Determination of toxic glycols and alcohols in an emergency setting requires a rapid yet accurate and reliable method. To simultaneously determine diethylene glycol (DEG) along with ethylene glycol, methanol, isopropanol, acetone, and ethanol, we modified a previously developed gas chromatographic (GC) method. The system used a Hewlett-Packard 6890 GC with EPC, a Gooseneck splitless liner, and an Rtx-200 capillary column (30 m x 0.53-mm i.d., 3 mm). After serum samples were deproteinized using ultrafiltration (Millipore Ultrafree-MC), 1 mL of the protein-free filtrate was manually injected into the GC. Internal standards for alcohols (and acetone) and glycols were n-propanol and 1,3-butanediol, respectively. All compounds eluted within 3.5 min (linear temperature gradient from 40 to 260 degrees C); total run time was 6.5 min. Limit of detection and linear range for all compounds were 1 or 2.5 mg/dL and 0-500 mg/dL, respectively. In addition, there was no interference from propionic acid, propylene glycol, and 2,3-butanediol. The modifications in the equipment and temperature program allowed increased resolution and thus, detection and reliable quantitation of DEG and other common toxic glycols and alcohols of clinical interest.