Simultaneous Analysis of 22 Volatile Organic Compounds in Cigarette Smoke Using Gas Sampling Bags for High-Throughput Solid-Phase Microextraction

Abstract

Quantifying volatile organic compounds (VOCs) in cigarette smoke is necessary to establish smoke-related exposure estimates and evaluate emerging products and potential reduced-exposure products. In response to this need, we developed an automated, multi-VOC quantification method for machine-generated, mainstream cigarette smoke using solidphase microextraction gas chromatography–mass spectrometry (SPME-GC–MS). This method was developed to simultaneously quantify a broad range of smoke VOCs (i.e., carbonyls and volatiles, which historically have been measured by separate assays) for large exposure assessment studies. Our approach collects and maintains vapor-phase smoke in a gas sampling bag, where it is homogenized with isotopically labeled analogue internal standards and sampled using gas-phase SPME. High throughput is achieved by SPME automation using a CTC Analytics platform and custom bag tray. This method has successfully quantified 22 structurally diverse VOCs (e.g., benzene and associated monoaromatics, aldehydes and ketones, furans, acrylonitrile, 1,3-butadiene, vinyl chloride, and nitromethane) in the microgram range in mainstream smoke from 1R5F and 3R4F research cigarettes smoked under ISO (Cambridge Filter or FTC) and Intense (Health Canada or Canadian Intense) conditions. Our results are comparable to previous studies with few exceptions. Method accuracy was evaluated with third-party reference samples (≤15% error). Short-term diffusion losses from the gas sampling bag were minimal, with a 10% decrease in absolute response after 24 h. For most analytes, research cigarette inter- and intrarun precisions were ≤20% relative standard deviation (RSD). This method provides an accurate and robust means to quantify VOCs in cigarette smoke spanning a range of yields that is sufficient to characterize smoke exposure estimates.

Distinguishing Petroleum (Crude Oil and Fuel) From Smoke Exposure within Populations Based on the Relative Blood Levels of Benzene, Toluene, Ethylbenzene, and Xylenes (BTEX), Styrene and 2,5-Dimethylfuran by Pattern Recognition Using Artificial Neural Networks

“…Cigarette tobacco smoke BTEXS and 2,5-dimethylfuran levels used in this study were quantified using Tedlar bag collection of machine smoked cigarettes followed by equilibrium headspace SPME/GC/MS analysis as described elsewhere (Sampson et al 2014). These cigarette smoke VOC levels were generated using the ISO (3308:2012) and Canadian Intense (CI) protocols from 50 U.S. brand varieties of cigarettes from brand families that comprise 78% of the market share at the time of the sampling (Pazo et al 2016).…”

Simultaneous Determination of Furan and Vinyl Acetate in Vapor Phase of Mainstream Cigarette Smoke by GC-MS

“…Up to now, the major trapping methods of furan in vapor phase of mainstream cigarette smoke were direct injection method (Hatzinikolaou et al 2006, Grob et al 1965, Vickroy et al 1976) and gas bag trapping method (Sampson et al 2014). Grob et al (1965) reported on determination of furan in cigarette smoke directly through a gas sampling valve by gas chromatography (GC) coupled with flame ionization detector (FID) without sample collection.…”

“…However, soft photoionization and puff-by-puff analysis were adopted in their reports, which made these methods complicated and difficult to operate. Sampson et al (2014) reported a method that the vapor phase of mainstream cigarette smoke was collected by a gas bag, and furan was detected by solidphase microextraction gas chromatography -mass spectrometry (SPME-GC-MS). And the emissions of furan in the research cigarettes (1R5F and 3R4F) under ISO and CI smoking regimens were reported.…”

“…And the emissions of furan in the research cigarettes (1R5F and 3R4F) under ISO and CI smoking regimens were reported. However, the SPME technique made the method difficult to operate and time-consuming (Sampson et al 2014).…”

“…The major trapping methods of VA in vapor phase of mainstream cigarette smoke are direct injection (Norman et al 1968), cold trap (Diekmann et al 2002) and gas bag trapping combining with solid-phase microextraction (SPME) (Sampson et al 2014). The VA content in cigarette smoke could be determined by GC-MS. Norman et al (1968) reported a method that the VA form mainstream cigarette smoke was quantitatively analyzed by GC-FID, but no VA was detected in the vapor phase of mainstream cigarette smoke under ISO smoking conditions because of its poor sensitivity and selectivity.…”