Abstract: A total of 32 pyrotechnic powder samples from 11 provinces were collected. In order to discriminate of samples from different regions, 40 elements in the samples were determined by inductively coupled plasma mass spectrometry (ICP-MS), and principal component analysis (PCA) was performed for elements with significant differences. Meanwhile, oxygen isotope ratio (δ¹⁸O value) was analyzed by elemental analysis-isotope ratio mass spectrometer. It was shown that the contents of elements in the samples from different regions had certain characteristics, and most different samples could be distinguished according to the analysis results of PCA. As shown by the results of δ¹⁸O value, samples from different regions had certain oxygen isotope characteristics, and the δ¹⁸O values of samples from different regions overlapped. In the distinction of samples from different regions, the content of elements and oxygen isotope ratios could corroborate each other. The both analysis results could realize the full discrimination of samples from different sources.