| Abstract | Korištenjem analize slijednim injektiranjem (engl. Sequential Injection Analysis, SIA), u ovom radu je razvijena i vrednovana nova metoda određivanja penicilamina u komercijalnim farmaceutskim pripravcima. Temelj razvijene metode je redoks reakcija u kojoj penicilamin sudjeluje kao reducens. Penicilamin reducira bis(batokuproindisulfonato)kuprat(II) u narančasto obojeni spoj bis(batokuproindisulfonato)kuprat(I). Nastali spoj postiže maksimalnu apsorbanciju pri valnoj duljini od 483 nm. Pri optimiziranim kemijskim uvjetima i uvjetima SIA sustava je ostvareno linearno dinamičko područje u rasponu koncentracija od 2,0 × 10-6 M do 6,0 × 10-5 M. Linearnom regresijskom analizom je dobivena krivulja umjeravanja, čija je jednadžba pravca y = 7182x + 0,0073. Izračunane su granica dokazivanja, LOD = 6,0 × 10-7 M i granica određivanja, LOQ = 2 × 10-6 M. Vrednovanjem metode su utvrđene i njene analitičke karakteristike: točnost uz iskoristivost u rasponu od 88,24 % do 99,07%, doseg reakcije od 99,30%, učestalost analize od 24 analize u triplikatu unutar jednog sata, tj. 72 analize/h, ponovljivost uz relativno standardno odstupanje od 3,53%. Osim acetilsalicilne kiseline, H3BO3, Na2SO4, natrijeva citrata, saharoze, laktoze, tartaratne kiseline i limunske kiseline, ostale pomoćne tvari u 500 puta većoj koncentraciji ne interferiraju prilikom određivanja penicilamina u realnom uzorku. Vrednovana i razvijena metoda je uspoređena sa standardnom metodom koju propisuje Britanska farmakopeja te se pokazala kao prikladna metoda za određivanje penicilamina u komercijalnim farmaceutskim pripravcima. |
| Abstract (english) | Using sequential injection analysis (SIA), a new method for the determination of penicillamine in commercial pharmaceutical preparations was developed and evaluated. The method is based on the redox reaction in which penicillamine participates as a reducing agent. Penicillamine reduces bis(bathocuproindisulfonato)cuprate(II) to the orange colored compound bis(bathocuproindisulfonato)cuprate(I). This compound achieves maximum absorbance at a wavelength of 483 nm. Using optimized chemical parameters and parameters of the SIA system, a linear dynamic range was accived in the concentration range from 2.0 × 10-6 M to 6.0 × 10-5 M. A linear regression analysis was used to obtain a calibration curve, whose equation is the y = 7182x + 0.0073. The LOD and LOQ of the developed method were calculated, where LOD was 6.0 × 10-7 M and LOQ was 2.0 × 10-6 M. The validation of this method also determined its analytical characteristics, such as accuracy with a range of recovery from 88.24 % do 99.07%, reach of the reaction 99.30%, analysis frequency of 24 analyses in triplicate within one hour, 72 analyses/h, reproducibility with a relative standard deviation of 3.53%. Apart from acetylsalicylic acid, H3BO3, Na2SO4, sodium citrate, sucrose, lactose, tartaric acid and citric acid, other excipients in a more concentrated amount do not interfere whit the determination of penicillamine in a real sample of a pharmaceutical preparation. The evaluated and developed method was compared with the standard method prescribed by the British Pharmacopoeia and proved to be a suitable method for the determination of penicillamine in commercial pharmaceutical preparations. |
