STUDI DINAMIKA PEMBENTUKAN KOKRISTAL TEOFILIN NATRIUM SAKARIN DIHIDRAT DENGAN FTIR

• Main Author: Ulfi Bahari, Muhamad
• Format: Final Project
• Language: Indonesia
• Online Access: https://digilib.itb.ac.id/gdl/view/64460
• Institution: Institut Teknologi Bandung

Co-crystals are crystalline materials composed of two or more stoichiometric components. The component can be atomic, molecular, or ionic compounds. Theophylline have been reported forming co-crystals with many compounds, and sodium saccharin had too, co-crystal of teophylline and sodium saccharin have not been reported yet. Usually the dynamics of the formation of co-crystal is using PXRD and DSC, but in this research FTIR instrument was used to identify the formation of co-crystals by using the principle of wave number shift of N-H stretching during ball milling at various speed. Theophylline monohydrate (TM), anhydrous theophylline (TA), sodium saccharin dehydrate (NSD), physical mixture of TM-NSD and TA¬NSD = 1:1.66 was characterized using polarized microscopy, Fourier-transform infrared spectroscopy (FTIR), differential thermal analysis (DTA), powder X-ray diffraction (PXRD), and Karl Fischer titration. Conduction of formation co-crystal with thermal contact method using polarizing microscope and the making of the phase diagram using Electrothermal 9100. TM-NSD and TA-NSD (1:1.66) was treated with ball mulling method to obtain the co-crystal, dynamics of co-crystals was observed with increased speed from 45, 75, and 105 rpm, the sampling was done at minute 0, 10, 20, 30, 40, 50, and 60. For characterization and ensure a co-crystal formation was used DTA and PXRD. Thermal contact method showed the formation of co-crystals TM-NSD and TA-NSD, the phase diagram is similar to the curve which formed co-crystal. FTIR spektra N-H streching shift in TM-NSD showed wave number shifted from 3108.69 cm-1 to 3127.97 cm-1 then 3131.83 cm', whereas the mixture TA-NSD shifted from 3124.12 cm-1 to 3131.83 cm* Wave number shifted from 3127.97 cm-1 then 3131.83 ens' in TM-NSD showed after 40 minutes of 45 rpm ball milling; 20 minutes of 75 rpm and 105 rpm; whereas TA-NSD showed after 20 minutes of 45 rpm ball milling; 10 minutes of 75 rpm and 105 rpm. It concluded that higher energy required to forming TM-NSD co-crystals to TA-NSD. Thermogram of DTA showed that the endothermic curve was melting point of co-crytal at 121°C. Diffractogram of milled TM-NSD and TA-NSD (1:1.66) was significantly different with diftactogram of their physical mixture. Base on all of research data, it can be concluded that FTIR can be used to study the dynamics of TM-NSD and TA-NSD co-crystal formation. Thermogram and diffractogram of milled TM-NSD and TA¬NSD have typical di ifractogram peaks at 20 = 12,32°; 17,48°; 26,86°; 27,4°; and 28,84° was supported and confirmed that both of them forming the co-crystals with the same crystal structure. However TM-NSD needs more energy than TA-NSD co-crystal forming due to its hydrate release.