The invention discloses a method for measuring the diglycol content in glyceryl triacetate. The method comprises the following steps of: weighing one gram of glyceryl triacetate sample; fixing the volume of the glyceryl triacetate sample in a volumetric flask with the volume of 25 millimeters by using absolute alcohol; and uniformly shaking the volumetric flask; sieving by a 0.45-micron organic filter membrane so as to perform gas chromatopraphy-mass spectrometry (GC/MS) analysis. A ZB-WAX capillary column is used, a procedure temperature raising mode is adopted and an ion detection mode is adopted for mass spectrum measurement. Under conditions of optimal solvent selection and measurement, a linearity range of the method is 0.1 to 10.0 mu g/mL, a detection limit is 0.01 mu g/g, and a quantitation limit is 0.03 mu g/g; and a relative standard deflection (n=10) is less than 1.6 percent and a recycling rate is 93.0 to 106.0 percent. In the method, the diglycol content in the glyceryl triacetate can be directly measured by adopting the GC/MS; and the method has the advantages of simplicity in operation, quickness, accuracy, high senstivity and high repetitiveness.