Tobacco (1.0 g) from cigarettes was placed into a 20-mL head-space vial. Internal standard solution (2 μL of 1 μg/μL 2,6-dichlorotoluene) and flavor spike mixture (1 μL of 1 μg/μL each benzaldehyde, tetra-methylpyrazine, methanol, and anethole in ethanol) were added. The samples were sealed and allowed to equilibrate for 2 h at room temperature before analysis (59) |
Flavor additives to tobacco (e.g., menthol, anethole, benzaldehyde, and tetramethylpyrazine)Headspace solid-phase microextraction-gas chromatographymass spectroscopy (HS-SPME-GCMS) for both qualitative and quantitative analysis) |
Feasible but could be very tedious, time consuming & unproductive |
Benzaldehyde = 66 ng/gmethanol = 120 ng/ganethole = 16 ng/gtetramethylpyrazine = 163 ng/gacetophenone = 41 ng/g |
10.0 g tobacco sample was added to 40 ml dichloromethane. Then the mixture was shaken overnight and steam distillated for 3 h to obtain 800 mL aqueous solution of volatile components using a simple apparatus (60) |
Lactones, benzaldehyde, 6-methyl-2-heptanone, 2,4-dimethyl-1-penten-3-one, etc.Steam distillation (SD), simultaneous distillation and extraction (SDE) and headspace co-distillation (HCD)-GC-MS utilized for all volatiles |
Feasible but could be very tedious, time consuming & unproductive |
Total detected 315.72–445.48 μg/g |
Evaluation of volatiles from flue-cured tobacco varieties, smoke organoleptic (61) |
Lactones, benzaldehyde, 6-methyl-5-hepten-2-one, etc.Steam distillation of 10 g tobacco, capillary GC/GC-MS |
Distillation system must be available |
200–600 μg/g |
Smokeless tobacco products including snuff, plug tobacco, chewing tobacco, pellets, and snus (62) |
α- and β-angelica lactonesHeadspace gas chromatography mass spectrometry (HS-GC-MS) |
Feasible. However, reference standards for β-angelica lactone unavailable or difficult to obtain |
The limit of detection was 30 ng/g and limit of quantitation 65 ng/g with a variability of 9–44% (RSD) |
Tobacco samples used for analysis were Brazilian flue-cured, Kentucky Burley, N. rustica, and Greek and a sample of commercially available roasted peanuts (63) |
Benzaldehyde, 6-methyl-5-hepten-2-one, acetone, hexenal Chromatography-mass selective detection-flame ionization detection (PT-GC-MSD-FID) hyphenated technique with purge-and-trap-gas |
Feasible with little modification |
Semiquantitative and qualitative analysis |
Qualitative and quantitative analysis was developed and validated for volatile flavour components in flue-cured tobacco (64) |
Flavour components in flue-cured tobacco (e.g., pyridine, 6-methyl-5-hepten-2-one, benzene acetaldehyde, benzaldehyde, furfural)HS-SPME followed by GC × GC-TOF-MS |
Feasible but must have TOF-MS on scope |
5.7–147.6 ng/g |
Determination of selective phenolic compounds in cigarette and MMC cigar smoke (65) |
Phenolics (e.g. hydroquinone, resorcinol, phenol, catechol, and o-, m-, and p-cresol).Ultra-high pressure liquid chromatography (UHPLC) and fluorescence detector (FLD) with a sub-2 μm pentafluoro-phenylpropyl phase analytical column |
Feasible high throughput method that is based on CRM 78, which has a run time of 10 minutes |
Quantitative and qualitative analysis |