Abstract: Proposes the method utilizing β-cyclodextrin cross-linking polymer enrich phenyl-mercury in sample water，chooses ethanol to elutriate off the enriched phenyl-mercury，and uses hydride-generation atomic fluorescence spectrometry method to quantitatively analyse digestive product，through experiment to optimize the chemical and instrument conditions. Discusses the influence of brominating agent dosage and brominating time to digestive rate，the influence of oscillating time to adsorption rate，the inflence of eluting time to eluting rate，discusses the factors such as the interference of concomitant ions，the precision and the detection limit，analyses the sample and draws the standard curve. The method is sensitive，selective and precise，the detection limit is 0. 36 ng/mL and RSD is 2. 29%（n = 10，c = 4 ng/mL）.

Key words: β-cyclodextrin cross-linking polymer, phenyl-mercury, hydride-generation, atomic fluorescence spectrometry