Using the conventional XAD 8/4method with general columns to isolate dissolved organic matter (DOM) is extremely time-consuming and labor-intensive. This study presents a rapid and effective method using solid-phase extraction (SPE) cartridges packed with XAD 8/4 resins for isolating various DOMs. The relative fraction (percentage hydrophobic, transphilic, and hydrophilic) of the various DOMs processed by both methods showed similar values. Moreover, changes in the molecular weight distribution of effluent fromXAD8/4 resins processed by bothmethods showed the same ultraviolet (UV) and fluorescence absorbance pattern s. The biopolymer compositions of eluates from XAD 8/4 resins also showed no significant difference between the two methods. However, higher carbon recovery of the isolation method using SPE cartridges was found (with columns: 88.9%; with SPE: 95.9%). In addition, the proposed method using SPE cartridges packed with XAD 8/4 resins is much faster than that using general columns (with columns: 1468 min; with SPE: 485 min). The proposed isolation method is highly efficient and accurate; it is an excellent candidate method for isolating various DOMs.