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Background: In recent years, heated tobacco products (HTPs), which are widely used in Japan, have been sold by various brands using additives such as flavors. It has been reported that the components of mainstream smoke are different from those of conventional cigarettes. In this study, we established an analytical method for furans and pyridines in the mainstream smoke, which are characteristic of HTPs and particularly harmful among the generated components, and investigated the amount of component to which the smokers are exposed., Methods: We established a simple analytical method for simultaneous analysis of gaseous and particulate compounds in the mainstream smoke of HTPs (IQOS, glo, ploom S) in Japan by combining a sorbent cartridge and glass fiber filter (Cambridge filter pad (CFP)). Both the sorbent cartridge and CFP were extracted using 2-propanol and analyzed via GC-MS/MS to determine the concentration of furans and pyridines generated from each HTP., Results: The results showed that the levels of target furans such as furfural, 2-furanmethanol, 2(5H)-furanone, and 5-methylfurfural tended to be higher in the mainstream smoke of glo than in standard cigarettes (3R4F). Pyridine, which is generated at a high level in 3R4F as a combustion component, and 4-ethenylpyridine (EP), which is a known marker of environmental tobacco smoke, were detected. Among these components, 2-furanmethanol and pyridine are classified as Group 2B (possibly carcinogenic to humans) by the International Agency for Research on Cancer (IARC). Therefore, it is possible that they will contribute to the health effects caused by use of HTPs., Conclusions: Using the new collection and analytical method for furans and pyridines in the mainstream smoke of HTPs, the level of each compound to which smokers are exposed could be clarified. By comprehensively combining information on the amount of ingredients and toxicity, it will be possible to perform a more detailed calculation of the health risks of using HTPs. In addition, the components detected in this study may be the causative substances of indoor pollution through exhaled smoke and sidestream smoke; therefore, environmental research on the chemicals generated from HTPs would be warranted in future studies., (© 2021. The Author(s).)

As a new form of cigarettes, heated tobacco products (HTPs) have been rapidly distributed worldwide. In this study, an improved method for analyzing gaseous and particulate compounds generated from HTPs is described. Smoke is collected using a GF-CX572 sorbent cartridge with 300 mg of carbon molecular sieves, that is, Carboxen 572 (CX572), and a 9 mm glass-fiber filter (GF). After collection, the CX572 particles from the cartridge are transferred along with the GF and deposited into a vial containing two phases of carbon disulfide and methanol. The CX572 particles settle into the lower carbon disulfide phase, while nonpolar compounds are desorbed. After the sample is allowed to stand, the solution is slowly stirred. The two-phase mixture of carbon disulfide and methanol is combined into a homogeneous solution. Polar compounds are then desorbed, while the desorbed nonpolar compounds remain in solution. For the analysis of carbonyl compounds, an enriched 2,4-dinitrophenylhydrazine solution is added to a portion of the combined solution for derivatization and subsequent high-performance liquid chromatography analysis. For the analysis of volatile organic compounds and water, a portion of the combined solution is analyzed by gas chromatography-mass spectrometry or equipped with a thermal conductivity detector. By applying the proposed GF-CX572 one-cartridge method to the analysis of the mainstream smoke generated from HTPs and traditional cigarettes, several chemical compounds are detected, and the chemical composition of smoke is revealed. The GF-CX572 one-cartridge method can analyze gaseous and particulate chemical compounds from the HTP smoke by utilizing not only the entire puff volume but also one puff volume because the GF-CX-572 cartridge can be replaced with a new cartridge within 3 s. An overview of the chemicals generated from HTPs is obtained in detail by one-puff volume sampling. In addition, the generated chemical compounds strongly depend on the temperature of tobacco leaves in HTPs.

