The invention relates to a method for determining 
chloramphenicol in freshwater pond 
sediment by applying a liquid chromatograph / 
mass spectrometer. The method comprises the following steps of firstly, collecting a 
sediment sample of an 
aquaculture pond; secondly, extracting the sample; thirdly, purifying with n-
hexane; fourthly, extracting water saturated 
ethyl acetate solution; fifthly, blowing extracting solution to be dry with 
nitrogen gas, and dissolving the dry extracting solution with 
acetonitrile-water (5+95) to obtain standby solution; sixthly, performing 
solid phase extraction column for eluting; seventhly, extracting the water saturated 
ethyl acetate solution, and blowing dry with the 
nitrogen gas; eightly, dissolving 
methanol water (50+50), whirling, filtering by a 
microfiltration membrane of 0.22[mu]m and determining by using the liquid chromatograph / 
mass spectrometer. According to the method disclosed by the invention, by pretreatment for the freshwater pond 
sediment, a matrix disturbing substance is removed, the sensitivity is improved, and the pretreatment process is optimized; in addition, the sample is prevented from being derivaed, so that the operation step is simplified; a reliable detection means can be provided for checking a 
pollution source and evaluating the influence of the 
ecological environment on healthy breeding.