Laser-induced breakdown spectroscopy (LIBS) is evaluated as a potential analytic technique for rapid screening and quality control of anti-diabetic tablets. This paper proposes a simple LIBS-based method for the quantitative analysis of two active pharmaceutical ingredients (APIs): metformin (Met) and glybenclamide (Gly). In order to quantify both APIs, chlorine (Cl) concentration was estimated by employing the Cl/Br optical emission ratio, where Br was introduced as internal standard. Calibration curves were prepared, achieving linearity higher than 99%. On the other hand, for comparison to the proposed method, an isocratic reversed-phase high-performance liquid chromatography (RP-HPLC) method was also developed for quantitative determination of the same analytes by ultraviolet (UV) detection. The chromatographic separation was achieved on a Phenomenex Hypersil C18, 250 mm × 4.6 mm, 5 ?m column. The mobile phase was K<sub>2</sub>HPO<sub>4</sub>/H<sub>3</sub>PO<sub>4</sub>-CH<sub>3</sub>OH and flow rate was 1.0 mL min<sup>?1</sup>. The method is linear over a range of 10-60 ?g mL<sup>?1</sup> for Gly and 5-30 ?g mL<sup>?1</sup> for Met and the correlation coefficients were ?0.99. Recoveries were found to be in the range of 95-101%. Furthermore, four different commercial brands of each active agent were evaluated by both proposed LIBS and chromatographic methods and results were compared with each other. The comparison was satisfactorily validated by analysis of variance (ANOVA).

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