Headspace solid-phase microextraction coupled to comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry for the analysis of aerosol from tobacco heating product

Abstract

A method involving headspace solid-phase microextraction (HS-SPME) and comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-TOFMS) was developed and optimised to elucidate the volatile composition of the particulate phase fraction of aerosol produced by tobacco heating products (THPs). Three SPME fiber types were studied in terms of extraction capacity and precision measurements. Divinylbenzene polydimethylsiloxane appeared as the most efficient coating for these measurements. A central composite design of experiment was utilised for the optimization of the extraction conditions. Qualitative and semi-quantitative analysis of the headspace above THP aerosol condensate was carried out using optimised extraction conditions. Semi-quantitative analyses of detected constituents were performed by assuming that their relative response factors to the closest internal standard (t) were equal to 1. Using deconvoluted mass spectral data (library similarity and reverse match >750) and linear retention indices (match window of ±15 index units), 205 peaks were assigned to individual compounds, 82 of which (including 43 substances previously reported to be present in tobacco) have not been reported previously in tobacco aerosol. The major volatile fraction of the headspace contained ketones, alcohols, aldehydes, alicyclic hydrocarbons alkenes, and alkanes. The method was further applied to compare the volatiles from the particulate phase of aerosol composition of THP with that of reference cigarette smoke and showed that the THP produced a less complex chemical mixture. This new method showed good efficiency and precision for the peak areas and peak numbers from the volatile fraction of aerosol particulate phase for both THP and reference cigarettes.

Levels of selected analytes in the emissions of “heat not burn” tobacco products that are relevant to assess human health risks

“…Their determined levels for nicotine, TPM, and water are comparable to ours. Another group developed a headspace solid-phase microextraction-based method for semi-quantitative assessment of VOCs emitted by HNB products (Savareear et al 2017). The issue of toxicant reduction is complex, since these calculations depend on the reference product.…”

Qualitative Analysis of E-Liquid Emissions as a Function of Flavor Additives Using Two Aerosol Capture Methods

“…Analysis was performed to determine if the peaks were being obscured by the glycerol peak and no major signals were found. If one were attempting to detect as many species as possible, using GC techniques to reduce the intensity of the glycerol peak could be used, such as using the heart-cutting system with Deans Switch, as has been done previously for the qualitative analysis of e-cigarette emissions using thermal desorption gas chromatography [ 14 ]. In addition, there were five compounds that were only observed in the filter pads and one only observed in the e-liquid.…”

“…Additionally, several commercially available puffing machines, including Vitrocell [ 2 , 4 , 6 ], Cerulean [ 5 ], Borgwaldt [ 7 ], Teague Enterprises [ 10 ], and CH Technologies [ 8 ], and some non-commercial machines [ 1 , 3 , 9 ] have been employed to generate emissions. A number of prior reports have also qualitatively determined the composition of e-cig emissions using a single type of sampling technique [ 9 , 13 , 14 , 15 ]. The majority of prior studies do not report attempts to validate the puffing machine itself, and its interaction with the e-cig being tests.…”

Urinary volatomic profile of traditional tobacco smokers and electronic cigarettes users as a strategy to unveil potential health issues

“…The aldehydes found in urine are produced during lipid peroxidation of lipid alkoxyl radicals and are common constituents of natural flavors of foods and beverages [38,46]. Nevertheless, aldehydes can be formed during smoking from precursors of polysaccharides, pectins, proteins, and possibly, triglycerides present in tobacco [47]. They constitute a group of reactive compounds responsible for damaging the respiratory tract [12,26].…”