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Determination of candesartan in human plasma with liquid chromatography - tandem mass spectrometry
Vanja Forjan, Lea Cvitkovič-Maričič, Helena Prosen, Darinka Brodnjak-Vončina, 2016, original scientific article

Abstract: A sensitive, specific and rapid liquid chromatography - tandem mass spectrometry method was developed and validated for the determination of candesartan in human plasma. Analyte was separated from endogenous components present in plasma by solid phase extraction. Chromatographic separation was performed on Gemini C18 analytical column using mobile phase acetonitrile – 5 mM ammonium formate pH 2 (90:10, v/v) at flow rate of 0.3 mL/min. For detection, tandem mass spectrometry in SRM mode with positive electrospray ionization was used. The mass transitions m/z 441.1 > 263.1 and 445.1 > 267.1 were used to determine candesartan by using candesartan-d4 as an internal standard. After development, the method was validated according to the requirements of EMA regulatory guidelines in the concentration range 1 - 400 ng/ml in human plasma. Limit of quantification (LLOQ) was 1 ng/ml. The developed and validated method proved to be very fast and reproducible and was therefore successfully implemented in pharmacokinetic and bioequivalence studies with large number of study samples.
Keywords: candesartan, liquid chromatography, tandem mass spectrometry, human plasma
Published in DKUM: 17.08.2017; Views: 1548; Downloads: 391
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Razvoj, validacija in primerjava bioanaliznih metod HPLC in LC-MS/MS za določanje kandesartana v humani plazmi
Vanja Forjan, 2016, master's thesis

Abstract: Kandesartan je farmakološko aktivni metabolit kandesartan cileksetila iz skupine sartanov, ki se uporablja za zdravljenje hipertenzije. V okviru magistrske naloge smo najprej razvili metodo za določanje kandesartana v humani plazmi, ki obsega pripravo plazemskih vzorcev z ekstrakcijo na trdno fazo na ekstrakcijskih kolonah Strata X in analizo pripravljenih plazemskih vzorcev s HPLC instrumentalno tehniko. Razvito metodo smo validirali in dokazali, da je selektivna, točna, ponovljiva in linearna v območju od 4 ng/ml do 400 ng/ml. Da smo dosegli spodnjo mejo določljivosti 1 ng/ml, smo za detekcijo uporabili tandemsko masno spektrometrijo (LC-MS/MS) v SRM načinu z uporabo pozitivne ionizacije z elektro- razprševanjem. Po končanem razvoju smo metodo statistično ovrednotili v koncentracijskem območju od 1 do 400 ng/ml v humani plazmi in pri tem uporabili metodo internega standarda, ovrednotenje metode pa smo izvedli z določitvijo naslednjih validacijskih parametrov: selektivnost, linearnost, ponovljivost in pravilnost, spodnja meja določljivosti (LLOQ), izkoristek priprave vzorca, vpliv matrice, matrični faktor, vpliv redčenja, vpliv hemolitične plazme, testiranje čistosti sistema ter različne stabilnostne pogoje kandesartana v raztopinah in plazmi. Razviti in ovrednoteni metodi sta se v praksi izkazali kot učinkoviti, saj lahko z njima analiziramo veliko število vzorcev v kratkem času, hkrati pa sta natančni, točni in robustni v daljšem časovnem obdobju.
Keywords: kandesartan, SPE, HPLC, LC-MS/MS
Published in DKUM: 19.07.2016; Views: 2037; Downloads: 237
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