Pharmaceutical preparations are the final product of a technological process that gives the drugs the characteristics appropriate for easy administration, proper dosage, and enhancement of the therapeutic efficacy. The design of pharmaceutical preparations in nanoparticulate form has emerged as a new strategy for drug delivery (Pasquali, Bettini, and Giordano, 2006). Particle size (PS) and particle size distribution (PSD) are critical parameters that determine the rate of dissolution of the drug in the biological fluids and, hence, have a significant effect on the bioavailability of those drugs that have poor solubility in water, for which the dissolution is the rate-limiting step in the absorption process (Perrut, Jung, and Leboeuf, 2005; Van Nijlen et al., 2003). Supercritical antisolvent (SAS) processes have been widely used to precipitate active pharmaceutical ingredients (APIs) (Chattopadhyay and Gupta, 2001; Rehman et al., 2001) with a high level of purity, suitable dimensional characteristics, narrow PSD, and spherical morphologies. The SAS process is based on the particular properties of the supercritical fluids (SCFs). These fluids have diffusivities two orders of magnitude larger than those of liquids, resulting in a faster mass transfer rate SCF properties (solvent power and selectivity) can be also adjusted continuously by altering the experimental conditions (temperature and pressure). As a consequence, SCFs can be removed from the process by a simple change from the supercritical to room conditions, which avoids difficult post-treatments of waste liquid streams. Carbon dioxide (CO2) at supercritical conditions, among all possible SCFs, is largely used because of its relatively low critical temperature (31.1 degrees C) and pressure (73.8bar), low toxicity, and low cost. In this article, we show some results about processed antibiotics (ampicillin and amoxicillin), two of the world's most widely prescribed antibiotics, when they are dissolved in 1-methyl-2-pyrrolidone (NMP) and carbon dioxide is used as antisolvent.