2 research outputs found
Simultano UV-spektrofotometrijsko odreÄivanje ramiprila, acetilsalicilne kiseline i atorvastatin kalcija u kapsulama primjenom kemometrijskih metoda
In the present work, three different spectrophotometric methods for simultaneous estimation of ramipril, aspirin and atorvastatin calcium in raw materials and in formulations are described. Overlapped data was quantitatively resolved by using chemometric methods, viz. inverse least squares (ILS), principal component regression (PCR) and partial least squares (PLS). Calibrations were constructed using the absorption data matrix corresponding to the concentration data matrix. The linearity range was found to be 1-5, 10-50 and 2-10 Āµg mLā1 for ramipril, aspirin and atorvastatin calcium, respectively. The absorbance matrix was obtained by measuring the zero-order absorbance in the wavelength range between 210 and 320 nm. A training set design of the concentration data corresponding to the ramipril, aspirin and atorvastatin calcium mixtures was organized statistically to maximize the information content from the spectra and to minimize the error of multivariate calibrations. By applying the respective algorithms for PLS 1, PCR and ILS to the measured spectra of the calibration set, a suitable model was obtained. This model was selected on the basis of RMSECV and RMSEP values. The same was applied to the prediction set and capsule formulation. Mean recoveries of the commercial formulation set together with other figures of merit (calibration sensitivity, selectivity, limit of detection, limit of quantification and analytical sensitivity) were estimated. Validity of the proposed approaches was successfully assessed for analyses of drugs in the various prepared physical mixtures and formulations.U radu su opisane tri razliÄite spektrofotometrijske metode za odreÄivanje ramiprila, acetilsalicilne kiseline i atorvastatin kalcija u sirovinama i formulacijama. Preklapanje podataka kvantitativno je rijeÅ”eno pomoÄu kemometrijskih metoda, tj. metodama inverznih najmanjih kvadrata (ILS), regresije glavnog sastojka (PCR) i djelomiÄnih najmanjih kvadrata (PLS). Kalibracije su postavljene pomoÄu matrice podataka za apsorpciju koja odgovara matrici pripadajuÄih koncentracija. PodruÄje linearnosti za ramipril iznosilo je 1ā5, za acetilsalicilnu kiselinu 10ā50, a za atorvastatin kalcij 2ā10 Āµg mLā1. Matrica s apsorbancijama dobivena je mjerenjem apsorbancije nultog reda na valnim duljinama izmeÄu 210 i 320 nm. Set podataka za koncentracije ramiprila, acetilsalicilne kiseline i atorvastatin kalcija u smjesi statistiÄki je tako organiziran da osigura maksimalnu koliÄinu informacije u spektrima i minimalizira greÅ”ku multivarijantnih kalibracija. Primjenom odgovarajuÄih algoritama za PLS, PCR i ILS na snimljene spektre kalibracijskog seta dobiven je dobar model, koji je odabran na temelju RMSECV i RMSEP vrijednosti. Isti model je primijenjen i na set s predviÄenim vrijednostima i na kapsule sa smjesom ove tri ljekovite tvari. OdreÄena je srednja vrijednost povrata za komercijalnu formulaciju te ostale analitiÄke izvedbene znaÄajke (kalibracijska osjetljivost, selektivnost, granica dokazivanja, granica odreÄivanja i analitiÄka osjetljivost). PotvrÄena je primjenjljivost predloženih metoda u analizama lijekova u fiziÄkim smjesama i u gotovim ljekovitim oblicima