The quantitative analysis method for volatile impurities in diallyldimethylammonium chloride (DADMAC) monomer solution was established in this paper. The volatile impurities were quantitatively analyzed with trichloromethane as extraction solvent and n-hexane as internal standard by using gas chromatography (GC) coupled with solvent extraction, and the chromatographic conditions, quantitative methods, and extraction conditions were systematically investigated in detail. The results showed that excellent linear relationships of 5 volatile impurities (dimethylamine, allyldimethylamine, allyl chloride, allyl alcohol, and allyl aldehyde) were obtained in the range of 1-100 mg·L-1. The method also showed good specificity, recovery (95.0%-107.5%), and relative standard deviation (RSD, 1.40%-7.67%). This method could accurately detect the whole volatile impurities in DADMAC monomer solution quantitatively in one time with a low detection limit. Furthermore, this method is conducive to the preparation of highly pure DADMAC monomer and the development of national and international standards of the DADMAC monomer product quality, and the results could provide a strong foundation for the regulation and mechanism research of impurities on monomer reactivity in polymerization.