A new method for the determination of cyclophosphamide content of polyalkylcyanoacrylate nanoparticles was developed. The analyses were carried out by inductively coupled plasma atomic emission spectrometry (ICP-AES) by measuring the phosphorus content in the drug. The results obtained by this non-selective technique were compared with those given by high performance liquid chromatography (HPLC) a selective procedure that permits the detection of the cyclophosphamide molecule, and its degradation products. Sensitivity and reproducibility of both procedures were also determined. The ICP-AES method was demonstrated to be valid for sensitivity, precision, accuracy and specificity. In spite of ICP method is not a suitable procedure to analyze the degradation products of cyclophosphamide, the sensitivity of ICP is higher than chromatographic technique. Nevertheless, both procedures are appropriate for the determination of cyclophosphamide-loaded nanoparticles.