Razvoj in validacija HPLC analizne metode za določanje nesteroidnih protivnetnih učinkovin

Zabukovec, Tina

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Title:	Razvoj in validacija HPLC analizne metode za določanje nesteroidnih protivnetnih učinkovin
Authors:	ID Zabukovec, Tina (Author) ID Kolar, Mitja (Mentor) More about this mentor... ID Brodnjak-Vončina, Darinka (Comentor) ID Stana-Kleinschek, Karin (Comentor)
Files:	MAG_Zabukovec_Tina_2014.pdf (2,23 MB) MD5: F5475845A57D8084578BA86B5BAA2455
Language:	Slovenian
Work type:	Master's thesis/paper
Typology:	2.09 - Master's Thesis
Organization:	FKKT - Faculty of Chemistry and Chemical Engineering
Abstract:	V sklopu magistrskega dela smo preučevali razvoj in validacijo tekočinske kromatografije (HPLC-UV/VIS) analizne metode za določanje nesteroidnih protivnetnih učinkovin ter prenos razvite metode na tekočinski kromatografiji sklopljeni z masno spektrometrijo (LC-ESI-MSMS). Izbiro analiznega sistema za kvalifikacijo in kvantifikacijo narekujejo predvsem različni postopki priprave vzorcev. Posebno pozornost smo namenili različnim postopkom priprave takšnih oblog vezanih z analgetiki (sredstva proti bolečinam), ki spadajo v družino nesteroidnih antirevmatikov (NSAID). Lastnost alginatnih kopren, pri nanosu na kožno vnetje, je da se oblikujejo po rani oziroma vnetju, s čemer je doseženo vzdrževanje optimalne vlažnosti, njegove fizikalno-kemijske lastnosti pa povzročijo zgodnejše zacelitve in delujejo hemostatsko. Z vezavo nesteroidnih protivnetnih učinkovin v visoko vpojne netkane obloge, smo želeli doseči počasno in kontrolirano sproščanje na mestu vnetja. Rezultati kažejo, da s prvotno uporabljenimi postopki vezave naproksena na alginatno oblogo ne dosežemo željenega sproščanja, s postopki modifikacije prvotne metode pa je enakomerno sproščanje doseženo. Za kvantifikacijo sproščenega naproksena iz tako pripravljenih oblog pa smo z uporabo predhodno razvite metode 2 s postopki validacije metode preverli, da metoda daje točne in natančne razultate ter je primerna za rutinsko določanje nesteroidnih protivnetnih učinkovin. Mobilna faza in ostali parametri pri razvoju analizne metode 2 so bili izbrani dvodimenzionalno, saj je metoda uporabna tako na HPLC-UV/VIS kot tudi na LC-ESI-MSMS. Izbor uporabe sistema je odvisen predvsem od koncentracijskega območja sproščenega naproksena iz alginatnih oblog, ki je odvisen predvsem od načina priprave. V primeru sproščanja iz alginatnih oblog je sistem LC-ESI-MSMS primeren predvsem v načinu MRM, kjer v vzorcu lahko kvalificiramo in kvantificiramo točno določen fragment, m/z 231.
Keywords:	HPLC, nesteroidne protivnetne učinkovine (NSAID), validacija, površinske lastnosti
Place of publishing:	Maribor
Publisher:	[T. Zabukovec]
Year of publishing:	2014
PID:	20.500.12556/DKUM-45676
UDC:	543.544.5:677.017.86(043.2)
COBISS.SI-ID:	18213654
NUK URN:	URN:SI:UM:DK:X0URLA0U
Publication date in DKUM:	11.09.2014
Views:	4976
Downloads:	639
Metadata:
Categories:	KTFMB - FKKT
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Secondary language

Language:	English
Title:	DEVELOPMENT AND VALIDATION OF HPLC ANALYTICAL METHOD FOR THE DETERMINATION OF NON-STEROIDAL ANTI-INFLAMMATORY DRUGS
Abstract:	The topic of following dissertation is the development and validity of high-performance liquid chromatography (HPLC-UV/VIS), which is the method of analysis for determining non-steroid anti-inflammatory substances. Furthermore, it discusses the transfer of developed method on LC-ESI-MSMS, where different procedures of sample preparation are the ones, which influence our choice of analysis system for qualification and quantification. A lot of attention was given to different procedures of preparing such dressings, which are connected to analgesics (painkillers) that belong to the group of non-steroidal anti-rheumatics (NSAID). The characteristic of the alginate dressings is that after applying them on the spot of skin inflammation, they are formed on the wound or inflammation, thereby optimal skin moisture is achieved, and physical-chemical characteristics cause faster healing and hemostatic effect. By putting non-steroid anti-inflammatory substances in high-absorbing non-woven fabric dressings, we wished to achieve slow and controlled release on the spot of inflammation. The results show that we do not achieve the wanted release by implementing the procedures of applying naproxen on the alginate dressing. However, with the procedures of modification of the primary method the even release can be achieved. Moreover, for the quantification of the released naproxen from dressings prepared that way by implementing the method 2, with the procedures of validity of the method, we managed to check, whether the method gives correct and accurate results, and is therefore suitable for routine prescription of non-steroid anti-inflammatory substances. The mobile phase and other parameters at development of the analysis of the method 2 were selected two-dimensionally, since the method can be useful on HPLC-UV/VIS as well as on LC-ESI-MSMS. The choice of system which is going to be used, depends mainly of the concentration area of the released naproxen from the alginate dressings. However, this depends mainly of the manner of preparation. In case of release from the alginate dressings, the system LC-ESI-MSMS is suitable mainly in the manner MRM, where even the precisely determined fragment, m/z 231, can be qualified and quantified in a sample.
Keywords:	HPLC, non-steroidalanti-inflammatory drugs (NSAIDs), validation, measurement uncertainty

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