Background: The ammonia contained in tobacco fillers and mainstream and sidestream cigarette smoke accelerates nicotine dependence in cigarette smokers. Ammonia has been included in the non-exhaustive priority list of 39 tobacco components and emissions of cigarette published by the World Health Organization (WHO) Study Group on Tobacco Product Regulation. The development of a simple ammonia detection method will contribute to the establishment of tobacco product regulation under tobacco control policies and allow surveys to be conducted, even by laboratories with small research budgets., Methods: We developed a simple colorimetric method based on the salicylate-chlorine reaction and absorption spectrometry with two reagents (sodium nitroprusside and sodium dichloroisocyanurate). To compare this method to conventional ion chromatography, we analyzed the ammonia levels in tobacco fillers extracted from 35 Japanese commercially marketed cigarette brands manufactured by four tobacco companies (Japan Tobacco (JT) Inc., British American Tobacco (BAT), Philip Morris Japan, and Natural American Spirit). We also analyzed the ammonia levels in the sidestream smoke from cigarettes of the brands that were found to contain high or low tobacco filler ammonia levels., Results: The ammonia levels in the reference cigarette (3R4F) measured by our method and ion chromatography were similar and comparable to previously reported levels. The ammonia levels in tobacco fillers extracted from 35 cigarette brands ranged from 0.25 to 1.58 mg/g. The mean ammonia level of JT cigarette brands was significantly higher (0.83 ± 0.28 mg/g) than that of Natural American Spirit cigarette brands (0.30 ± 0.08 mg/g) and lower than those in the other two cigarette brands (1.11 ± 0.19 mg/g for BAT and 1.24 ± 0.15 mg/g for Philip Morris) (p < 0.001 by Bonferroni test). The ammonia levels in the sidestream smoke of CABIN, Marlboro Black Menthol, American Spirit Light, and Seven Stars were 5.89 ± 0.28, 5.23 ± 0.12, 6.92 ± 0.56, and 4.14 ± 0.19 mg/cigarette, respectively. The ammonia levels were higher in sidestream smoke than in tobacco filler., Conclusions: Our simple colorimetric could be used to analyze ammonia in tobacco fillers and sidestream smoke. There were significant differences between the ammonia levels of the 35 commercially marketed cigarette brands in Japan manufactured by four tobacco manufacturers. Over 90% of the ammonia in sidestream smoke was in gaseous phase.

Because of the health effects of secondhand smoke, the Japanese government is trying to establish an effective law for total avoidance of secondhand smoke in indoor environments for tobacco-free Tokyo Olympic and Paralympic games 2020, as requested by the International Olympic Committee (IOC) and the World Health Organization (WHO). Meanwhile, Philip Morris International has begun selling a new heat-not-burn tobacco, iQOS, which it claims is designed not to produce secondhand smoke. There is little scientific data, however, of the hazards and toxicity of iQOS. In this study, we evaluated several harmful compounds (nicotine, tar, carbon monoxide (CO) and tobacco-specific nitrosamines (TSNAs)) in the mainstream smoke and fillers of iQOS, and compared their concentrations with those from conventional combustion cigarettes. The concentrations of nicotine in tobacco fillers and the mainstream smoke of iQOS were almost the same as those of conventional combustion cigarettes, while the concentration of TSNAs was one fifth and CO was one hundredth of those of conventional combustion cigarettes. These toxic compounds are not completely removed from the mainstream smoke of iQOS, making it necessary to consider the health effects and regulation of iQOS.

Objective: Some Japanese smokers imported Japanese cigarette brands from other Asian countries for personal use because of the increase in tobacco tax in 2010, which meant that privately importing the cigarettes was cheaper than purchasing them in Japan. We assumed that the health hazards of locally made cigarettes were different from those of privately imported cigarettes, despite the brands being the same. In this study, we carried out a comparative toxicological analysis of domestic and privately imported cigarettes., Methods: Privately imported cigarettes of five brands and domestic cigarettes of the brand named "MILD SEVEN ORIGINAL" were selected for the study. The level of polycyclic aromatic hydrocarbons (PAHs) in mainstream smoke was determined by high-performance liquid chromatography using fluorescence detection. The mutagenicity of mainstream smoke was assessed using the Salmonella typhimurium strains TA100, TA98, and YG1024 with the metabolic activation system (S9mix) by preincubation assay. The levels of heavy metals in cigarette fillers were determined by inductively coupled plasma-mass spectrometry., Results: The level of PAH in the mainstream smoke from the privately imported cigarettes was higher than that in the smoke from the domestic cigarettes. However, the mutagenic activity of the mainstream smoke from the privately imported cigarettes was equivalent to that from the domestic cigarettes. The levels of nickel and cadmium in the fillers of the privately imported cigarettes were higher than those in the domestic cigarettes., Conclusion: The levels of constituents in the fillers and mainstream smoke from the privately imported cigarettes were higher than those in the fillers and mainstream smoke from the domestic cigarettes. The majority of Japanese smokers are unaware of these findings. The guidelines regulating tobacco products recommend that articles 9 and 10 of the World Health Organization (WHO) Framework Convention on Tobacco Control should be fully implemented in Japan.

