The use of solid-phase extraction for the analysis of liquid media containing low microg/L levels of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX), mononitroso-RDX (MNX), dinitroso-RDX (DNX), and trinitroso-RDX (TNX) is examined. Aqueous samples (100 mL) consisting of water and a microbiological basal medium are spiked with known concentrations of RDX, MNX, DNX, and TNX. The compounds are extracted from the liquid media using a Porapak RDX cartridge and then eluted from the cartridge with 5 mL of acetonitrile. The eluent is concentrated to 1 mL before analysis by high-pressure liquid chromatography (HPLC). The method detection limits for RDX are 0.1 microg/L in water and 0.5 microg/L in the basal medium after a 100-fold concentration. For MNX, DNX, and TNX, the method detection limits are approximately 0.5 microg/L in water and approximately 1 microg/L in the basal medium after a 100-fold concentration. Interferences in the basal medium and a contaminant in the standard made quantitation for MNX and TNX, respectively, is less accurate below the 1 microg/L level. Solid-phase extraction of the liquid media gave good recoveries of nitramines and nitroso intermediates from a microbiological basal medium, allowing HPLC detection of RDX and the nitroso intermediates in the low microg/L (ppb) range.