A method for the simultaneous determination of arsenic, antimony, lead and mercury in cosmetics by microwave digestion atomic fluorescence spectrometry was established. After the sample solution was decomposed by microwave digester, acid was removed at 120 ℃ on the pretreatment heater. And then arsenic, antimony, lead and mercury were simultaneous determined by hydride generation dual channel atomic fluorescence spectrometer with 1.0% nitric acid as carrier and 5.0% thiourea-ascorbic acid as reductant. The results show that the linearity of arsenic, antimony, lead and mercury is good in the corresponding concentration range, and the correlation coefficients R 2 are 0.999 3, 0.998 4, 0.997 3 and 0.999 7, respectively. The recovery of four elements is 91.7%-101.9%. This method has the advantages of simple operation, fast speed, wide linear range and strong applicability.