Analysis of samples available in small volumes is an important challenge in analytical chemistry. Therefore, we have dealt with the development of a new miniaturized micro-volume voltammetric cell (MVVC) for the determination of reducible organic compounds in micro-volumes (20-50 mu L). The MVVC is composed of two compartments, a micro-volume compartment, where the analyte is present along with the working electrode, separated by means of an agar membrane (about 2 mm) from a large-volume compartment containing the supporting electrolyte and the counter and reference electrodes. This MVVC was tested by the determination of sodium anthraquione-2-sulfonate as a model substance for structurally similar anthraquinone-based anti-cancer drugs. Using differential pulse voltammetry at a polished silver solid amalgam electrode, the following analytical parameters were obtained: linear dynamic range from 1 mu mol L-1 to 1 mmol L-1, repeatability of 0.7% (on the concentration level 0.1 mmol L-1), and limit of detection of 0.15 mu mol L-1.