PEMBUATAN DAN ANALISIS KRISTAL TUNGGAL KOKRISTAL TEOFILIN ANHIDRAT – NATRIUM SAKARIN DIHIDRAT DENGAN BEBERAPA PELARUT

• Main Author: Agiana P, Evalianty
• Format: Final Project
• Language: Indonesia
• Online Access: https://digilib.itb.ac.id/gdl/view/45435
• Institution: Institut Teknologi Bandung

Cocrystal is a crystal form which consists of two or more components with specific stoichiometric ratio. Theophylline has been reported to form cocrystal with sodium saccharin with specific stoichiometric ratio, but the single crystals determination of the cocrystal has not done. Quality of single crystals are influenced by several factors, including temperature and composition of solvent used. Analysis of single crystals are needed to determine the three-dimensional structure and the interaction that occurs certainty. Theophylline and sodium saccharin cocrystal also tested against extreme moisture. Theophylline anhydrous powder (TA), sodium saccharin dihydrate (NSD), and physical mixtures of TA-NSD = 2.4: 3.6 respectively were characterized using polarizing microscope, fourier-transform infrared spectroscopy (FTIR), powder x-ray diffractometry (PXRD), and Karl Fischer titration. Single crystals of TA-NSD cocrystal formation was done by slow evaporation method at room temperature and 12 °C using four types solvent mixtures, waterisopropanol 1:7; water-acetone 1:9; ethanol-dichloromethane 9:1; and ethanol. Rate formation of cocrystals was observed and characterized using polarizing microscope, fourier-transform infrared spectroscopy (FTIR), powder x-ray diffractometry (PXRD), and single crystals analysis using single crystal x-ray diffractometry (SC-XRD). Stability test was applied to TA-NSD cocrystal at RH: 95%. Single crystals only formed in water-isopropanol solvent 1: 7 with size 0.6 to 1.2 cm (room temperature) and 0.6 to 1 cm (temperature 12 °C) and solvent of water-acetone 1: 9 with size 0.5 to 1.1 cm (room temperature). On the other solvents, cocrystal only formed in crystalline form and thin crystals with a size of ?5 mm (room temperature and 12 °C). Visual observation that supported by polarizing microscope magnification showed TA-NSD cocrystal has needleshaped and translucent color. FTIR spectra analysis results showed N-H stretching of cocrystal shift from wavenumber 3124.12 cm -1 to 3127.97-3131.83 cm -1 . Result of PXRD analysis indicated that TA-NSD cocrystal diffractogram has sharp peaks on 2?= 5.58; 12.32; 17.48; 22.40; 26.86; 27.4; 28.84 and 34.1°. Results of analysis with SC-XRD showed that TA-NSD cocrystal has monoclinic crystal system with a axis: 14.539 Å; b axis: 6.8430 Å; c axis: 16.129 Å; ?angle: 99.239°; with volume 1583.9 Å 3 . The structure has not been reported previously. Stability test against moisture results are analyzed by FTIR spectra and indicate that cocrystal unchanged shift N-H strain which means it does not happen decomposition at cocrystal bond. Conclusion: From all the observations and analysis, TA-NSD cocrystal has needle shaped, translucent color and monoclinic crystal system with volume 1583.9 Å 3 . The single crystals formed at room temperature and 12 °C with a water-isopropanol solvent and at 12 °C temperature with water-acetone 1: 9. In addition, the results of stability test against moisture showed that TA-NSD cocrystal is stable against moisture.