This thesis deals with fabrication of carboxymethyl chitosan nanofibers containing Doxorubicin anti-cancer drug first, and then the release of Doxorubicin from the nanofibrous matrix of carboxymethyl chitosan is discussed. The nanofibrous carboxymethyl chitosan mat samples produced by electrospinning in this work consisted of 16.7, 25 and 34% (W/W) Doxorubicin. The electrospinning solutions contained 3 – 5% of carboxymethyl chitosan in a solvent system consisting of trifluoroacetic acid – dichloromethane with ratios (V/V) of 80:20, 85:15 and 90: 10 as well as Doxorubicin. It was found that from the above samples, only the solution containing 4% carboxymethyl chitosan in trifluouroacetic acid – dichloromethane (85-15) led to uniform electrospun nanofibers.The diameter of the electrospun nanofibers was measured by SEM micrographs and measurement software. The diameter of these nanofibers containing 16.7, 25 and 34% (W/W) Doxorubicin lies in the range of 390 – 460 nm, respectively. As can be seen increasing the amount of Doxorubicin leads to higher diameter of electrospun nanofibers. Unfortunately, all the attempts to electrospin low diameter nanofibers failed. FTIR analysis showed no reaction occurring between Doxorubicin and carboxymethyl chitosan. Moreover, X-Ray diffraction patterns showed that Doxorubicin is dispersed in crystallite forms in the matrix of crystalline carboxymethyl chitosan. As far as the release of Doxorubicin from the phosphate buffer solution (pH = 7.4) is concerned, HPLC investigations showed that carboxymethyl chitosan nanofibers containing Doxorubicin have the capability of controlled release of this drug for anti-cancer treatments. It was found that the release of 16.7% Doxorubicin sample from carboxymethyl chitosan nanofibrous matrix occurs according to non-Fick diffusion mechanism. However, the 25 and 34% samples showed Fick diffusion behavior. Keywords: Nanofibres, Carboxy methyl Chitosan, Doxorubicin, Drug delivery