We have developed a new analytical method for the determination of nicotine, tar, volatile organic compounds and carbonyls in main-stream cigarette smoke using a sorbent cartridge packed with Carboxen 572 (CX-572) and a Cambridge filter pad (CFP) followed by the two-phase/one-pot elution method. A CX-572 cartridge is installed between the intake of the CFP and the pump of the smoking machine. Gaseous compounds collected with the CX-572 cartridge and total particulate matter (TPM) collected with the CFP are coeluted simultaneously in the same vial and then analyzed by high-performance liquid chromatography (HPLC), gas chromatography-mass spectrometry (GC/MS) and gas chromatograph-thermal conductivity detector (GC/TCD). Carbonyl compounds are determined by adding derivatizing reagent (2,4-dinitrophenylhydrazine, DNPH) to the eluate followed by HPLC analysis. VOCs and nicotine are determined by GC/MS, and water is determined by GC/TCD. The same sample eluate solution is used for HPLC, GC/MS and GC/TCD analyses. As a result of measuring main-stream cigarette smoke generated from reference cigarettes, almost all carbonyl compounds and VOCs except formaldehyde were passed through a CFP and trapped in a CX-572 cartridge. 100% of nicotine, tar and TPM were trapped in a CFP. 50% of water and 53% of formaldehyde were trapped in a CFP. The one-pot data is almost equal to the sums of CFP (particulate matter) and CX-572 (gaseous compounds) data. The two-phase/one-pot elution method can simultaneously measure nicotine, tar, volatile organic compounds and carbonyl compounds in cigarette smoke with simple operation and small amounts of reagents., (Copyright © 2015 Elsevier B.V. All rights reserved.)

Objective: The tobacco tax in Japan was increased in October, 2010. Subsequently, the quantity of sales of domestic cigarette products decreased temporarily. However, smokers could import cigarettes directly through the internet. Because of the high value of the yen and the low price of foreign cigarettes, an individual could import cigarettes easily; however, the contents and emissions from privately imported cigarettes have not been investigated yet. In this study, we carried out a comparative analysis of domestic and privately imported cigarettes., Methods: Privately imported cigarettes from five brands and domestic cigarettes from the brand "Mild Seven" were selected for the study. For the fillers of the cigarettes, the levels of nicotine and tobacco-specific nitrosamines (TSNAs) were determined by methods that are usually used for cigarette products. For the mainstream smoke, the levels of tar, nicotine, carbon monoxide, and TSNAs were also determined by the methods used for cigarettes., Results: The average nicotine and TSNA levels in the fillers of the domestic cigarettes were 15.1 ± 0.19 mg/g and 1,920 ± 85.1 ng/g, respectively. The amounts of nicotine and tar in the mainstream smoke from the privately imported cigarettes were lower than those from the domestic cigarettes. However, the levels of TSNAs in the mainstream smoke from the privately imported cigarettes were higher than those from the domestic cigarettes., Conclusions: The amounts of TSNAs in the fillers of and mainstream smoke from the privately imported cigarettes were higher than those from the domestic cigarettes. Japanese smokers should be careful about consuming privately imported cigarettes because there is a variation in the amount of hazardous constituents in these cigarettes, even when they are from the same brand.

We developed a simple method for the simultaneous determination of volatile organic compounds (VOCs) and carbonyls in the mainstream cigarette smoke using a sorbent cartridge at ambient temperature without the traditional cryogenic impinger. A sorbent cartridge is installed between intake filter and the pump of the smoking machine. Collection of cigarette mainstream smoke is performed according to the Canadian Intense regime or the ISO regime. As adsorbent, Carboxen 572 (CX-572) is the most suitable for collection of VOCs and carbonyls in the mainstream cigarette smoke. Elution of VOCs and carbonyls from CX-572 is performed by the two-step elution with carbon disulfide and methanol. VOCs are eluted by first elution with carbon disulfide and carbonyls are eluted by second elution with methanol. For VOCs, a portion of eluate is analyzed by gas chromatography-mass spectrometry. For carbonyls, a portion of eluate is derivatized with enriched 2,4-dinitrophenylhydrazine solution and analyzed by high-performance liquid chromatography. Measurement values by CX-572 cartridge method are very close to those obtained by traditional impinger method except for 2-butanone. Impinger methods use 2,4-dinitrophenylhydrazine solution containing 50% water and 2-butanone-DNPhydrazone may be hydrolyzed with water. In the CX-572 method, the hydrolysis of 2-butanone is prevented because the eluate solution contains no water. CX-572 method can measure cigarette smoke resulting from not only one whole cigarette but also from one puff volume because of its high sensitivity and simple operation., (Copyright © 2013 Elsevier B.V. All rights reserved.)

