Gradijentna HPLC analiza raloksifen hidroklorida i primjena u kontroli kvalitete

A rapid, sensitive and selective method for the determination of raloxifene hydrochloride (RLX) in pure drug and in tablets was developed using gradient high performance liquid chromatography (HPLC). The devised method involved separation of RLX on a reversed phase Hypersil ODS column and determination with UV detection at 284 nm. The standard curve was linear (R = 0.999) over the concentration range of 50-600 μg mL1 with a detection limit of 0.04 μg mL1 and a quantification limit of 0.16 μg mL1. Intra-day and inter-day precision and accuracy of the method were established according to the current ICH guidelines. Intra-day RSD values at three QC levels (250, 450 and 550 μg mL1) were 0.20.5% based on the peak area. The intra-day relative error (er) was between 0.2 and 0.5%. The developed method was successfully applied to the determination of RLX in tablets and the results were statistically compared with those obtained by a literature method. Accuracy, evaluated by means of the spike recovery method, was excellent with percent recovery in the range 97.7103.2 with precision in the range 1.62.2%. No interference was observed from the conformulated substances. The method was economical in terms of the time taken and the amount of solvent used.Koristeći gradijentnu tekućinsku kromatografiju visoke učinkovitosti razvijena je brza, osjetljiva i selektivna metoda za određivanje raloksifen hidroklorida (RLX), čiste supstancije i u tabletama. U radu je primijenjena reverzno-fazna kolona Hypersil ODS te UV detekcija pri 284 nm. Standardna krivulja bila je linearna (R = 0,999) u koncentracijskom području 50600 μg mL1. Granica detekcije bila je 0,04 μg mL1 a granica određivanja 0,16 μg mL1. Repetabilnost, intermedijalna preciznost i ispravnost ispitivane su prema važećim ICH uputama. Mjerenjem površine ispod pika na tri koncentracijske razine (250, 450 i 550 μg mL1) procijenjena je repetabilnost na 0,20,5%. Relativna pogreška procijenjena unutar jednog dana (er) bila je između 0,2 i 0,5%. Razvijena metoda uspješno je primijenjena za određivanje RLX u tabletama. Rezultati su statistički uspoređeni s rezultatima dobivenim prema ranije objavljenoj metodi. Analitički povrat bio je u rasponu 97,7103,2 uz preciznost od 1,6 do 2,2%. Nije primijećena interferencija pomoćnih tvari. Metoda je ekonomična s obzirom na utrošeno vrijeme i količine upotrebljenog otapala