Quantitative Analysis of Humectants in Tobacco Products Using Gas Chromatography (GC) with Simultaneous Mass Spectrometry (MSD) and Flame Ionization Detection (FID)

Abstract

This paper describes the modification of an existing gas chromatographic (GC) method to incorporate simultaneous mass spectrometric (MSD) and flame ionization detection (FID) into the analysis of tobacco humectants. Glycerol, propylene glycol, and triethylene glycol were analyzed in tobacco labeled as roll-your-own (RYO), cigar, cigarette, moist snuff, and hookah tobacco. Tobacco was extracted in methanol containing 1,3-butanediol (internal standard), filtered, and separated on a 15 m megabore DB-Wax column. Post-column flow was distributed using a microfluidic splitter between the MSD and FID for simultaneous detection. The limits of detection for the FID detector were 0.5 μg/mL (propylene glycol and triethylene glycol) and 0.25 μg/mL (glycerol) with a linear range of 2-2000 μg/mL (propylene glycol and triethylene glycol) and 1-4000 μg/mL (glycerol). The limits of detection for the MSD detector were 2 μg/mL (propylene glycol and triethylene glycol) and 4 μg/mL (glycerol) with a linear range of 20-2000 μg/mL (propylene glycol and triethylene glycol) and 40-4000 μg/mL (glycerol). Significant improvement in the sensitivity of the MSD can be achieved by employing selective ion monitoring (SIM) detection mode. Although a high degree of correlation was observed between the results from FID and MSD analyses, marginal chromatographic resolution between glycerol and triethylene glycol limits the applicability of FID to samples containing low levels of both of these humectants. Utilizing MSD greatly improves the reliability of quantitative results because compensation for inadequate chromatographic resolution can be accomplished with mass selectivity in detection.

A Screening Method by Gas Chromatography-Mass Spectrometry for the Quantification of 24 Aerosol Constituents from Heat-Not-Burn Tobacco Products

“…For that reason, this constituent is also of interest. Usually, these compounds are analyzed using multiple analytical methods, with each method specific for an analyte or compound class (1), such as for phenolic compounds (5,6), volatiles (7-9), or humectants (10,11), each with a corresponding aerosol collection method (12), leading to a high workload for the assessment of aerosol from heat-not-burn prototypes (13).…”

An isotope dilution ultra high performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of sugars and humectants in tobacco products

“…Native sugars are also present in tobacco and these, along with added sugars, can impart palatable sensory attributes and make tobacco products more appealing, especially to children and youth [1]. Humectants retain moisture, extend the shelf life of tobacco products and facilitate the manufacturing process [2]. Sugars and humectants are considered safe in food products; however, sugars could serve as precursors for organic acids or harmful chemicals in smoke, such as acetaldehyde, formaldehyde, acrolein, acetone and 2-furfural, among others formed during combustion [3].…”

“…Clarke et al developed an LC-MS/MS method for the determination of sugars (including glucose, fructose, and sucrose) in tobacco products in which co-eluting sugar compounds from tobacco matrix can be resolved by mass spectrometry, if the compounds form ions with different mass-to-charge ratios [17]. Existing methods for humectant detection range from IC to GC to GC-MS [2, 10]. Tang et al developed an IC method, and applied it to analyze 12 sugars, alditols, and humectants in tobacco [9].…”

“…Tang et al developed an IC method, and applied it to analyze 12 sugars, alditols, and humectants in tobacco [9]. Rainey, et al concluded that a GC-MS method can compensate for the inadequate chromatographic resolution between the analyzed humectants [2]. …”

Stability and Concentrations of Humectants in Tobacco

“…While GLY occurs naturally in many varieties of plants, including tobacco, PG and tri-ethylene glycol (TEG) do not [4]. The humectant concentrations vary greatly among different cigarettes [5].…”