Efficient tuberculosis treatment requires the use of good quality medicines. The present study developed a method of dosage by High Performance Liquid Chromatography (HPLC) coupled with the dissolution of a combination of fixed doses of four anti-tuberculous (Isoniazid, Pyrazinamide, Ethambutol Hydrochlorate, Rifampicine). The elaborated protocol was thereafter used to assess the quality of medicines commonly used in Benin as per the National Program for Tuberculosis Control (PNT). An analytical procedure was developed and validated by statistical tests of Cochran and Grubbs. Five lots of anti-tuberculous were randomly sampled (from India and tuberculosis screening and treatment centres in Benin). These lots were subjected to a number of tests including preliminary, disintegration, identifications and dissolution tests coupled with HPLC and dosages. The established procedure is demonstrated to be applicable with 80% accuracy. Results of the quality control revealed 100% conformity to all the tests for all tested drugs from all lots. The elaborated procedure is therefore applicable, rapid, effective and simple.