Simple, precise and accurate high performance thin layer chromatographic method for analysis of thiocolchicoside and aceclofenac both as a bulk drug and in combined dosage form was developed and validated. The method employed TLC (Thin Layer Chromatography) aluminum plates precoated with silica gel 60F-254 as a stationary phase and isopropyl alcohol: ammonia (9:1v/v) as mobile phase. The retention factor for thiocolchicoside and aceclofenac were found to be 0.43 ± 0.03 and 0.67 ± 0.03 respectively. Densitometric analysis was carried out in the absorbance mode at 260 nm. The method was validated for precision, recovery and robustness. The linear regression analysis data for the calibration spots showed good relationship with (regression) r2 = 0.9972 for thiocolchicoside and (regression) r2=0.9973 for aceclofenac in the amount range of 200–1200 ng/spot.
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