E-cigarettes are gaining popularity in the U.S. as well as in other global markets. Currently, limited published analytical data characterizing e-cigarette formulations (e-liquids) and aerosols exist. While FDA has not published a harmful and potentially harmful constituent (HPHC) list for e-cigarettes, the HPHC list for currently regulated tobacco products may be useful to analytically characterize e-cigarette aerosols. For example, most e-cigarette formulations contain propylene glycol and glycerin, which may produce aldehydes when heated. In addition, nicotine-related chemicals have been previously reported as potential e-cigarette formulation impurities. This study determined e-liquid formulation impurities and potentially harmful chemicals in aerosols of select commercial MarkTen(®) e-cigarettes manufactured by NuMark LLC. The potential hazard of the identified formulation impurities and aerosol chemicals was also estimated. E-cigarettes were machine puffed (4-s duration, 55-mL volume, 30-s intervals) to battery exhaustion to maximize aerosol collection. Aerosols analyzed for carbonyls were collected in 20-puff increments to account for analyte instability. Tobacco specific nitrosamines were measured at levels observed in pharmaceutical grade nicotine. Nicotine-related impurities in the e-cigarette formulations were below the identification and qualification thresholds proposed in ICH Guideline Q3B(R2). Levels of potentially harmful chemicals detected in the aerosols were determined to be below published occupational exposure limits.

Peanut stems and leaves have been used traditionally as both herbal medicines and special food in Asia. In this study, the main functional compounds of peanut stems and leaves extracts were identified using UPLC separation coupled to high resolution mass spectrometry (QTOF-MS), and a traditional medicine library. Three different extraction solvents (ethyl acetate, petroleum ether and n-butanol) were evaluated to prepare the extracts of peanut stems and leaves. A total of 283 chemical compounds were identified in peanut stems and leaves extracts, of which 207 compounds are tentatively new identifications in Genus Arachis. The integration of data acquisition and processing with the traditional medicine library provides a simple, efficient process to effectively facilitate the identification of chemical ingredients in complex natural product extracts. The integrated workflow for separation, detection and identification of functional compounds in natural products using UPLC/QTOF-MS greatly improves productivity for development of traditional herbal medicines. Copyright © 2016 John Wiley & Sons, Ltd.

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Several microbial volatile organic compounds (MVOCs) that can serve as potential chemical markers for microbial contamination in tobacco have been identified. Four different fungal species, Aspergillus niger (AN), A. ornatus (AO), Pencillium chrysogenum (PC) and Rhizopus stolonifer (RS), commonly reported in moldy tobacco were cultured and screened for MVOCs. Because the MVOCs emitted by a microbial species are substrate specific, the fungal strains were separately grown on potato dextrose agar (PDA) and tobacco products. MVOCs from the mold cultures grown on PDA and tobacco products were extracted using closed-loop stripping analysis (CLSA) and identified by gas chromatography/time-of-flight mass spectrometry (GC/TOF-MS). Some of the prominent tobacco mold markers identified by this method include: 1-octen-3-ol; 2-octen-1-ol; 2-methyl-1-butanol; 3-methyl-1-butanol; 1-octene and 2-pentanone. In particular, 1-octen-3-ol was detected in all the mold cultures and moldy tobacco samples analyzed. Olfactory evaluation of 1-octen-3-ol indicated a characteristic musty odor and the odor threshold was determined to be approximately 200 ng/ml. The limits of detection for 1-octen-3-ol using GC/TOF-MS and GC/mass selective detector (MSD) in the full-scan mode and selected ion monitoring (SIM) mode were investigated. The CLSA-GC/TOF-MS demonstrates a fast, sensitive and semi-quantitative analytical technique for screening tobacco materials for the presence of mold via chemical markers of microbial contamination.

The USA Food and Drug Administration (FDA) established benzo[a]pyrene (B[a]P) as a harmful and potentially harmful constituent (HPHC) found in tobacco products. Tobacco manufacturers are required to report HPHC quantities to the FDA; however, there is currently no standardized method for determination of B[a]P in smokeless tobacco products (STPs). This work details a sensitive, selective and rapid method for the determination of B[a]P in STPs, cigarette filler and tobacco. Tobacco is extracted using methanol followed by solid-phase extraction and concentration prior to analysis by gas chromatography/mass spectrometry in the selected ion monitoring mode. Cooperation Centre for Scientific Research Relative to Tobacco reference products and 3R4F Kentucky reference cigarette filler were used for method validation. All method validation requirements were met including linearity, accuracy, precision, robustness, limit of detection (LOD) and limit of quantitation (LOQ), and stability. Calibration range of 0.5-125 ng mL-1 was achieved with the coefficient of determination (R2) greater than 0.995. The method LOQ and LOD were 0.729 and 0.216 ng/g, respectively. Using standardized methods for the measurement of HPHCs in tobacco products will reduce variability and ensure accurate data for regulatory reporting.