Set up a microwave digestion-inductively coupled plasma mass spectrometry and hydride atomic fluorescence spectrometry determination of arsenic，mercury，selenium，antimony in food.Digestion conditions，working conditions of the instrument was optimized by testing the inductively coupled plasma mass spectrometry and atomic fluorescence spectrometry as a method of comparison research，comparison of both linear range，accuracy，precision，etc.In the optimization of experimental conditions，the use of national standards of material test and verify the reliability of the two methods and accuracy，measurements are according with the standard values.The results show that the two methods of high accuracy，good precision and high sensitivity has a strong comparability，etc.