Determination of Metoprolol and Felodipine in Binary Mixture Using Chemometric Assisted Spectrophotometric and High-Performance Liquid Chromatographic-UV Mmethods

Abstract

Four methods were developed for simultaneous determination of metoprolol and felodipine without previous separation. In the first method both drugs were determined using first derivative UV spectrophotometry, with zero crossing measurement at 222 and 235 nm for metoprolol and felodipine, respectively. The second method depends on first derivative of the ratios spectra by measurements of the amplitudes at 250.1 nm for metoprolol and 224.3 nm for felodipine. Calibration graphs are established in the range of 20-150 µg/ml and 10-60 µg/ml for metoprolol and felodipine, respectively. The third method describes the use of multivariate spectrophotometric calibration for the simultaneous determination of the analyzed binary mixture where the resolution is accomplished by using partial least squares (PLS) regression analysis. Although the components show high degree of spectral overlap, they are simultaneously determined with high accuracy and without interference of pharmaceutical dosage form excipients. A comparison with the related multivariate method of classicial least squares (CLS) analysis is done showing less relative results due to severe spectral overlap of the studied drugs. In the fourth method (HPLC), a reversed-phase column and a mobile phase of methanol:water:acetonitrile (70:22:8 v/v/v/) at 0.9 ml/min flow rate is used to separate both drugs and UV detection at 260 nm. Good linearities are obtained in concentration range of 0.15-15 µg/ml for metoprolol and 0.03-5 µg/ml for felodipine. All the proposed methods are extensively validated. They have the advantage of being economic and time saving. All the described methods can be readily utilized for the analysis of pharmaceutical formulations, the fourth method (HPLC) is successfully applied for the analysis of both drugs in human serum samples. The results obtained by adopting the proposed methods are statistically analyzed and compared with those obtained by reported methods.

Quantification of Zolpidem in Canine Plasma

“…It was necessary to validate each step in the analytical method so that this protocol can be utilised in future pharmacokinetic and toxicological studies (Salem and Abdallah, 2007;Carrillo-Lopez et al, 2010).…”

RP-HPLC method development and validation for simultaneous estimation of ramipril and felodipine

“…RMP was determined individually by spectrophotometric methods [5][6][7], HPLC [6,[8][9][10], HPTLC [11,12] and electrochemical methods [13][14][15][16]. On the other hand, FLD was determined individually by UV spectroscopy [17][18][19][20], HPLC [18,[21][22][23], spectrofluorimetric [24], gas chromatography [25] and electrochemical methods [26,27]. Meanwhile, some spectrophotometric [28,29], HPLC [28][29][30][31] and HPTLC [32] methods were reported for the simultaneous determination of both drugs.…”

Development and validation of TLC–densitometric method for simultaneous determination of two binary antihypertensive mixtures containing felodipine in fixed dose combinations

“…Only a few methods have been reported in the literature for the assay of FLD–MTP mixture, using chemometrically assisted spectrophotometric, HPLC (Rontogianni et al ., ; Salem and Abdallah, ; Wen‐Gang et al ., ) and spectrofluorimetric methods (Walash et al ., ; Zhang et al ., ).…”

“…Individual determination of FLD has been carried out in human plasma by capillary gas chromatography (Ahnoff, ), high selectivity gas chromatography (Ahnoff et al ., ) and HPLC (Lindmark et al ., ; Lopez et al ., ; Soons et al ., ; Wen‐Gang et al ., ). In pharmaceutical formulations, FLD has been determined by HPLC (Baranda et al ., ; Björklund et al ., ; Cardoza and Amin, ; El Yazbi et al ., ; Fusun et al ., ; Karlsson et al ., ; Salem and Abdallah, ), spectrofluorimetric (El Yazbi et al ., ; Walash et al ., ) and spectrophotometric methods (Basavaiah et al ., ; El Yazbi et al ., ; Fusun et al ., ; Gottfries et al ., ; Marciniec et al ., ; Meyyanathan et al ., ; Salem and Abdallah, ).…”