Abstract: With the development of nuclear energy, tritium and ¹⁴C have become the main radionuclide emissions to the environment, and get more and more attention of people. Therefore, the monitoring technique about organic tritium and ¹⁴C in environmental biological medium becomes the key point for the monitoring work, and how to extract organic tritium and ¹⁴C in biological samples is the key for monitoring and analysis work. This article provides the method to extract and measure the organic tritium and ¹⁴C by oxidation combustion, then to measure. The measured results show that the device blank recovery rate can reach 87.1% and 96.4%; the standard addition recovery rate can reach 84.8% and 95.7% respectively. The specific activity of organic tritium and ¹⁴C in biological samples of pine needles are (8.89±0.54) Bq/kg (fresh weight, 3.19 Bq/L, n=3) and (22.2±1.90) Bq/kg (fresh weight, 0.150 Bq/g (carbon), n=3); and the detection lower limits of organic tritium and ¹⁴C are 4.04 Bq/kg (fresh weight, 1.29 Bq/L) and 14.3 Bq/kg (fresh weight, 0.096 Bq/g (carbon)); and the expanded uncertainty of this analysis method of organic tritium and ¹⁴C are 25.6% and 39.4% (k=2) respectively. Analysis results have the same level with similar biological samples, and the analysis results are reliable.