2A liquid chromatography method is reported for the determination of diclofenac potassium and its impurities using Quality by Design criteria. Central composite design was used for the investigation of the influence of critical parameters on performance that included the methanol concentration in the mobile phase, the pH of the aqueous phase, and the potassium dihydrogen phosphate concentration in the aqueous phase. Mathematical models enabled theoretical examination of experimental space to achieve maximal separation in minimal analysis time. A Monte Carlo simulation was used to evaluate the risk of uncertainty in model predictions, to adjusting process parameters, and to identify design space. Fractional factorial design was employed for robustness testing and method was fully validated. Optimal conditions were a C18 150 mm 4.6 mm, 5 m particle size column; a methanol -68.3 mmol L 1 potassium dihydrogenphosphate (68.7:31.3, v/v) mobile phase at pH 3.0, a flow rate of 1 mL min 1 , a column temperature of 25C, and ultraviolet detection at 254 nm.
Identifikacija karakterističnih antocijanina u proizvodima dobijenim iz ploda aronije tehnikom visokoefikasne tečne hromatografije (HPLC) Kratak sadržaj Plod aronije ima široku primenu kao boja i korigens ukusa u prehrambenoj industriji, zbog svojih adstringentnih osobina i tamnoljubičaste boje. Ova biljka ima dugogodišnju primenu u tradicionalnoj medicini u Evropi i Severnoj Americi, i postoje brojne naučne studije o njenim farmakološkim efektima. Plodovi su bogati fenolnim sastojcima (procijanidinima, antocijaninima i fenolnim kiselinama). Poznato je da ovi sastojci imaju osobine antioksidanasa, i stoga imaju primenu u prevenciji srčanih, inflamatornih i malignih bolesti. Antocijanini su biljni pigmenti široko rasprostranjeni u obojenom voću i cveću. Količina i sastav u bobicama se razlikuju u odnosu na biljnu vrstu, način uzgajanja i obrade. U poređenju sa ostalim bobicama i voćem, aronija ima jednostavan sastav antocijanina,, koji uglavnom čine cijanidin glikozidi. Cilj ovog rada je bio identifikacija karakterističnih antocijanina u proizvodima od aronije i razlikovanje aronije od drugih biljnih izvora sličnog sastava. Za dobijanje karakterističnog hromatografskog fingerprinta korišćena je HPLC/PDA tehnika. Na hromatogramu rastvora uzorka aronije, karakteristična su četiri pika, koji odgovaraju pikovima glavnih antocijanina aronije (cijanidinarabinozid, cijanidin-glukozid, cijanidin-galaktozid i cijanidin-ksilozid). Na hromatogramima dobijenim iz rastvora drugih uzoraka, razlikuje se distribucija pikova. Ima više pikova, na različitim retencionim vremenima, i nema pikova karakterističnih antocijanina aronije. Ovo ukazuje da se navedna metoda može primeniti za razlikovanje preparata aronije od mogućih falsifikata.
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