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.