The invention discloses a method for measuring residual quantity of 
diethylstilbestrol in aquatic products by utilizing a liquid chromatogram fluorescent method, comprising the following steps: (1) weighing 100g of ground 
aquatic product samples in a 50mL plastic 
centrifuge tube, adding 20mL of acetic 
ether, homogenizing for 230s, centrifuging for 10min with the speed of 7000r / min, moving the acetic 
ether layer to a 100mL 
pear-shaped flask, utilizing 2mL of normal 
hexane and acetic 
ether with a volume ratio of 85:15 to dissolve residue, and then stirring for 6min; (2) activating an SLH column by utilizing 5mL of normal 
hexane and 5mL of acetic ether, adding extracting solution on the SLH column, utilizing 10mL of normal 
hexane and acetic ether with the volume ratio of 82:20 to elute by controlling the flow rate at 2mL / min, collecting eluent, carrying water bath at the temperature of 450 DEG C, and then carrying out 
nitrogen drying till the original state; and (3) adding 1mL of 
sulfuric acid to the 
centrifuge tube of 
nitrogen drying, then adding 8mL of water in the 
centrifuge tube, utilizing 1mL of mobile phase for metering volume so as to be measured by an efficient 
liquid phase chromatogram. The method for measuring residual quantity of 
diethylstilbestrol in aquatic products has advantages of low cost, simple method, and low measuring limit, is suitable for popularization and use in the production and practice and is a technology demanded by the market, and has positive social meaning and social demand.