20.500.12556/DKUM-92940 Uporaba sistema dissowash&dose v farmacevtski analitiki magistrsko delo The use of the dissowash&dose system in pharmaceutical analysis Magistrsko delo prikazuje uporabo sistema dissoWASH&DOSE za izvajanje ciklov čiščenja med izvajanjem testov raztapljanja in določanje prenosa analita (angl. carry over, CO). Teste raztapljanja smo izvedli s tremi aktivnimi farmacevtskimi učinkovinami (API) – kofeinom (KOF), paracetamolom (PA) in natrijevim naproksenatom (NN). Najprej smo izvedli delno validacijo spektrofotometričnih metod za vsak analit. Linearno koncentracijsko območje smo za KOF določili od 1,00 mg/L do 30,00 mg/L, za PA in NN pa od 1,00 mg/L do 19,00 mg/L. Linearnost smo ovrednotili z izračunom kvadrata korelacijskega koeficienta, ki je bil za vse API ≥0,9990 in izračunom koeficienta kvalitete, katerega vrednosti so bile ≤5,00 %. Točnost smo ovrednotili z izračunom povprečnih izkoristkov, ki so bili na treh testiranih koncentracijskih nivojih znotraj zastavljenega kriterija 95,00–105,00 %. Natančnost smo ovrednotili z relativnim standardnim odmikom, ki je bil za vse API <10,00 %. Meja zaznavnosti je bila za vse API <0,01 mg/L. Z določanjem volumnov (V) odmerjanja medija za raztapljanje in medija za čiščenje pri ciklu čiščenja reakcijskih posod in pri ciklu čiščenja pokrova, temperaturnih senzorjev, vzorčevalnih kanul in mešal, smo preverili točnost in natančnost odmerjanja sistema dissoWASH&DOSE. Zastavljena hipoteza je bila, da bo sistem dissoWASH&DOSE uspešno izvedel cikel čiščenja s CO nižjim od 0,50 %. Izvedli smo preizkuse nižanja V čistilnega medija za čiščenje reakcijskih posod ter čiščenje pokrova, temperaturnih senzorjev, vzorčevalnih kanul in mešal, da bi preverili, kako skupni V čistilnega medija obeh ciklov čiščenja vpliva na CO. CO je bil <0,50 % za vse API pri vseh testiranih V čistilnega medija obeh ciklov čiščenja, tj. pri skupnih V obeh ciklov čiščenja 430 mL, 330 mL, 230 mL, 130 mL in 40 mL. Posledično lahko s sistemom dissoWASH&DOSE zadovoljivo očistimo reakcijske posode, pokrove, temperaturne senzorje, vzorčevalne kanule in mešala tudi pri nižjih V čistilnega medija ter je zato primeren za zaporedno izvajanje testov raztapljanja za KOF, NN in PA v farmacevtski analitiki. The master's thesis shows the use of the dissoWASH&DOSE system for performing cleaning cycles during dissolution tests and determining analyte carry over (CO). The dissolution tests were performed with three active pharmaceutical ingredients (APIs) – caffeine (KOF), paracetamol (PA) and naproxen sodium (NN). First, a partial validation of the spectrophotometric methods was performed for each analyte. The linear concentration range for KOF was determined from 1.00 mg/L to 30.00 mg/L, and for PA and NN from 1.00 mg/L to 19.00 mg/L. Linearity was evaluated by calculating the square of the correlation coefficient, which was ≥0.9990 for all APIs, and calculating the quality coefficient, the values of which were ≤5.00%. Accuracy was evaluated by calculating the average recoveries, which were within the set criterion of 95.00–105.00% at three tested concentration levels. Precision was evaluated by the relative standard deviation, which was <10.00% for all APIs. Limit of detection was <0.01 mg/L for all APIs. By determining the volumes (V) of dosing of the dissolution medium and cleaning medium in the cleaning cycle of the dissolution vessels and in the cleaning cycle of the lid, temperature sensors, sampling cannulas and stirrers, the accuracy and precision of the dosing of the dissoWASH&DOSE system was checked. The hypothesis was that the dissoWASH&DOSE system would successfully perform a cleaning cycle with CO lower than 0.50%. The tests of decreasing the V of the cleaning medium for cleaning the dissolution vessels and cleaning of the lid, temperature sensors, sampling cannulas and stirrers were performed to check how the total V of the cleaning medium of both cleaning cycles affects CO. CO was <0.50% for all APIs at all tested V of the cleaning medium of both cleaning cycles, i.e. at total V of both cleaning cycles of 430 mL, 330 mL, 230 mL, 130 mL and 40 mL. As a result, the dissoWASH&DOSE system can satisfactorily clean dissolution vessels, lids, temperature sensors, sampling cannulas and stirrers even at lower V of the cleaning medium and is therefore suitable for consecutively performing dissolution tests for KOF, NN and PA in pharmaceutical analytics. testi raztapljanja UV-VIS spektrofotometrija prenos analita KOF paracetamol natrijev naproksenat dissolution tests UV-VIS spectrophotometry carry over caffeine paracetamol naproxen sodium true true false [L. Embreuš] Slovenski jezik Angleški jezik Magistrsko delo/naloga 2025-05-27 22:36:25 2025-07-02 07:23:24 2025-07-24 03:09:27 0000-00-00 00:00:00 2025 0 Maribor 0 Maribor 1 spletni vir (1 datoteka PDF (XIII, 60 f.)) 0000-00-00 NiDoloceno NiDoloceno NiDoloceno 0000-00-00 0000-00-00 0000-00-00 542:615.012(043.2) 243585795 MAG_Embreus_Lana_2025.pdf MAG_Embreus_Lana_2025.pdf 1 26569ED364C15A0E7B9440D22AE765B3 9c9af890e67c6e913082474d55cba5003caba2d3b9aaece13d9b2f348f47ace8 027a5a65-538f-11f0-84e1-00155d000105 https://dk.um.si/Dokument.php?lang=slv&id=192865 Fakulteta za kemijo in kemijsko tehnologijo 0 0 0