reactions by the mass shift method could eliminate spectral interferences. Compared with the O 2 and H 2 reaction modes, the present approach delivered much higher sensitivity and lower limit of detection (LOD) of the analytes. The accuracy of the developed method was evaluated via standard addition method and comparative analysis by sector field ICP-MS (SF-ICP-MS). The study indicates that in the MS/MS mode, use of N 2 O as reaction gas can provide interference-free conditions and sufficiently low LODs for analytes. The LODs of Si, P, S, and Cl could reach down to 17.2, 4.43, 10.8, and 31.9 ng L −1 , respectively, and the recoveries were in the range of 94.0−106%. The determination results of the analytes were consistent with those obtained by SF-ICP-MS. This study presents a systematic method for the precise and accurate quantification of Si, P, S, and Cl in high-purity Mg alloys by ICP-MS/MS. The developed method provides valuable reference that can be expanded and applied to other fields.