Enantioselective determination of metoprolol in plasma by liquid chromatography on a silica-bonded α 1-acid glycoprotein column

Development of a sensitive and rapid method for quantitation of (S)-(−)- and (R)-(+)-metoprolol in human plasma by chiral LC–ESI–MS/MS

“…As evident from the available literature, bulk of the methods reported on enantiomeric analysis of metoprolol is based on direct analysis on chiral columns [7] , [10] , [11] , [12] , [13] , [14] , [17] , [18] , [19] , [20] , [21] , [22] , [23] . This is apparently due to comparable or better assay sensitively [19] without an additional derivatization step during sample processing than indirect methods.…”

“…Moreover, easy availability of wide variety of stable and rugged chiral stationary phases has further propelled their use in enantioselective analysis. All five major classes of stationary phases including macrocyclic glycopeptide [20] , [22] , polysaccharide [10] , [12] , [13] , [14] , [17] , [18] , [19] , [21] , protein [11] , [17] , [23] , cyclodextrin [17] and Pirkle-type [17] have been used in the separation and quantitation of metoprolol enantiomers from biological samples with varying degree of success. Moreover, these stationary phases can be used under normal and reversed-phase conditions and also with modified polar organic mobile phases, except the protein based stationary phase.…”

“…All reported methodologies based on direct approach have used either SPE [10] , [14] , [19] , [20] or liquid–liquid extraction (LLE) in the presence of a base [7] , [11] , [12] , [13] , [17] , [18] , [19] , [21] , [22] for quantitative recovery of analytes. As metoprolol is a basic drug (pka 9.7), it can be readily converted to an unionized state with a base for better extraction efficiency during LLE.…”

“…As metoprolol is a basic drug (pka 9.7), it can be readily converted to an unionized state with a base for better extraction efficiency during LLE. Several solvent systems such as dichloromethane [17] , [18] , dichloromethane-diisopropyl ether [7] , [19] , [21] , diethyl ether [12] , [13] , dichloromethane-diethyl ether [11] and ethyl acetate [22] have been used previously for LLE. Thus, both these conventional techniques were tested for optimum recovery with minimum matrix interference during method development trials.…”

“…Moreover, ionic strength, pH, type and concentration of organic modifiers play a significant role in the retention and resolution on protein- based phases [1] . Chiral-AGP column has been used previously by Persson et al [11] with a mobile phase consisting of phosphate buffer (pH 7.0) and acetonitrile under gradient HPLC conditions. Similarly, Kim et al [17] used a 20 mM phosphate buffer as the mobile phase to obtain a resolution ( R s ) of 1.79 for metoprolol enantiomers under isocratic conditions.…”

Development of a sensitive and rapid method for quantitation of (S)-(−)- and (R)-(+)-metoprolol in human plasma by chiral LC–ESI–MS/MS

“…As evident from the available literature, bulk of the methods reported on enantiomeric analysis of metoprolol is based on direct analysis on chiral columns [7] , [10] , [11] , [12] , [13] , [14] , [17] , [18] , [19] , [20] , [21] , [22] , [23] . This is apparently due to comparable or better assay sensitively [19] without an additional derivatization step during sample processing than indirect methods.…”

“…Moreover, easy availability of wide variety of stable and rugged chiral stationary phases has further propelled their use in enantioselective analysis. All five major classes of stationary phases including macrocyclic glycopeptide [20] , [22] , polysaccharide [10] , [12] , [13] , [14] , [17] , [18] , [19] , [21] , protein [11] , [17] , [23] , cyclodextrin [17] and Pirkle-type [17] have been used in the separation and quantitation of metoprolol enantiomers from biological samples with varying degree of success. Moreover, these stationary phases can be used under normal and reversed-phase conditions and also with modified polar organic mobile phases, except the protein based stationary phase.…”

“…All reported methodologies based on direct approach have used either SPE [10] , [14] , [19] , [20] or liquid–liquid extraction (LLE) in the presence of a base [7] , [11] , [12] , [13] , [17] , [18] , [19] , [21] , [22] for quantitative recovery of analytes. As metoprolol is a basic drug (pka 9.7), it can be readily converted to an unionized state with a base for better extraction efficiency during LLE.…”

“…As metoprolol is a basic drug (pka 9.7), it can be readily converted to an unionized state with a base for better extraction efficiency during LLE. Several solvent systems such as dichloromethane [17] , [18] , dichloromethane-diisopropyl ether [7] , [19] , [21] , diethyl ether [12] , [13] , dichloromethane-diethyl ether [11] and ethyl acetate [22] have been used previously for LLE. Thus, both these conventional techniques were tested for optimum recovery with minimum matrix interference during method development trials.…”

“…Moreover, ionic strength, pH, type and concentration of organic modifiers play a significant role in the retention and resolution on protein- based phases [1] . Chiral-AGP column has been used previously by Persson et al [11] with a mobile phase consisting of phosphate buffer (pH 7.0) and acetonitrile under gradient HPLC conditions. Similarly, Kim et al [17] used a 20 mM phosphate buffer as the mobile phase to obtain a resolution ( R s ) of 1.79 for metoprolol enantiomers under isocratic conditions.…”

