Faculty of Pharmacy, Lj. (FFALJ)
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Razvoj in validacija analitike HPLC za ugotavljanje plazemskih koncentracij haloperidola in njegovih metabolitov : Development and validation of HPLC method for quantification of haloperidol and its metabolites in human blod plasmaPolanc, DarjaV diplomski nalogi smo razvili analizno metodo za spremljanje terapevtskih koncentracij haloperidola in dveh metabolitovČ 4-(4-klorofenil)-4-hidroksipiperidin (metabolit 1) in ... 4-(4ć-klorofenil)-(4ć-fluorofenil)-4-hidroksi-1-piperidinbutanol (metabolit 2). Metoda izbire je bila tekoèinska kromatografija visoke loèljivosti (HPLC) v kombinaciji z ekstrakcijo na trdni fazi (SPE). Postopek ekstrakcije smo razvili za analizo baziènih spojin. Uporabili smo kolone Bond Elut C18. Ekstrakcija je potekala v stirih fazahČ kondicioniranje kolone, nanos vzorca, spiranje kolone ter eluiranje analitov (metabolita 1, metabolita 2 in haloperidola). Zaradi uporabe baziènih topil smo ze pred elucijo sprali s kolone metabolit 3, ki je kislina (3-(4-florobenzoil) propanojska kislina). Ekstrahirane vzorce smo posusili s tokom dusika in nato suh ostanek raztopili v mobilni fazi. Za interni standard smo uporabili klorov analog haloperidola. Analizo smo izvajali s kolono Hypersil C18 (250 x 4.6 mm, velikost delcev 5 m), s predkolono Hypersil C18 (10 x 4.6 mm, velikost delcev 5 m) in predfiltrom (4 x 3.0 mm). Kolono smo termostatirali na 35 C, pretok mobilne faze pa je bil 0.9 mLžmin. Mobilna faza je bila sestavljena iz fosfatnega pufra (0.050 M, pH 2.5) in metanola (47Č53). Injicirali smo 50 L vzorca. Doloèili smo optimalne valovne dolzine detekcijeČ 210 nm za metabolit 2 in haloperidol, 219 nm za metabolit 1 in 255 nm za interni standard. Retencijski èasi metabolita 1, metabolita 2, haloperidola in internega standarda so bili 4.4, 8.3, 10.0 in 16.5 min. Analiza enega vzorca plazme je tako trajala 18.5 min. Izkoristki ekstrakcije vseh analitov pri treh razliènih koncentracijah sobili priblizno 90%. Metoda je linearna v obmoèju od 10 ngžmL do 200 ngžmL. Pearsonov koeficient (R2) je visji od 0.996. Meja detekcije za haloperidol je 1.4 ngžmL, za metabolit 1 2.5 ngžmL in za metabolit 2 1.9 ngžmL. Pri med dnevni ponovljivosti so bili koeficienti variacije manjsi od 5.1%. Toènost metode za vse tri analite, v celotnem koncentracijskem obmoèju, je med 90.0% in 109.8%. Metoda je validirana po ICH smernicah in primerna za spremljanje terapevtskih koncentracij haloperidola in njegovih metabolitov v plazmi.Type of material - undergraduate thesisPublication and manufacture - Ljubljana : [Polanc, D.], 2005Language - slovenianCOBISS.SI-ID - 1688689
Author
Polanc, Darja
Other authors
Mrhar, Aleš |
Grabnar, Iztok
Topics
haloperidol |
analitika |
validacija |
HPLC analitika |
metode |
SPE
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Knjižnica dp 0000000615 Polanc Darja Razvoj IN: 0008153 Knjižnica dp 615 Polanc Darja Razvoj IN: 0008153 |
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Database name | Field | Year |
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Links to authors' personal bibliographies | Links to information on researchers in the SICRIS system |
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Polanc, Darja | ![]() |
Mrhar, Aleš | 06086 |
Grabnar, Iztok | 16107 |
Source: Personal bibliographies
and: SICRIS
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