A novel attenuated total reflection (ATR) sensor, whichintegrates solid-phase extraction (SPE) and infrared detection, is presented. The flow cell, which enables the on-line coupling with a sequential injection system, is thecore of the proposed sensor since it allows the continuousdelivery of different solutions through the ATR and alsothe continuous spectrum acquisition. A SPE sorbentmaterial (LiChrolut EN) was located in the sensitiveelement of the ATR without using any external coatingsubstance, increasing the versatility of the system. Amarked sensitivity enhancement was obtained as theanalyte was concentrated before detection. The new sensor was qualitatively and quantitatively validated using thedetermination of caffeine in soft drinks as the modelanalytical problem. Linearity, precision (RSD = 4%), andsensitivity (LOD = 7
g/mL) levels have been established.Finally, the main advantages and limitations of the newproposal are presented and compared with existing alternatives.