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Za djelatnu tvar koja se koristi u liječenju shizofrenije, olanzapin, bilo je potrebno pronaći otapalo koje je najpogodnije u vidu morfologije dobivenih kristala. Provedena je kristalizacija s izobutil acetatom, metl izobutil ketonom, etil acetatom i toluenom kao otapalom. Istraživanje je provedeno u šaržnom kristalizatoru. Zbog bolje morfologije kristala i krivulje topljivosti odabran je toluen kao najpogodnije otapalo te se daljnje istraživanje kristalizacije odvija u toluenu. U okviru ovog rada, istražen je utjecaj vrste miješala na morfologiju i granulometrijska svojstva kristala. Korištena su četiri različita miješala, od kojih se s dva miješala postiže aksijalni tok, a s dva radijalni tok. Također, istražen je utjecaj broja okretaja miješala na svojstva dobivenih kristala. Istraživanje je provedeno pri 150, 250 i 350 okretaja u minuti. U svrhu karakterizacije dobivenih kristala olanzapina u različitim uvjetima provedbe procesa, provedena je analiza kemijskog sastava metodom difrakcije rendgenskih zraka, analiza granulometrijskih svojstava gdje je raspodjela veličina čestica određena metodom laserske difrakcije te pomoću FBRM sonde, a morfologija kristala je analizirana optičkim i pretražnim elektronskim mikroskopom pod različitim uvećanjima. Toplinska svojstva kristala olanzapina istražena su diferencijalnim pretražnim kalorimetrom i termogravimetrijskom analizom. For the active pharmaceutical ingredient used in the treatment of schizophrenia, olanzapine, it was necessary to find the solvent which is most suitable in the form of the morphology of the crystals obtained. Crystallization was performed with isobutyl acetate, methyl isobutyl ketone, ethyl acetate and toluene as solvent. The research was conducted in a batch crystallizer. Due to the better crystal morphology and solubility curve, toluene was chosen as the most suitable solvent, and further crystallization research was carried out in toluene. In this work, the effect of the type of mixer on the morphology and granulometric properties of crystals was investigated. Four different mixers were used, of which two mixers achieve axial flow and two radial flow. Also, the effect of the stirrer speed on the properties of the obtained crystals was investigated. The study was conducted at 150, 250, and 350 rotations per minute. In order to characterize the obtained olanzapine crystals under different process conditions, the chemical composition was analyzed by X-ray diffraction, granulometric properties were also analyzed by measuring particle size distribution using laser diffraction method and FBRM probe, and crystal morphology was analyzed by optical and scanning electron microscope with different magnifications. The thermal properties of olanzapine crystals were investigated by differential scanning calorimeter and with thermogravimetric analysis. |
