<abstract xmlns="http://www.w3.org/1999/xhtml"><p>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.</p></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.

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

Indiana University-Purdue University Indianapolis, Department of Chemistry and Chemical Biology, 402 N. Blackford St., LD 326, Indianapolis, IN 46202, U.S.A

Alcohol and Tobacco Tax & Trade Bureau, Scientific Services Division, 6000 Ammendale Road, Beltsville, MD 20705, U.S.A.

Contributions to Tobacco & Nicotine Research

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

This paper describes the modification of an existing gas chromatographic (GC) method to incorporate simultaneous mass spectrometric (MSD) and flame ionization...

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

Published Online: Dec 30, 2014

Page range: 576 - 585

Received: Jan 25, 2013

Accepted: May 14, 2013

DOI: https://doi.org/10.2478/cttr-2013-0934

© 2013 Beiträge zur Tabakforschung International

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.