Objectives: Mainstream smoke from cigarettes contains tobacco-specific N'-nitrosamines (TSNAs) listed as Group 1 and 3 carcinogens by the International Agency for Research on Cancer (IARC). Herein, we report on a method of measuring the concentrations of TSNAs in mainstream smoke from the ten top-selling Japanese cigarette brands using an ISO regime by International Organization for Standardization (ISO) and HCI regime of Health Canada., Methods: Tar in mainstream smoke was collected on a Cambridge filter pad using a smoking machine. The filter pad was immersed in 40 mL of ammonium acetate (pH 6.8) and shaken for 30 min. The extract was then loaded into a C18 column. After washing with 5 mL of 10% methanol and eluting with 5 mL of 70% methanol, the eluate was concentrated to 1 mL for LC-MS/MS analysis., Results: The concentrations of TSNAs in all cigarette brands were higher when determined using the HCI regime than when determined using the ISO regime. Furthermore, the concentrations of TSNAs measured using both the ISO and HCI regimes showed negligible correlation to the tar and nicotine concentrations indicated on package labels. The cigarette samples used in the study were categorized into four classes: ultralow-, low-, medium-, and high-yield brands, which corresponded to 1, 3-6, 8-10, and 14 mg tar/cigarette, respectively. The concentration of TSNAs in ultralow-yield cigarettes was 210 ng/cigarette, as measured using the HCI regime, which was nearly equal to that in high-yield cigarettes (180 ng/cigarette)., Conclusions: Exposure to TSNAs from mainstream smoke from ultralow-yield cigarettes is comparable to that from high-yield cigarettes. To properly evaluate the risk of smoking, not only the concentrations of tar and nicotine but also those of other chemicals, including TSNAs, should be printed on package labels.

A new method for the determination of acrolein and other carbonyls in cigarette smoke using a dual cartridge system has been developed. Each cartridge consists of reagent-impregnated silica particles. The first contains hydroquinone (HQ) for the inhibition of acrolein polymerization, while the second contains 2,4-dinitrophenylhydrazine (DNPH) for the derivatization of carbonyls. Smoke samples were firstly drawn through the cartridge containing HQ-impregnated silica (HQ-silica) and then through the DNPH-impregnated silica (DNPH-silica). Acrolein in the sample was completely trapped in the first HQ-silica cartridge. Some other airborne carbonyls were also trapped by the HQ-silica, and those that pass through were trapped in the second DNPH-silica cartridge. Extraction was performed in the reverse direction to air sampling. When solvent was eluted through the dual-cartridges, excess DNPH was washed into the HQ bed where it reacted with acrolein and other trapped carbonyls to form the corresponding hydrazone derivatives. All of the hydrazones derived from airborne carbonyls were completely separated and measured using high-performance liquid chromatography. This HQ-DNPH-method can be applied for the determination of acrolein and other alpha,beta-unsaturated aldehydes, such as crotonaldehyde, in cigarette smoke., (Copyright 2010 Elsevier B.V. All rights reserved.)

Introduction: There is no standardized aerosol exposure apparatus to deliver heated tobacco products (HTPs) for in vivo experiments. Therefore, we developed a novel HTPs aerosol exposure apparatus for mice and demonstrated that nicotine and other chemicals in HTPs aerosol generated by the apparatus can be delivered to mice which replicate human smoke.Aims and Methods: The amounts of nicotine, tar, and carbon monoxide (CO) in IQOS (Marlboro Regular HeatSticks) aerosol generated by two types of apparatuses were determined. C57BL/6N mice were exposed to IQOS aerosol, followed by determination of the urinary nicotine metabolites. Further, the skin surface temperature of mice was monitored to confirm the vasoconstriction action of nicotine.Results: The amount of chemicals in IQOS aerosol by the novel air push-in inhalation apparatus for HTPs (APIA) was equivalent to that of the analytical vaping machine (LM4E) (1.60 ± 0.08 [APIA] vs. 1.46 ± 0.07 mg/stick [LM4E] in nicotine and 0.55 ± 0.04 [APIA] vs. 0.45 ± 0.01 mg/stick [LM4E] in CO). After mice were exposed to IQOS aerosol by APIA, the urinary nicotine metabolite levels were determined; peak values in cotinine and 3-hydroxycotinine (3-HC) were 6.82 μg/mg creatinine at 1 hour after exposure and 32.9 μg/mg creatinine at 2 hours after exposure, respectively. The skin surface temperature decreased and was lower (33.5°C ± 0.5°C) at 30 minutes than before exposure (37.6°C ± 0.8°C).Conclusions: The new apparatus for HTPs aerosol exposure to mice showed good performances in terms of both chemical analysis of collected aerosol and fluctuations in the urinary nicotine metabolites.Implications: The APIA reported in this study can expose small animals to HTPs aerosol, including nicotine and other chemical substances as same amounts as LM4E and replicate actual human smoking process by in vivo experiments. Therefore, the experiments using APIA can provide evidence to assess the health risks of HTPs use. [ABSTRACT FROM AUTHOR]