The invention discloses preparation of a hydrophobic low-temperature co-melt and a method for extracting Congo red, acid golden yellow and red 2G from meat products and aquatic products. The inventionbelongs to the technical field of food detection. In order to solve the problems of tedious steps, high reagent consumption, high possibility of causing respiratory tract injury to personnel and thelike in the traditional method, the method comprises the steps of mixing a hydrogen bond receptor and a hydrogen bond donor, heating until the mixture is completely changed into transparent clear liquid, and cooling to room temperature. The detection method comprises the steps of taking a dry sample, adding water for ultrasonic treatment, centrifuging and taking a supernatant; mixing, whirling andstanding the hydrophobic low-temperature co-melt and all the supernatant to generate oily liquid drops, sucking all the oily liquid drops, dissolving with acetonitrile, fixing the volume, and filtering with a microporous organic filter membrane to obtain a filtrate; and measuring the filtrate by using a liquid chromatograph-mass spectrometer. Under the condition that the detection rate is guaranteed, the detection efficiency is greatly improved, the detection cost is reduced, the test steps are greatly simplified, and the detection method is good in applicability and stability.