in tobacco to curb youth tobacco use and prevent the use of additives that are harmful. In this study, a highly robust, sensitive, and precise method based on silylation and GC-MS/MS with an improved backflushing system was developed for the simultaneous analysis of 171 FACHs in cigarette smoke. Silylation has been shown to have advantages in terms of high selectivity and sensitivity to chemicals with carboxyl and hydroxyl groups, especially when combined with GC-MS/MS. The extraction and silylation conditions were optimised. Dichloromethane was used as the extraction agent. BSTFA in combination with 1% TMCS and 0.2% TMSI was selected as silylating agent for high silylation efficiency, particularly for hindered analytes. The method has been validated. The limit of detection (LOD) ranged from 0.6 to 332.3 ng/mL. 91.1% out of the analytes in QC samples had precisions lower than 10% during one month run. The improved backflushing system with a fused silica splitter was shown to be crucial in the excellent long-term robustness of the method. The developed method was used to determine flavour additives in 270 practical cigarette smoke samples with reliable results. A total of 154 FACHs were identified with wide-range levels among different cigarette brands. [ABSTRACT FROM AUTHOR]

[Display omitted] • A GC–MS/MS method was developed to determine 559 aroma compounds in cigarette smoke. • An analyte protectant mixture that suited wide polar range solvents was proposed. • The use of precolumn backflushing markedly improved the instrument robustness. • This method is fit-for-purpose in routine analysis of a large number of samples. Trace analysis of multi-targets in complex matrices such as cigarette smoke has always been a great challenge for analysts. In this paper, a high-throughput qualitative and quantitative method was developed and validated to determine 559 aroma compounds in mainstream smoke using gas chromatography-tandem mass spectrometry. Among four commonly used extraction solvents, dichloromethane showed obvious advantages in extracting the target aroma compounds with different polarity. An analyte protectant mixture consisting of 3-methoxy-1,2-propanediol, 1,2-octandiol, 1,2-nonanediol, and 1,2-tetradecanediol was first presented to compensate for the matrix effect, which was suitable for solvents of a wide polarity range such as hexane, dichloromethane, acetone, acetonitrile, and methanol. Moreover, the introduction of precolumn backflushing markedly improved the instrument robustness in analyzing complex cigarette smoke. The results showed that the system retained good stability after 30 days of injection. The proposed method performed well in terms of key validation parameters: accuracy (70.3–118.8% for 552 compounds), inter/intraday precision (0.1–10.7% and 0.2–18.2%), and sensitivity (limit of detection 0.12–102.54 ng/mL). Finally, this method was successfully applied to analyze 12 different commercial cigarette brands. The proposed method has good application prospects based on its robustness and may be used as a potential tool to transfer the cigarette design from an experience-dependent mode to a digital design mode. This method also shows potential in assaying aroma compounds in essentials, food or plant-based substrates. [ABSTRACT FROM AUTHOR]

• Exogenous dietary AGEs have been suggested to increase health risk. • Oral use tobacco products are used as substitute for cigarette smoking due to their "reduced risk" and no second-hand smoke. • Thus, oral use tobacco products may increase AGEs intake due to their oral form of use. • To the best of our knowledge, no survey of CML and CEL levels in oral use tobacco products has been reported. • The free and total CML and CEL in different oral use tobacco products was determined in this work for the first time. • What's more, the relationship of CML (or CEL) and lysine, total amino acid, reducing carbohydrates was studied also. Exogenous dietary advanced glycation endproducts (AGEs) have been suggested to increase health risk. Oral use tobacco products are used as substitute for cigarette smoking due to their "reduced risk" and no second-hand smoke. They may increase AGEs intake due to their oral form of use. However, research on AGEs in oral use tobacco products is limited. A HPLC-MS/MS method was developed to survey free and total Nε-Carboxymethyllysine (CML) and Nε-Carboxyethyllysine (CEL) levels in different oral use tobacco products in this work. HPLC conditions, such as HPLC column and mobile phase additive were optimized. With the optimized conditions, analytical method performance for three types of oral use tobacco matrix (i.e. CRP2, gum and dissolvable tobacco product) was characterized. CML and CEL showed higher recovery in all three sample matrix, and the recovery of CML and CEL was in the range of 88.7%-120%, 90.0%-110%, respectively. The developed method showed good intra-day and inter-day precision with RSDs for both free and total CML (or CEL) of less than 9.7%. Limit of detections (LODs) of CML and CEL were 0.36 and 0.25 ng/mL, respectively. Sample analysis for 21 oral use tobacco products was conducted with the developed method. As for oral use tobacco products, total CML and CEL was much more than those of their free state, indicating that CML and CEL exist mainly protein adducts. In addition, the content of CML was higher than that of CEL for both free and total state. Oral use tobacco products I (i.e. dry snuff, moist snuff, suns and chew) had the highest CML (i.e. 44.89–608.69 µg/g) and CEL (i.e. 15.98–77.70 µg/g) levels, compared with oral use tobacco products II (i.e. gum) with the least CML (i.e. 0.7–0.8 µg/g) and CEL (i.e. 0.14–0.18 µg/g) levels. It mainly depended on the composition and processing technology of oral use tobacco products. Both total CML and CEL showed linear relationship with lysine and total amino acid (i.e. R > 0.77). However, there was no linear relationship between total CML (or CEL) and total reducing carbohydrates (i.e. R < 0.5). [ABSTRACT FROM AUTHOR]