A partially automated module for the routine determination of illicit non-steroid antiinflammatory drugs (NSAIDs) in biological fluids from race horses was built, tested, refined, and shown to work. This pretreatment module retains 17 NSAIDs on an Amberlite XAD-2 column before back-elution derivatization with methyl iodide in acetonitrile. Methylated derivatives are manually injected into a gas chromatograph connected to a mass spectrometer. The quantification limits thus achieved are 50-100 ng/mL in 1 mL of urine or plasma. The proposed method is more expeditious than its manual liquid-liquid and liquid-solid extraction counterparts and is similar in speed to a typical gas chromatographic program.