Abstract: To determine the concentration of trace vanadium in saline lake brines, a vanadium pre-purification process is established to reduce the matrix effect of the huge coexisting ions. Two steps, extraction and stripping, are included in the process. The factors affecting the vanadium purification efficiencies are investigated in detail and the optimum conditions are determined to be: vanadium in the solutions was extracted by the organic phase containing 30% D2EHPA (v/v), 20% TBP (v/v) in n-hexane for 30 min at pH 3.0, and then stripped with 3 mol/L H₂SO₄ for 10 min. Trace vanadium in two natural brine samples are pre-purified using this process and their concentrations are determined by inductively coupled plasma-mass spectrometry (ICP-MS) with sensitivity and limit of detection (LOD) for ⁵¹V are 53 171 cps/(µg/L) and 1.88 ng/L, respectively. The standard addition recoveries of the brine samples are ~100% but with small relative standard deviations (RSD<0.6%), indicating that the method can be used to measure the concentration of trace vanadium in natural complicated waters, such as seawater and saline lake brines.