Abstract: The flame atomic fluorescence spectrometry (FAFS) and inductively coupled plasma mass spectrometry (ICP-MS) were used to determine cadmium in lead-zinc ores. Through comparative study, the correlation coefficients of calibration curves of the two methods were good (r>0.999 5), and the limit of detection, accuracy, and precision of the methods met the requirements of the quality specifications. After comparing the actual samples of lead-zinc ores, there were no significant difference between the two methods. Compared to ICP-MS, the FAFS has shorter measurement time and higher precision, making it suitable for the determination of large quantities of lead-zinc ore samples.