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A facile and inexpensive method using solid phase extraction (SPE) on OASIS HLB and HPLC with fluorescence detector (FLD) determination of aflatoxin M-1 (AFM(1)) in liquid milk and milk powder was described. The detection limits of this method provided were 0.006 mu g/kg for liquid milk and 0.026 mu g/kg for milk powder. The recoveries obtained in all food matrices were between 85.4 and 96.9%, and the RSDs were between, 0.8 and 3.6%. Furthermore, a total of 31 samples were detected using OASIS HLB and immunoaffinity column (IAC) as a comparison, both cleanup methods obtained consistent results. The level of AFM(1) contamination found in 8 samples among the tested samples did not exceed the Chinese legal limit (0.5 mu g/kg). This method was applied successfully to analyse AFM(1) in liquid milk and milk powder without interference peaks. (C) 2012 Elsevier Ltd. All rights reserved.