Abstract: To address the challenge in efficiently and accurately determining the moisture content of heated tobacco materials, accurate determination methods such as Karl Fischer, gas chromatography, and near-infrared spectroscopy were systematically compared and optimized. The mechanism of the effect of high doses of volatile substances on accuracy was investigated using glycerol as a representative. Based on this, a determination method and result correction models for the moisture content of heated tobacco material samples prepared by different production processes were established. The results showed that: 1) After optimizing the determination parameters, the spiked recoveries for Karl Fischer and gas chromatography methods were in the range of 99.50%-102.70% and 98.64%-108.70%, respectively. 2) To promote the efficiency of moisture content determination of heated tobacco materials during the production process, a polynomial moisture content correction model for using near-infrared spectrometry was established using the Karl Fischer method results as a baseline. The moisture content errors were reduced from 1.75% to 0.32% after the correction, which met the requirements for quality control in the actual production process. The combined Karl Fischer and near-infrared spectroscopy method is suitable for the moisture content determination in the whole process of heated tobacco material processing with both accuracy and efficiency, and easy to operate.