20.500.12556/DKUM-11950 RAZVOJ IN UPORABA MIKRO PLINSKE KROMATOGRAFIJE ZA DOLOČANJE ATMOSFERE V FARMACEVTSKI EMBALAŽI DETERMINATION OF ATMOSPHERE IN PHARMACEUTICAL PACKAGES USING MICRO GAS CHROMATOGRAPHY Namen diplomske naloge je bil s pomočjo mikro plinske kromatografije (µGC) razviti enostavno in zanesljivo analizno metodo za določevanje kisika in vode v farmacevtski embalaži ter jo ustrezno ovrednotiti. Najprej smo s pomočjo plinskih standardnih mešanic razvili metodo na µGC instrumentu ter optimizirali analizne pogoje (temperaturo vhoda, injektorja in kolone, čas črpanja vzorca, čas injiciranja in čas analize ter tlak kolone). Kot nosilni plin smo pri vseh analizah uporabili argon. Ker µGC instrument ni imel posebnega nastavka za injiciranje atmosfere iz farmacevtske embalaže, smo ga modificirali in opremili z injekcijsko iglo, ki smo jo dodatno zatesnili in z navojem privili na injektor. Za čim boljšo ponovljivost injiciranja pri določanju atmosfere v žepkih smo poskrbeli tako, da smo na žepke nanesli silikon (Tekasil-Neutral Profi), in ga sušili pri sobni temperaturi 72 ur. S pomočjo modificirane igle smo nato prodrli v notranjost žepka, ne da bi pri tem kontaminirali vsebino vzorca z zunanjo atmosfero. Metodo smo uspešno uporabili na več vzorcih ter jo primerjali s plinsko kromatografijo v povezavi z masno spektrometrijo. The aim of the diploma thesis is to develop a simple and reliable analytical method for determination of oxygen and water content in pharmaceutical packaging blisters using micro gas chromatography (µGC). In the first place conditions of analytical procedure were optimised, namely inlet temperature, injector temperature, column temperature, sampling time, injection time, run time and column pressure. For this purpose standard gas mixtures were used. Argon was used as the carrier gas in the GC analysis. The µGC instrument was not equipped with an attachment for the injection of atmosphere from pharmaceutical packaging blisters. Consequently, the attachment had to be made especially from a modified hypodermic needle that further required sealing with a screw mount to the injector. For obtaining best reproducibility of injections for determination of atmosphere in pharmaceutical packages we applied silicon (Tekasil-Neutral Profi), which was then permitted to dry for 72 hours, so that it became completely dry. Using the modified hypodermic needle it was possible to penetrate into the interior of the blister. This made possible for the atmosphere in the blister to be sampled without possible contamination from the external atmosphere. The method was successfully applied to a number of samples and was compared with the existing method using gas chromatography coupled with mass spectrometry. plinska kromatografija mikro GC toplotna prevodnost TCD – detektor farmacevtska embalaža. gas chromatography Micro GC thermal conductivity TCD – detector Pharmaceutical Blister Packaging. true true false [T. Kocjančič] Slovenski jezik Angleški jezik Diplomsko delo 2009-09-25 15:44:51 2009-12-22 09:25:18 2022-04-12 07:05:27 2022-04-18 03:35:03 2009 0 Maribor 0 0000-00-00 NiDoloceno NiDoloceno NiDoloceno 0000-00-00 0000-00-00 0000-00-00 543.544.3:661.12(043.2) 13926934 URN:SI:UM:DK:5FL02OUM VS_Kocjancic_Tjasa_2009.pdf VS_Kocjancic_Tjasa_2009.pdf 1 406BA9F00250C52F5A127654A40A4195 02012c9ef5c83c0f201a68b3de55a39a21d78e7bcd732c0d45813dcce05023a1 45cafce6-7c03-11eb-bb7a-00155d0001ca 20.500.12556/dkum/aab6a1ce-e905-4069-b37c-951eb9447a8c https://dk.um.si/Dokument.php?lang=slv&id=10986 Fakulteta za kemijo in kemijsko tehnologijo 0 0 0