Abstract: A qualitative and quantitative analysis method for glucose degradation products (GDPs) in extraneal was established. The method involved the use of o-phenylenediamine (OPD) derivatization HPLC-DAD-MS/MS. The separation was performed on a Shim Pack Velox Biphenyl column (4.6 × 150 mm, 2.7 μm) at a column temperature of 50℃, with a flow rate of 1.0 mL/min. The mobile phase consisted of methanol (phase B) and 5 mmol/L ammonium formate (adjusted to pH 2.85 with formic acid, phase A) using gradient elution. Six GDPs were identified in extraneal, including 3-deoxyglucosone (3-DG), 3-Deoxy-galactosone (3-DGal), 4-deoxyglucosone (4-DG), furfural, 5-hydroxymethylfurfural (5-HMF), and 3, 4-dideoxyglucosone-3-ene (3, 4-DGE). To determine the content of α-dicarbonyl compounds in extraneal, a quantitative analysis method by OPD derivatization HPLC-MS/MS was further established. A SCIEX TRIOLE QUAD 3500 triple quadrupole mass analyzer was used, and multiple reaction monitoring (MRM) scanning was performed in the positive electrospray ionization (ESI) mode. The derivatization conditions were as follows: the analytes reacted with OPD (concentration of 1 mg/mL) in a methanol: water (2: 8, v: v) system at room temperature for 2 hours. Method validation results showed that the method have good specificity, linearity, accuracy, and precision. The limits of detection (LOD) for glucosone, 3-DG, 3-DGal, and 3, 4-DGE were 4.97 ng/mL, 2.44 ng/mL, 4.75 ng/mL, and 0.50 ng/mL, respectively, and the limits of quantification (LOQ) were 9.94 ng/mL, 4.88 ng/mL, 9.50 ng/mL, and 1.00 ng/mL, respectively. In conclusion, the method established in this study can effectively and accurately detect α-dicarbonyl glucose degradation products in extraneal, which is of great significance for its quality control.