20.500.12556/DKUM-13906 Validacija HPLC metode za medfazno spremljavo sinteze (S)-1-[3-(Dimetilamino)propil]-1-(4-fluorofenil)-1,3-dihidro-5-izobenzofurankarbonitrila Validation of HPLC method for monitoring of in-process control during synthesis of (S)-1-[3-(Dimethylamino)propyl]-1-(4-fluorophenyl)-1,3-dihydroisobenzofuran-5-carbonitrile Namen diplomskega dela je bil ovrednotiti in validirati HPLC medfazni analizni metodi za določevanje enantiomerne čistosti intermediata in kromatografske čistosti produkta pri medfazni spremljavi sinteze (S)-1-[3-(dimetilamino)propil]-1-(4-fluorofenil)-1,3-dihidro-5-izobenzofurankarbonitrila. Poudarek je bil na določitvi validacijskih parametrov, izdelavi validacijskega načrta, validacije, ovrednotenju rezultatov s statističnimi metodami in na interpretaciji rezultatov. Obe metodi sta natančni, točni, linearni, selektivni in robustni. Določene so bile meje zaznavanja, meje določanja in stabilnost raztopin za obe metodi. Metodi sta primerni za rutinsko določanje enantiomerne čistosti intermediata in kromatografske čistosti produkta pri medfazni spremljavi sinteze (S)-1-[3-(dimetilamino)propil]-1-(4-fluorofenil)-1,3-dihidro-5-izobenzofurankarbonitrila. The purpose of diploma thesis was to validate and evaluate in-process HPLC methods for monitoring and determination of enantiomer purity of an intermediate substance and chromatographic purity of the product at synthesis of (S)-1-[3-(Dimethylamino)propyl]-1-(4- fluorophenyl)-1,3-dihydroisobenzofuran-5-carbonitrile. The main emphasis was to establish validation parameters, preparing validation plan, realization of validation, evaluation of validation results with statistical methods and interpretation of results. Both validated methods are precise, accurate, linear, selective and robust. Limit of detection, limit of quantitation and stability of standard and sample solutions were established. Methods are suitable for determination of enantiomer purity of intermediate substance and of chromatographic purity of the product at synthesis of (S)-1-[3-(Dimethylamino)propyl]-1-(4-fluorophenyl)-1,3-dihydro isobenzofuran-5-carbonitrile. dobra laboratorijska praksa DLP validacija HPLC intermediat enantiomer enantiomerna čistost kromatografska čistost good laboratory practice GLP validation HPLC intermediate substance enantiomer enantiomer purity chomatographic purity true true false [B. Smolkovič] Slovenski jezik Angleški jezik Diplomsko delo 2010-05-09 11:18:16 2010-05-25 10:49:47 2022-04-12 11:34:56 2023-12-16 03:36:06 2010 0 Maribor 0 0000-00-00 NiDoloceno NiDoloceno NiDoloceno 0000-00-00 0000-00-00 0000-00-00 543.544.5(043.2) 14263574 URN:SI:UM:DK:VUTTIZWZ VS_Smolkovic_Bojan_2010.pdf VS_Smolkovic_Bojan_2010.pdf 1 F3FC33703CF9BFB5BA28DF12B30BF650 b99e734b1c96ac655b40919d9462e418639ff882ce771b556fd284af0dd2ae21 05e3cb4d-7c04-11eb-bb7a-00155d0001ca 20.500.12556/dkum/04825a45-e0ef-4577-9b51-3cd3bc1e2fe5 https://dk.um.si/Dokument.php?lang=slv&id=14440 Fakulteta za kemijo in kemijsko tehnologijo 0 0 0