The paper describes the results of experimental studies using custom developed optical biopsy system for diagnostics in vivo during the procedure of fine needle aspiration biopsy. Experimental studies were conducted in laboratory mice with inoculated hepatocellular carcinoma. The measurements were carried out using fluorescence spectroscopy and diffuse reflectance spectroscopy methods to reveal metabolic and morphological changes in tissues. The results show that the developed approach is sensitive for cancer detection. Quantified differences in the maximum of fluorescence spectra and diffuse reflectance spectra between tumor and normal tissues were demonstrated and approved with morphological analysis