PRIPRAVA STANDARDOV PIMEKROLIMUSOVIH NEČISTOČ

Brodar, Marjeta

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Title:	PRIPRAVA STANDARDOV PIMEKROLIMUSOVIH NEČISTOČ
Authors:	ID Brodar, Marjeta (Author) ID Finšgar, Matjaž (Mentor) More about this mentor...
Files:	VS_Brodar_Marjeta_2016.pdf (3,94 MB) MD5: 9938E01BDD26AF232235363752583CAD
Language:	Slovenian
Work type:	Bachelor thesis/paper
Typology:	2.11 - Undergraduate Thesis
Organization:	FKKT - Faculty of Chemistry and Chemical Engineering
Abstract:	Učinkovine, ki so sestavni del zdravil, morajo biti učinkovite, varne in kakovostne. Vse to pa preverjamo s pomočjo raznih analitskih postopkov. Pri analitskih metodah, poleg same vsebnosti aktivne učinkovine, dokazujemo tudi prisotnost nečistoč. Pokazale so se potrebe po zagotavljanju standardov posameznih nečistoč pimekrolimusa. Namen tega diplomskega dela je, da zagotovimo zadostno količino posamezne prečiščene nečistoče. Da nam je to uspelo, smo morali najprej pridobiti zadostno količino začetnega materiala. V diplomskem delu smo se opredelili na analitski del izolacije posamezne nečistoče pimekrolimusa. Začetni material vsake posamezne nečistoče smo najprej analizirali na LC/MS/MS-instrumentu. Tako smo dobili UV in masne spektre vstopnih vzorcev. Na podlagi tega smo se odločili v katerem delu preparativne analize bomo zbirali frakcije. Sledilo je čiščenje nečistoče s preparativno HPLC kromatografijo. Najprej smo morali optimizirati samo metodo, glede na posamezno nečistočo. Pri preperativni HPLC kromatografiji smo zbirali posamezne frakcije, katere smo nato analizirali na LC/MS/MS- instrumentu in se na podlagi rezultatov odločili, katere frakcije so dovolj čiste, da gredo lahko v izolacijo, katere zavržemo in katere združimo in ponovno čistimo s preparativno HPLC kromatografijo. Na koncu smo frakcije, v katerih je bila prisotna čista nečistoča združili in izolirali. Izolirano nečistočo smo ponovno analizirali, da smo potrdili njeno čistost. Končna potrditev je bila narejena z NMR analizo. Strmimo k čimboljšem izkoristku izolacije nečistoče.
Keywords:	pimekrolimus, nečistoče pimekrolimusa, preparativna HPLC kromatografija, LC/MS analitika.
Place of publishing:	Maribor
Publisher:	[M. Brodar]
Year of publishing:	2016
PID:	20.500.12556/DKUM-63052
UDC:	543.544.5HPLC(043.2)
COBISS.SI-ID:	20323862
NUK URN:	URN:SI:UM:DK:WM9H0KKI
Publication date in DKUM:	17.10.2016
Views:	1813
Downloads:	196
Metadata:
Categories:	KTFMB - FKKT
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Secondary language

Language:	English
Title:	PREPARATION OF STANDARDS FOR PIMECROLIMUS IMPURITIES
Abstract:	Substances, which are a part of medicines, must be effective, safe, and qualitative. All that is checked by using various analysis procedures. In addition to content of active substance, in analysis methods we also prove the presence of impurities. The needs for ensuring standards of individual impurities of pimecrolimus were revealed. The purpose of this graduation thesis is to provide a sufficient amount of individual purified impurity. In order to do that, first we had to obtain a sufficient amount of the starting material. Some of the impurities were obtained by synthesis at the Genetics department, and others at the TLCM department, where they were obtained with taking on industrial preparative chromatography. In the graduation thesis, we focused on the analysis part of isolation of individual impurity of pimecrolimus. The starting material of each individual impurity was first analysed on LC/MS/MS-instrument. Therefore, we obtained UV and mass spectra of input samples. Based on that, we decided in which part of the preparative analysis we will collect fractions. This was followed by cleaning the impurity with preparative HPLC chromatography. First, we had to optimise the method itself in regard to the individual impurity. In preparative HPLC chromatography we collected individual fractions that were later analysed on LC/MS/MS- instrument, and based on the results we determined, which fractions are clean enough to go to isolation, which are discarded, and which are united and once again cleaned with preparative HPLC chromatography. At the end, the fractions, in which a clean impurity was present, were united and isolated. The isolated impurity was once again analysed to confirm its cleanliness. The final confirmation was made at the RFU department at the company LEK Mengeš by NRM analysis. We are directed toward optimization of efficiency of isolation of the impurity. The results show that we managed to isolate the impurities with content of more than 80%.
Keywords:	pimecrolimus, impurities of pimecrolimus, preparative HPLC chromatography, LC/MS/MS-analysis

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