Development of a sensitive and rapid method for quantitation of (S)-(−)- and (R)-(+)-metoprolol in human plasma by chiral LC–ESI–MS/MS

“…As evident from the available literature, bulk of the methods reported on enantiomeric analysis of metoprolol is based on direct analysis on chiral columns [7] , [10] , [11] , [12] , [13] , [14] , [17] , [18] , [19] , [20] , [21] , [22] , [23] . This is apparently due to comparable or better assay sensitively [19] without an additional derivatization step during sample processing than indirect methods.…”

“…Moreover, easy availability of wide variety of stable and rugged chiral stationary phases has further propelled their use in enantioselective analysis. All five major classes of stationary phases including macrocyclic glycopeptide [20] , [22] , polysaccharide [10] , [12] , [13] , [14] , [17] , [18] , [19] , [21] , protein [11] , [17] , [23] , cyclodextrin [17] and Pirkle-type [17] have been used in the separation and quantitation of metoprolol enantiomers from biological samples with varying degree of success. Moreover, these stationary phases can be used under normal and reversed-phase conditions and also with modified polar organic mobile phases, except the protein based stationary phase.…”

“…All reported methodologies based on direct approach have used either SPE [10] , [14] , [19] , [20] or liquid–liquid extraction (LLE) in the presence of a base [7] , [11] , [12] , [13] , [17] , [18] , [19] , [21] , [22] for quantitative recovery of analytes. As metoprolol is a basic drug (pka 9.7), it can be readily converted to an unionized state with a base for better extraction efficiency during LLE.…”

“…As metoprolol is a basic drug (pka 9.7), it can be readily converted to an unionized state with a base for better extraction efficiency during LLE. Several solvent systems such as dichloromethane [17] , [18] , dichloromethane-diisopropyl ether [7] , [19] , [21] , diethyl ether [12] , [13] , dichloromethane-diethyl ether [11] and ethyl acetate [22] have been used previously for LLE. Thus, both these conventional techniques were tested for optimum recovery with minimum matrix interference during method development trials.…”

“…Moreover, ionic strength, pH, type and concentration of organic modifiers play a significant role in the retention and resolution on protein- based phases [1] . Chiral-AGP column has been used previously by Persson et al [11] with a mobile phase consisting of phosphate buffer (pH 7.0) and acetonitrile under gradient HPLC conditions. Similarly, Kim et al [17] used a 20 mM phosphate buffer as the mobile phase to obtain a resolution ( R s ) of 1.79 for metoprolol enantiomers under isocratic conditions.…”

Development of a sensitive and rapid method for quantitation of (S)-(−)- and (R)-(+)-metoprolol in human plasma by chiral LC–ESI–MS/MS

“…As evident from the available literature, bulk of the methods reported on enantiomeric analysis of metoprolol is based on direct analysis on chiral columns [7] , [10] , [11] , [12] , [13] , [14] , [17] , [18] , [19] , [20] , [21] , [22] , [23] . This is apparently due to comparable or better assay sensitively [19] without an additional derivatization step during sample processing than indirect methods.…”

“…Moreover, easy availability of wide variety of stable and rugged chiral stationary phases has further propelled their use in enantioselective analysis. All five major classes of stationary phases including macrocyclic glycopeptide [20] , [22] , polysaccharide [10] , [12] , [13] , [14] , [17] , [18] , [19] , [21] , protein [11] , [17] , [23] , cyclodextrin [17] and Pirkle-type [17] have been used in the separation and quantitation of metoprolol enantiomers from biological samples with varying degree of success. Moreover, these stationary phases can be used under normal and reversed-phase conditions and also with modified polar organic mobile phases, except the protein based stationary phase.…”

“…All reported methodologies based on direct approach have used either SPE [10] , [14] , [19] , [20] or liquid–liquid extraction (LLE) in the presence of a base [7] , [11] , [12] , [13] , [17] , [18] , [19] , [21] , [22] for quantitative recovery of analytes. As metoprolol is a basic drug (pka 9.7), it can be readily converted to an unionized state with a base for better extraction efficiency during LLE.…”

“…As metoprolol is a basic drug (pka 9.7), it can be readily converted to an unionized state with a base for better extraction efficiency during LLE. Several solvent systems such as dichloromethane [17] , [18] , dichloromethane-diisopropyl ether [7] , [19] , [21] , diethyl ether [12] , [13] , dichloromethane-diethyl ether [11] and ethyl acetate [22] have been used previously for LLE. Thus, both these conventional techniques were tested for optimum recovery with minimum matrix interference during method development trials.…”

“…Moreover, ionic strength, pH, type and concentration of organic modifiers play a significant role in the retention and resolution on protein- based phases [1] . Chiral-AGP column has been used previously by Persson et al [11] with a mobile phase consisting of phosphate buffer (pH 7.0) and acetonitrile under gradient HPLC conditions. Similarly, Kim et al [17] used a 20 mM phosphate buffer as the mobile phase to obtain a resolution ( R s ) of 1.79 for metoprolol enantiomers under isocratic conditions.…”