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A simple, sensitive, selective, and stability-indicating high-performance thin-layer chromatography method with fluorescence detection was developed for the analysis of a mixture of tamsulosin hydrochloride and tolterodine tartrate, used in the management of benign prostatic hyperplasia in their laboratory-prepared binary mixture and dosage form. The separation was employed on thin-layer chromatography silica gel 60 aluminum sheets. As developing system, ethyl acetate–n-hexane–diethylamine (9:3:1, V/V) was used. Tamsulosin and tolterodine had retention factors (RF) of 0.40 ± 0.03 and 0.85 ± 0.03, respectively. A 225 nm excitation wavelength was used for the fluorescence detection. Linearity was in the range of 10.0–200.0 and 100.0–900.0 ng/band for tamsulosin and tolterodine, respectively. The method was validated successfully according to the International Council for Harmonisation guidelines. Our suggested method for determining tamsulosin and tolterodine in their dosage forms and in the presence of their degradation products could be conveniently applied in quality-control laboratories.

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