SACCHARIN ISOMOPHYSM: Thermal and structural investigation

D.A. Vargas (PG)1, A.P.G. Ferreira (PQ)1, E.T.G. Cavalheiro (PQ)1. 1 Universidade de So Paulo,So Carlos (SP),Brasil.

Saccharin is sugar substituent in pharmaceutical industry; it is used as excipient in the formulations to mask bitter taste of active ingredients [1]. In the solid pharmaceutical formulations the sweetening ability of saccharin could be limited for the existence of polymorphism, which would affect the quality of drug [2]. In this it was investigated the existence of polymorphic forms of saccharin. Via recrystallization from different solvents, sublimation- solidification and antisolvent precipitation three morphologically different saccharin crystals were obtained. These crystals presented prismatic, acicular and laminar habits. Figure 1 presented photographs of each type of crystals. The crystals were characterized thermal and structurally, by differential scanning calorimetry (DSC) and X-ray powder diffraction (XRPD). The DSC curves obtained are presented in Figure 2 and The XRPD profiles are presented in Figure 3. The crystals do not presented differences in their melting points and additional peaks were observed in the DSC curves of the acicular and laminar forms. These endothermal events could be attributed to solid/solid transitions. However, the XRPD profiles dont display structural differences between the tree types of crystals. This saccharin crystals seems to be are a case of isomorphism, whit different crystal habits which correspond to the same unit cell and the macroestructural differences do not mean microestructural distintions.

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Figure 1. Optic microscopy images of saccharin crystals. a) Via recristalizatin from ethanol solutions; b) By sublimation/solidification; c) By antisolvent precipitation from acetone solutions and addition of antisolvent sodium saccarin aqueous solution.

Figure 2. DSC curves for the saccharin crystals. Sample mass: 3 mg ( 0.1 g); aluminum sample holder; 10 Cmin-1 heating rate.

Figure 3. Saccharin crystals Powder diffractograms.

References [1] PEARSON, R.L. Saccharin. In: NABORS, O.L. (Ed.). Alternative sweetener. New York: Marcel Dekker, 2001. p. 147-166. [2] DAVID, J.; GRANT, W. Theory and origin of polymorphism. In: BRITTAIN, H.G. (Ed.). Polymorphism in pharmaceutical solids. New York: Marcel Dekker Inc, 1999, p 1- 33.