Determination of saccharin in pharmaceuticals by high performance thin layer chromatography

Abstract

A simple, accurate and selective high performance thin layer chromatographic method for the determination of saccharin in pharmaceuticals has been developed. The chromatography was performed on silica-gel 60F254 plates with ethyl acetate-carbon tetrachloride-acetic acid (3 + 4 + 0.5 v/v/v) as the mobile phase. The chromatographic zones corresponding to the saccharin spots were scanned in the reflectance/absorbance mode at λ=230 mm. For the standard curves, two series of saccharin sodium salt solutions were prepared: in methanol (solvent 1) and in ethyl acetate-acetic acid (9:1, v/v) mixture (solvent 2). A linear calibration relationship was observed within the concentration range from 300-1200 ng saccharin sodium salt per spot correlation coefficients being 0.998 (solvent 1) and 0.995 (solvent 2). The relationship between the peak area and the amount of saccharin sodium salt was evaluated by linear regression analysis. The limits of detection and quantification of saccharin sodium salt were 35 ng and 110 ng per spot (solvent 1), respectively, and 45 ng and 150 ng per spot (solvent 2) respectively. Mean recovery values of 103.5 % (solvent 1) and 102.3 % (solvent 2), and RSD values of 4.42 % (solvent 1) and 2.53 % (solvent 2) were obtained. The proposed method was applied for saccharin determination in two pharmaceutical preparations, effervescent tablets and a carbomer- based gel.

Predložena je jednostavna i selektivna metoda za određivanje saharina u farmaceutskim preparatima primenom visoko efikasne tankoslojne hromatografije. Određivanja su vršena na silika-gel pločama 60F254 koristeći kao mobilnu fazu smešu etilacetata, ugljentetrahlorida i sirćetne kiseline (3 + 4 + 0,5, v/v/v). Pripremljene su dve serije standardnih rastvora natrijumove soli saharina: u metanolu (rastvarač 1) i smeši etilacetat-sirćetna kiselina (9:1, v/v) (rastvarač 2). Kalibracione krive snimljene su na talasnoj dužini od 230 nm u opsegu nanetih količina natrijumove soli saharina (300-1200 ng), sa koeficijentima korelacije 0,998 (rastvarač 1) i 0,995 (rastvarač 2). U ispitivanom opsegu utvrđena je linearna zavisnost između površine pikova i količine natrijumove soli saharina. Limit detekcije i limit kvantifikacije saharina iznosili su redom 35 ng i 110 ng (rastvarač 1) i 45 ng i 150 ng (rastvarač 2). Dobijene su sledeće vrednosti za "recovery" i relativnu standardnu devijaciju: 103,5 % i 4,42 % (rastvarač 1) i 102,3 % i 2,53 % (rastvarač 2). Predložena metoda je primenjena za određivanje saharina u šumećim tabletama Kalcijum® i Daktanol® gelu.