As a new form of cigarettes, heated tobacco products (HTPs) have been rapidly distributed worldwide. In this study, an improved method for analyzing gaseous and particulate compounds generated from HTPs is described. Smoke is collected using a GF-CX572 sorbent cartridge with 300 mg of carbon molecular sieves, that is, Carboxen 572 (CX572), and a 9 mm glass-fiber filter (GF). After collection, the CX572 particles from the cartridge are transferred along with the GF and deposited into a vial containing two phases of carbon disulfide and methanol. The CX572 particles settle into the lower carbon disulfide phase, while nonpolar compounds are desorbed. After the sample is allowed to stand, the solution is slowly stirred. The two-phase mixture of carbon disulfide and methanol is combined into a homogeneous solution. Polar compounds are then desorbed, while the desorbed nonpolar compounds remain in solution. For the analysis of carbonyl compounds, an enriched 2,4-dinitrophenylhydrazine solution is added to a portion of the combined solution for derivatization and subsequent high-performance liquid chromatography analysis. For the analysis of volatile organic compounds and water, a portion of the combined solution is analyzed by gas chromatography-mass spectrometry or equipped with a thermal conductivity detector. By applying the proposed GF-CX572 one-cartridge method to the analysis of the mainstream smoke generated from HTPs and traditional cigarettes, several chemical compounds are detected, and the chemical composition of smoke is revealed. The GF-CX572 one-cartridge method can analyze gaseous and particulate chemical compounds from the HTP smoke by utilizing not only the entire puff volume but also one puff volume because the GF-CX-572 cartridge can be replaced with a new cartridge within 3 s. An overview of the chemicals generated from HTPs is obtained in detail by one-puff volume sampling. In addition, the generated chemical compounds strongly depend on the temperature of tobacco leaves in HTPs.
We developed an analytical method for analyzing electronic cigarette (E-cigarette) smoke, and measured the carbonyl compounds and volatile organic compounds generated by 10 brands of second-generation E-cigarettes. A glass filter (Cambridge filter pad) for particulate matter and a solid sorbent tube packed with Carboxen-572 for gaseous compounds were used to collect E-cigarette smoke. These were then analyzed using a two-step elution method with carbon disulfide and methanol, followed by high-performance liquid chromatography (HPLC) and gas chromatography mass spectrometry (GC/MS). Formaldehyde (FA), acetaldehyde (AA), acetone (AC), acrolein (ACR), propanal (PA), acetol (AT), glyoxal (GO), and methyl glyoxal (MGO) were detected by HPLC in some E-cigarettes. Propylene glycol (PG), glycerol (GLY), and some esters were detected by GC/MS. GO and MGO exist mainly as particulate matter. AA, AC, ACR, PA, and AT exist mainly as gaseous compounds. FA exists as both particulate matter and gaseous compounds. These carbonyl compounds have carbon numbers C1 - C3. The main components of E-liquid are PG (C3) and GLY (C3). Therefore, the oxidation of liquids, such as PG and GLY in E-cigarettes upon incidental contact with the heating element in E-cigarette, is suggested as being a possible cause for carbonyl generation. When the puff number exceeds a critical point, carbonyl generation rapidly increases and then remains constant. The results of this study are now being used to determine the following E-cigarette smoking protocol: puff volume, 55 mL; puff duration, 2 s; and puff number, 30. E-cigarette analysis revealed very large variation in carbonyl concentration among not only different brands, but also different samples of the same product. Typical distributions of carbonyl concentration were not observed in any of the E-cigarettes tested, and the mean values greatly differed from median values.
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