This paper describes a simple approach to determine gold nanoparticles in liver and river water samples. The method of purification of nanoparticles from the matrix is based on the stabilization of gold nanoparticles with a cationic surfactant followed by a microliquid-liquid extraction in ionic liquid. Finally, the extracted nanoparticles can be analysed by UV/Vis detection or Raman spectroscopy. The precision of the proposed method for the analysis of liver tissue and river water samples was 9.7% and 18% respectively for UV/Vis analysis. The sensitivity was 1.17 × 10(-12) M for the analysis of 3 mL of liver homogenate or river water sample.