Abstract
A gas chromatography–mass spectrometry (GC–MS) method was validated for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) from the FDA list of 93 harmful or potentially harmful constituents of mainstream cigarette smoke (MCS). Target analytes were extracted from total particulate matter using accelerated solvent extraction with a toluene/ethanol solvent mixture. Matrix artefacts were removed by two-step solid-phase extraction process. Three different GC–MS systems [GC–MS (single quadrupole), GC–MS/MS (triple quadrupole) and GC–HRMS (high resolution, magnetic sector)] using the same separation conditions were compared for the analysis of MCS of 3R4F Kentucky reference cigarettes generated under ISO and intense smoking regimes. The high mass resolution (m/∆m ≥ 10,000) and associated selectivity of detection by GC–HRMS provided the highest quality data for the target PAHs in MCS. Owing to the HR data acquisition mode enabling measurement of accurate mass, limits of quantification for PAHs were 5 to 15-fold lower for GC–HRMS than for GC–MS/MS and GC–MS. The presented study illustrates that the optimised sample preparation strategy followed by GC–HRMS analysis provides a fit-for-purpose and robust analytical approach allowing measurement of PAHs at (ultra)low concentrations in MCS. Furthermore, the study illustrates the importance and benefits of robust sample preparation and clean-up to compensate for limited selectivity when low-resolution MS is used.
Highlights
Mainstream cigarette smoke (MCS) is an extremely complex aerosol comprising of vapour phase and particulate phase [1]
Visual inspection of the Cambridge filter pad (CFP) after extraction indicated that a more polar solvent such as methanol might extract Total Particulate Matter (TPM) more efficiently from the CFP compared with the non-polar cyclohexane (TPM residues remained visible on the pad)
Masala et al [27] reported 2–17× higher concentrations of Polycyclic aromatic hydrocarbons (PAHs) found in diesel particular matter when a solvent system of toluene/ethanol (9:1, v/v) coupled to Accelerated Solvent Extraction (ASE) was used compared to toluene [27]
Summary
Mainstream cigarette smoke (MCS) is an extremely complex aerosol comprising of vapour phase and particulate phase (total particulate matter, TPM) [1]. MCS contains over 6500 compounds [2], more than 100 of which are established toxicants [3]. Polycyclic aromatic hydrocarbons (PAHs) are a class of compounds containing hydrogen and carbon that comprise multiple aromatic rings. PAHs are formed during the incomplete combustion of organic material such as gas, coal, wood, tobacco and even chargrilled meat. PAHs do not occur naturally in tobacco plants; they can be introduced during tobacco curing and deposited from vehicle exhaust during transport [4–6]. PAHs are further formed during cigarette combustion—more than 500 different PAHs have been identified in cigarette smoke at yields varying from sub-ng/cigarette to μg/cigarette [2]
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