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The potential toxicity and biocompatibility of sodium yttrium fluoride, erbium and ytterbium doped (NaYF4: Er 3+ , Yb 3+ ) upconversion nanoparticles are of great importance for their biomedical applications. In this work, the acute toxicity of sodium yttrium fluoride, erbium and ytterbium doped (NaYF4: Er 3+ , Yb 3+ ) upconversion nanomaterials toxicity was evaluated. Rats received intravenous injection of 10 mg/kg of NaYF4: Er 3+ , Yb 3+ doped upconversion nanoparticles once dose and were observed at two different times (24 hours and 14 days post injection) for acute toxicity compared with control group. The results of hematological, blood biochemical analyses indicated that NaYF4: Er 3+ , Yb 3+ doped upconversion nanoparticles treated rats survived for 14 days without any evident of toxic effects. Histopathological analysis of major organs including liver had no obvious signs of abnormality after intravenous injection of rats by NaYF4: Er 3+ , Yb 3+ doped upconversion nanoparticles.