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Using triacontyl bonded silica（C30) as on-line solid-phase extraction（SPE) material and a specially designed online analytical system which allowed large sample volume injection，a high speed and robust online SPE-HPLC-MS method was established for the analysis of five estrogens and bisphenol A（BPA) in milk samples. The milk sample is pretreated with acetonitrile for protein precipitation and then treated with primary secondary amine for the removal of polar impurities in the matrix. Then the pretreated sample can be automatically loaded by a LC pump.