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This invention provides a method for detecting the diethyl sulfate content in methyl 4-acetamido-2-ethoxybenzoate. The method involves derivatizing the sample with sodium iodide-ascorbic acid and detecting the sample using a headspace gas chromatograph equipped with an ECD detector. The chromatographic column is an Agilent DB-624 30m × 0.53mm × 3μm column, the injection port temperature is 220℃, the detector temperature is 250℃, and the carrier gas is N2. 2， Flow rate: 1.5 mL / min, temperature programmed: initial column temperature 70℃, increased to 150℃ at a rate of 5℃ / min and held for 0 min; then run at 240℃ and held for 5 min, flow rate 3 mL / min. This invention provides a convenient, efficient, and accurate method for detecting the diethyl sulfate content in methyl 4-acetamido-2-ethoxybenzoate. This method uses gas chromatography to detect the diethyl sulfate content in methyl 4-acetamido-2-ethoxybenzoate, thereby effectively ensuring medication safety.