A simple and sensitive method for separation and quantitative determination of non-opioid analgesics from pharmaceutical preparations has been developed and validated. Commercial formulations of three non-opioid analgesics, viz. paracetamol, ibuprofen and diclofenac, were chosen for present studies. These were extracted, isolated, purified and recrystallized and were characterized by melting point, lambda(max) and IR. Quantitative determination was carried out using HPLC and TLC supplemented with UV spectrophotometry.