The invention relates to a method for determining five ultra-short chain perfluorinated compounds in agricultural products, which comprises the following steps: S1, weighing 1.00-5.00 g of homogeneous sample in a first
centrifuge tube, adding a certain amount of
internal standard and 1-5 mL of
ultrapure water, and carrying out vortex mixing for 1 min; s2, continuing to add 10 mL of 2%
formic acid acetonitrile, homogenizing at a high speed for 1 min, adding a
QuEChERS pretreatment bag, performing rapid vortex mixing uniformly, and performing high-speed
centrifugation for 5 min; s3, transferring the
acetonitrile on the upper layer into a second centrifugal tube filled with a purifying agent, carrying out full vortex, and carrying out high-speed
centrifugation for 5 minutes; s4, 5 mL of supernate is taken and put into a third centrifugal tube,
nitrogen blowing is performed at the temperature of 45 DEG C until the supernate is dry, 1 mL of
methanol water with the volume ratio being 1: 1 is added for constant volume,
centrifugation is performed at the high speed of 12000 r / min for 10 min, and supernate is sucked and passes through a 0.22-micron filter membrane; and S5, detecting the supernate passing through the filtering membrane in the step S4 by liquid
chromatography-
tandem mass spectrometry. Due to the adoption of the technical scheme, the method for determining the five ultra-short-chain perfluorinated compounds in the agricultural product can be used for simultaneously determining the five ultra-short-chain perfluorinated compounds in the agricultural product.