This study aimed to select and optimize a sample extraction method for the determination of nitrite from milk powder. The absorbance of the experimental water stored for different periods of time was detected by three extraction methods, heat extraction, ultrasonic extraction and ultrasonic decolorization. The color and spiked recoveries of the filtrates from the three methods were evaluated. The nitrite content of quality control samples was determined by ultrasonic decolorization and the limit of detection (LOD) of this method was investigated. The results indicated that storage time did not affect the absorbance of the experimental water. The recoveries of the ultrasonic decolorization method were over 90%, with relative standard deviations (RSD) less than 10%. and the measured results of the quality control samples were within the characteristic value range with LOD of 0.4 mg/kg, which meets the laboratory quality control requirements. The ultrasonic decolorization method has good accuracy and accuracy, and it is recommended that it be used for the decolorization of colored substances in the national standard method.