The objective of this study was to assess the quality of cotrimoxazole tablets produced by a Tanzanian manufacturer by a newly instituted quality assurance program. Tablets underwent a diffuse reflectance spectroscopy procedure with periodic quality assessment confirmation by assay and dissolution testing using validated HPTLC techniques (including weight variation and disintegration evaluations). Based on results from the primary test methods, the first batch of product was <80% compliant, whereas subsequent batches reached >99% compliance. This approach provides a model for rapidly assuring product quality of future procurements of other products that is more cost effective than traditional pharmaceutical testing techniques.