Objective:In order to increase the added value of crayfish by-products.Methods:With chromatographic peaks and peak areas as the inspection indicators, the optimization on equilibrium time, addition of sodium chloride, extraction time and extraction temperature were optimized, and the composition of volatile flavor compounds was analyzed.Results:The optimal extraction conditions were equilibrium time 0 min, extraction temperature 75 ℃, extraction time 50 min, addition of sodium chloride 30% with 50/30 μm DVB/CAR/PDMS solid phase microextraction head. Under these conditions, a total of 34 volatile flavor compounds, including 5 alcohols, 12 aldehydes, 5 alkanes, 5 aromatic, 5 heterocyclic compounds and 2 esters, were detected in the crayfish boiled liquid. The total peak area was 5.54×108, and the comprehensive score was 95.47. The relative error between the experimental results and the predicted value was 4.53%.Conclusion:The 34 volatile flavor compounds can be extracted from the crayfish boiled liquid by headspace solid phase microextraction.